CN117165117A - Preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating - Google Patents
Preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating Download PDFInfo
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- CN117165117A CN117165117A CN202311279167.1A CN202311279167A CN117165117A CN 117165117 A CN117165117 A CN 117165117A CN 202311279167 A CN202311279167 A CN 202311279167A CN 117165117 A CN117165117 A CN 117165117A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/80—Processes for incorporating ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/30—Mixing paints or paint ingredients, e.g. pigments, dyes, colours, lacquers or enamel
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Abstract
The invention discloses a preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating, which comprises the following steps: the preparation of alloy powder, the preparation of glue, the preparation of diffusion coating, pretreatment, coating, surface drying and heat treatment, and the compounding of the glue, anti-adhesion powder and auxiliary agent ensures that the coercive force can be greatly improved under the use condition of less diffusion of heavy rare earth metal by controlling the components and granularity of the alloy powder, and the residual magnetism is hardly reduced or reduced slightly, and meanwhile, the phenomena of no falling of the coating and no adhesion between magnetic sheets after diffusion can be solved.
Description
Technical Field
The invention belongs to the grain boundary diffusion technology, and particularly relates to a preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating.
Background
The grain boundary diffusion can be divided into a surface coating diffusion method, a surface sputtering diffusion method and a gas phase evaporation method according to different diffusion sources, wherein the surface coating diffusion method is a method of preparing diffusion coating by mixing diffusion source materials, resin, auxiliary agents, solvents and the like, preparing a coating by brushing, spraying and the like, and performing high-temperature diffusion treatment after low-temperature surface drying. The coating diffusion method has the advantages that the coercive force of the magnet is improved, the remanence is not obviously reduced, and meanwhile, the method can also effectively reduce the dosage of the heavy rare earth additive and is suitable for large-scale production.
However, the method is also insufficient at present, for example, the diffusion depth is insufficient, the effective utilization rate is gradually reduced when the coating amount is increased, the coating is wasted, the phenomenon that the adhesive (the magnetic sheets are mutually adhered together) and the coating fall off are easy to occur, the adhesive can directly lead to the scrapping of a product, and the coating fall off can cause the diffusion material to separate from the base material so as to not achieve the purpose of diffusion, thereby causing the performance to be insufficient.
Disclosure of Invention
The invention aims to solve the problems in the background technology and provides a preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating.
The technical aim of the invention is realized by the following technical scheme:
a preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
s2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely dispersing and stirring the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder at a high speed under the protection of inert gas, and then taking out the mixture from the environment protected by the inert gas, continuing stirring at a high speed, and finishing the preparation of the diffusion coating.
The invention has the advantages that three alloy powders with different types (different element types) and different sizes are compounded, the synergistic diffusion effect of various alloys can be achieved, the coercive force is greatly improved under the condition of little residual magnetism reduction, the effect is better than that of a single material, and the utilization rate of rare earth can be improved.
Rare earth is not reduced basically, heavy rare earth is mainly reduced, and the price of the heavy rare earth is more expensive than that of common light rare earth and medium rare earth.
The design and the use of the glue, the anti-sticking powder and the auxiliary agent not only ensure that the coating does not fall off after diffusion, but also well prevent the adhesion phenomenon between the magnetic sheets after heat treatment.
After the bonded magnetic sheet is knocked out, unfilled corners and pits generally appear. Protrusions, etc., thereby resulting in rejection of the product.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce. The alloy powder is prepared by smelting, hydrogen breaking and jet milling processes in sequence.
The composite alloy powder is prepared by compounding three alloy powders of M0M1 and M2H, M Fe, and the grain sizes of M0M1 and M2H, M Fe are respectively controlled to be 0.5-1 mu M, 1-3 mu M and 0.5-1.5 mu M through smelting, hydrogen breaking and jet milling.
As improvement, the mass percentages of the three alloy powders of M0M1 and M2H, M Fe are respectively 20-45%, 35-50% and 15-20%.
The glue is prepared by completely dissolving resin in a solvent under the condition of mechanical stirring. The resin is mainly selected from polyvinyl butyral, polyethylene glycol, polyvinyl alcohol and polyvinyl pyrrolidone, and the solvent is mainly terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and propylene glycol butyl ether acetate or a combination of 1 or more of the above.
As a modification, the viscosity of the resin in step S2 is controlled to be 2-10 seconds. The viscosity of the resin is Saibot (Sagblt) n viscosity. Is a quantity of sample that is measured in "seconds" for 60 milliliters of sample to flow from the Sagnac viscometer at a specified temperature (e.g., 100 deg. F, F deg.F, 122 deg.F, etc.).
As an improvement, the mass percentage of the resin in the glue is 60-85%.
As a modification, the auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-glycidoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane
As improvement, the anti-adhesion powder is used for preventing the bonding between the neodymium iron boron magnetic sheets in the high-temperature treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the grain diameter is controlled within 80-120 mu m.
As an improvement, the diffusion coating comprises 60-85% of composite alloy powder by mass, 13-35% of glue by mass, 0.5-1.5% of auxiliary agent by mass and 2-5% of anti-adhesion powder by mass.
A diffusion treatment method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: carrying out ultrasonic degreasing, water washing, acid washing, ultrasonic water-based, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then carrying out water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate at 80-130 ℃ for 15-45 minutes, cooling to room temperature and discharging.
(4) And (3) heat treatment: tempering the sintered NdFeB substrate after surface drying at 850-950 ℃ for 5-35h, cooling to room temperature, tempering at 450-680 ℃ for 5-10h, cooling to room temperature, discharging, and finishing diffusion treatment.
Preferably, the preparation of diffusion coating adopts high-speed agitating unit, high-speed agitating unit is including jar body, primary stirring mechanism, secondary stirring mechanism, bleeder valve, the top of jar body is equipped with nitrogen gas air inlet, feed inlet, gas outlet, the bottom of protecting the jar body is equipped with the discharge gate, the bleeder valve is established on the discharge gate, primary stirring mechanism is established in the jar body, secondary stirring mechanism is established the discharge gate of bleeder valve.
According to the invention, nitrogen is pumped in through the nitrogen inlet, so that the tank body is in a nitrogen-protected environment, then the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder are subjected to high-speed dispersion stirring through the primary stirring mechanism, and after stirring, the mixture enters the secondary stirring mechanism through the discharge hole to continue high-speed stirring, so that the dispersity and the uniformity are improved.
Preferably, the primary stirring mechanism comprises a connecting rod, a driving gear, a driven gear and a rotating motor, wherein the rotating motor is arranged outside the tank body, the output end of the rotating motor penetrates through the tank body and extends to the inside of the tank body, the driving gear is arranged on the output end of the rotating motor, the driven gear is arranged on the outer side wall of the connecting rod, the driving gear and the driven gear are meshed with each other, a first stirring rod arranged in multiple layers is arranged on the side wall of the connecting rod, a hemispherical stirring blade is formed at the tail end of the stirring rod, a groove is formed in the hemispherical stirring blade, and a second stirring rod is arranged at the bottom of the connecting rod along the axial direction in an array mode.
According to the invention, the rotation of the rotating motor drives the rotation of the driving gear to drive the rotation of the driven gear, so that the connecting rod is driven to rotate, the stirring rod is enabled to stir at a high speed, in the stirring process, the hemispherical stirring blades stir in the ingredients, the hemispherical back forms a movable cavity in the rotating process, the ingredients form a movable vortex flow when filling the grooves, the contact reaction between the ingredients is more sufficient, the hemispherical stirring blades can well move in the fluid, the mechanical resistance is reduced, and the stirring is sufficient.
Preferably, the connecting rod is inside cavity, fixedly connected with intake pipe on the nitrogen gas air inlet of the jar body, the end fixedly connected with seal bearing of intake pipe, seal bearing's outer lane with intake pipe fixed connection, seal bearing's inner circle and the lateral wall fixed connection of connecting rod, the inside hollow structure that is of second puddler, the second puddler with the connecting rod switches on each other, every the venthole has all been seted up at the top of second puddler.
According to the invention, nitrogen is pumped into the connecting rod through the nitrogen inlet and then sprayed out from the air outlet, and oxygen cannot be completely removed easily because the density of the nitrogen is lower than that of the oxygen, and the oxygen can be completely removed through the mode of discharging from the air outlet, so that the alloy powder cannot be oxidized and burnt in the protection of the nitrogen.
Preferably, the top that the connecting rod is located the first puddler at top is equipped with keeps off material structure, keep off material structure including keeping off material cloth, outer bracing piece, interior bracing piece, first solid fixed ring, second solid fixed ring, electric putter, push pedal, first solid fixed ring and second solid fixed ring supreme and down overlap in proper order on the lateral wall of connecting rod, push pedal and first solid fixed ring slip establish on the connecting rod, push pedal and first solid fixed ring fixed connection, the second solid fixed ring is fixed on the connecting rod, there are a plurality of outer bracing piece along the circumferencial direction array of second solid fixed ring, outer bracing piece is articulated with the solid fixed ring of second, keep off the material and lay in the bottom of outer bracing piece, the one end of interior bracing piece with first solid fixed ring articulates, the other end is articulated with outer bracing piece, electric putter's motor end is fixed on the connecting rod, electric putter's push rod end and push pedal fixed connection.
According to the invention, the push plate pushes the first fixed ring downwards by pushing the electric push rod, so that the material blocking cloth is opened to be umbrella-shaped, the material at the bottom cannot splash above in the high-speed stirring process, and when the material needs to enter from the feed inlet, the electric push rod stretches and contracts, so that the first fixed ring is driven to move upwards, the material blocking cloth is folded, and the spread material blocking cloth is prevented from influencing the feed.
Preferably, the secondary stirring mechanism comprises a shell and a rotating shaft which can rotate in the shell, the right end of the rotating shaft is of a screw conveying structure, a first ball socket groove is formed in the left end of the rotating shaft, a second ball socket groove matched with the first ball socket groove is formed in the shell, and the length of R/2 is staggered between the first ball socket groove arranged on the rotating shaft and the adjacent second ball socket groove arranged on the second shell. The first ball socket groove and the second ball socket groove generate three-dimensional flow, and the materials are subjected to comprehensive actions such as shearing, stripping, coordination, kneading and the like, so that the materials are fully mixed.
The hydrogen breaking step adopts a hydrogen breaking device, the hydrogen breaking device comprises a frame, a lifting feeding mechanism, a hydrogen breaking furnace overturning mechanism, an M0M1 alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism, an M2H alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism, an M3Fe high-efficiency cooling hydrogen breaking furnace mechanism, an M0M1 alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism, an M2H alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism and a hydrogen breaking furnace transferring mechanism are sequentially arranged in the frame from left to right.
According to the invention, the reacted hydrogen breaking furnace is transferred to the hydrogen breaking furnace turnover mechanism through the hydrogen breaking furnace transfer mechanism, the hydrogen breaking furnace turnover mechanism turns the hydrogen breaking furnace from the horizontal direction to the vertical direction, the feed inlet of the hydrogen breaking furnace is upward, the discharge outlet is downward, the material is taken out through the discharge outlet, then the discharge outlet is closed, the feed inlet is opened, the material is conveyed to the upper part of the hydrogen breaking furnace turnover mechanism through the lifting feeding mechanism, the material falls into the hydrogen breaking furnace, and then the hydrogen breaking furnace is turned over, so that the hydrogen breaking furnace turns from the vertical direction to the horizontal direction, and then the hydrogen breaking furnace is transferred to the M0M1 alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism or the M2H alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism for heating, hydrogen breaking and cooling, so that the whole process is completed, the automation degree is high, and a plurality of hydrogen breaking furnaces can work simultaneously, and the working efficiency is improved.
Preferably, the high-efficient cooling hydrogen broken stove mechanism of M0M1 alloy melt-spun piece is including workstation, hydrogen broken stove body, heating furnace, bottom spray pipe, water catch bowl, side spray pipe, and hydrogen broken stove body passes through drive arrangement and can rotate, and drive arrangement can adopt the motor, and this is prior art through the furnace body rotation, therefore need not carry out in the case in detail, the workstation is established in the frame, the top at the workstation is placed in the horizontal lying of hydrogen broken stove body, the water catch bowl is established the bottom of hydrogen broken stove body and is fixed on the workstation, the bottom spray pipe is established on the water catch bowl, side spray pipe is located the both sides of hydrogen broken stove body, the heating furnace include with centre gripping in opposite directions the first half furnace body and the second half furnace body of hydrogen broken stove body, the bottom of first half furnace body and second half furnace body all is equipped with the slider, be equipped with the slide rail on the workstation, the slider is in slide on the slide rail, the one end of hydrogen broken stove body is connected with the device to vacuum in the hydrogen broken stove body, aerifys, and this is that the hydrogen is broken in the case, and the hydrogen can not carry out in the case in detail in the gas distribution device.
According to the invention, the first half furnace body and the second half furnace body are closed along the sliding rails like a hydrogen breaking furnace, the gas distribution device vacuumizes the hydrogen breaking furnace body and fills hydrogen, then the hydrogen breaking furnace rotates, the heating furnace heats the hydrogen breaking furnace, the gas distribution device dehydrogenates the hydrogen breaking furnace, then inert gas is injected into the furnace liner by the gas distribution device, the first half furnace body and the second half furnace body are separated and move along the respective sliding rails to be far away from the hydrogen breaking furnace, and then the bottom water spray pipe and the side water spray pipe spray water to the hydrogen breaking furnace, so that the spray area of the hydrogen breaking furnace is increased, and the high-efficiency full cooling is performed.
Preferably, the bottom of side spray pipe is equipped with the axis of rotation, the bottom of spray pipe runs through the axis of rotation, one side and the workstation of axis of rotation rotate to be connected, opposite side fixedly connected with upset motor, the motor end and the lateral wall fixed connection of workstation of upset motor, the workstation is located the bottom of slider and is equipped with the chamber that holds that can hold side spray pipe.
According to the invention, the rotation of the rotating shaft is controlled by the overturning motor, so that the side water spray pipe can be overturned to be in a vertical state for working when in use, and can be hidden in the accommodating cavity by overturning when not in use, thereby preventing the influence on the heating furnace.
Broken stove transfer mechanism of hydrogen is including establishing the roof in the workstation top, the bottom of roof is equipped with the transfer slide rail, the bottom of transfer slide rail is equipped with first slide, the bottom of slide is equipped with the distance adjustment slide rail, the sliding direction mutually perpendicular of distance adjustment slide rail and transfer slide rail, the bottom of distance adjustment slide rail is equipped with the second slide, the bottom of second slide is equipped with the lifting hook, two lifting hooks are located to correspond each other with the both ends of broken stove body of hydrogen, be equipped with lifting hook electric putter between lifting hook and the second slide, lifting hook electric putter's motor end and second slide fixed connection, lifting hook electric putter's push rod end and lifting hook fixed connection.
According to the invention, the lifting hook is moved to the side edge of the hydrogen breaking furnace through the distance adjusting slide rail, then the lifting hook electric push rod drives the lifting hook to move downwards, so that the lifting hook is positioned at the side edge of the neck opening of the hydrogen breaking furnace, then the lifting hook is moved through the distance adjusting slide rail, so that the lifting hook hooks the neck opening of the hydrogen breaking furnace, then the lifting hook electric push rod moves upwards, and then the lifting hook electric push rod moves to the hydrogen breaking furnace turnover mechanism or the M0M1 alloy melt-spun piece high-efficiency cooling hydrogen breaking furnace mechanism through the transferring slide rail, so that manual carrying is not needed, the hydrogen breaking furnaces of a plurality of stations can work simultaneously, and the working efficiency is improved.
Preferably, the turnover mechanism of the hydrogen breaking furnace comprises a first up-down sliding rail, a second up-down sliding rail, a first up-down sliding block, a first rotating motor, an electric push rod which is controlled to open and close, an annular clamp and a second rotating motor, wherein the first up-down sliding rail and the second up-down sliding rail are arranged on the side wall of the frame, the first up-down sliding rail and the second up-down sliding rail are oppositely arranged, the annular clamp is arranged between the first up-down sliding rail and the second up-down sliding rail, the annular clamp is composed of an upper semi-ring and a lower semi-ring, the output end of the first rotating motor is fixedly connected with the side wall of the lower semi-ring, the motor end of the first rotating motor is fixedly connected with the first up-down sliding block, the motor end of the electric push rod is fixedly connected with the output end of the second rotating motor, the motor end of the second rotating motor is slidingly arranged on the second up-down sliding rail, the push rod end of the electric push rod is provided with a rotating plate, and one end of the electric push rod is hinged with the side wall of the electric push rod.
According to the invention, the upper semi-ring is opened by controlling the opening and closing electric push rod to shorten, after the hydrogen breaking furnace moved by the hydrogen breaking furnace transferring mechanism is put in, the upper semi-ring and the lower semi-ring are combined by controlling the opening and closing electric push rod to clamp the hydrogen breaking furnace, then the upper semi-ring and the lower semi-ring are moved to a certain distance upwards by the sliding rail, the first rotating motor and the second rotating motor work simultaneously, the annular clamp is turned over, so that the hydrogen breaking furnace is in a vertical state, the later feeding and discharging are facilitated, after the feeding is completed, the first rotating motor and the second rotating motor are turned over to be in a horizontal state, the upper semi-ring is opened, the hydrogen breaking furnace transferring mechanism is used for lifting away the hydrogen breaking furnace, the later feeding and discharging are facilitated, and other hydrogen breaking furnaces can work when one hydrogen breaking furnace is used for feeding.
Preferably, the lifting feeding mechanism comprises a charging bucket horizontal movement sliding rail, an electric hoist and an electric hoist fixing plate, wherein the charging bucket horizontal movement sliding rail is arranged at the top of the frame, the charging bucket horizontal movement sliding rail is provided with two charging bucket horizontal movement sliding rails, the two charging bucket horizontal movement sliding rails are all arranged along the length direction of the frame, the electric hoist fixing plate is fixed on the charging bucket horizontal movement sliding rail, the electric hoist is arranged on the electric hoist fixing plate, and a mounting port which is convenient for lifting hooks of the electric hoist to move up and down is formed in the electric hoist fixing plate.
The bottom of frame is equipped with the delivery wagon, the delivery wagon is including two transport slide rails that are parallel to each other, it is equipped with the tray to slide on the transport slide rail, be fixed with the solid fixed ring on the tray, be equipped with the material jar in the solid fixed ring.
The charging bucket is including the open-top's jar body, the top of the jar body is equipped with the support frame, the shaping has the feed inlet on the support frame, the discharge gate has been seted up to the bottom of the jar body, be equipped with the bottom plate on the discharge gate, the diameter of bottom plate is greater than the diameter of discharge gate, the through-hole has been seted up at the middle part of support frame, be equipped with the slide bar in the through-hole, the bottom of slide bar extends to jar internal and bottom plate fixed connection, the top fixedly connected with charging bucket lifting hook of slide bar. The lower half part of the tank body is conical.
According to the invention, the tank body is placed on the fixed ring, the material is placed into the tank body through the feed inlet of the support frame, then the sliding rail is conveyed to the lower part of the frame, the electric hoist lifts the lifting hook of the tank, the sliding rail is horizontally moved to the upper part of the turnover mechanism of the hydrogen breaking furnace through the tank, then the lifting hook is fallen into the feed inlet of the hydrogen breaking furnace which is turned to the vertical direction, when the conical part of the tank is inserted into the feed inlet of the hydrogen breaking furnace, the electric hoist is continuously moved downwards, so that the bottom plate is opened, the material falls into the tank, then the electric hoist is moved upwards, the bottom of the tank body is closed, then the tank is horizontally moved along the sliding rail to return, and then the lifting hook is adjusted into the fixed ring, and finally the lifting feeding is completed through the conveying sliding rail to return, and manual feeding is not needed.
In summary, the invention has the following beneficial effects:
1. the alloy powder of three different structures and components is compounded, so that the diffusion channel is favorably optimized, the diffusion depth is improved, the effective utilization rate of the coating is improved, the microstructure of a base material is optimized, the anisotropism of the whole hard magnetic crystal grain is improved, the coercive force can be greatly improved under the use condition of less diffusion coating (heavy rare earth metal), and the residual magnetism is hardly reduced or reduced slightly.
2. The design and the use of the glue, the anti-sticking powder and the auxiliary agent not only ensure that the coating does not fall off after diffusion, but also well prevent the adhesion phenomenon between the magnetic sheets after heat treatment.
3. The high-performance diffusion coating of the invention ensures that the coercive force can be greatly improved under the use condition of less diffused rare earth metal by compounding the glue, the anti-adhesion powder and the auxiliary agent through controlling the components of the alloy powder and the granularity, the residual magnetism is hardly reduced or the residual magnetism is reduced slightly, and the phenomena of no falling of the coating and adhesion between magnetic sheets after diffusion are ensured.
4. According to the invention, nitrogen is pumped in through the nitrogen inlet, so that the tank body is in a nitrogen-protected environment, then the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder are subjected to high-speed dispersion stirring through the primary stirring mechanism, and after stirring, the mixture enters the secondary stirring mechanism through the discharge port to continue high-speed stirring, so that the dispersity and uniformity are improved, and the stirring efficiency is improved.
5. According to the invention, the push plate pushes the first fixed ring downwards by pushing the electric push rod, so that the material blocking cloth is opened to be umbrella-shaped, the material at the bottom cannot splash above in the high-speed stirring process, and when the material needs to enter from the feed inlet, the electric push rod stretches and contracts, so that the first fixed ring is driven to move upwards, the material blocking cloth is folded, and the spread material blocking cloth is prevented from influencing the feed.
Drawings
FIG. 1 is a graph comparing NdFeB performance of the present invention before diffusion and after diffusion in example 1;
FIG. 2 is a schematic cross-sectional view of the high speed stirring device of the present invention;
FIG. 3 is a schematic view of the striker mechanism of the present invention after being extended;
FIG. 4 is an enlarged schematic view of the present invention at A of FIG. 3;
FIG. 5 is a schematic cross-sectional view of a hemispherical stirring vane of the present invention;
FIG. 6 is a schematic perspective view of the striker mechanism of the present invention after being extended;
FIG. 7 is an overall schematic of the hydrogen fracturing unit of the present invention;
FIG. 8 is an overall schematic diagram of an efficient cooling hydrogen breaking mechanism for an M0M1 alloy melt-spun piece of the invention;
FIG. 9 is an overall schematic of the hydrogen destruction furnace turnover mechanism of the present invention;
FIG. 10 is a schematic perspective view of a bucket of the present invention;
fig. 11 is a schematic cross-sectional view of a bucket of the present invention.
Detailed Description
The following specific examples are intended to be illustrative of the invention and are not intended to be limiting, as modifications of the invention will be apparent to those skilled in the art upon reading the specification without inventive contribution thereto, and are intended to be protected by the patent law within the scope of the appended claims.
The invention is described in detail below with reference to the accompanying drawings.
Example 1
A preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
s2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely dispersing the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder for 30min under the condition of nitrogen protection and oxygen content less than or equal to 0.005% under the stirring condition of a high-speed dispersing machine of 1000rpm, taking out from the nitrogen protection environment, and continuously stirring for 2h under the condition of 1500rpm by adopting the high-speed dispersing machine to prepare the diffusion coating.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
The alloy powder is prepared by smelting, hydrogen breaking and air flow grinding processes, and the grain sizes of M0M1 and M2H, M Fe are controlled to be 0.5 mu M, 1 mu M and 0.5 mu M respectively through smelting, hydrogen breaking and air flow grinding.
The mass percentages of the M0M1, the M2H, M Fe three alloy powders are respectively 20 percent 5 percent, 35 percent and 15 percent.
The resin is mainly selected from polyvinyl butyral, and the solvent is mainly terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate, or 1 or more combinations of propylene glycol butyl ether acetate.
The viscosity of the resin is controlled to be 2 seconds, and the mass percentage of the resin in the glue is 60%.
The auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-epoxypropoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
The anti-adhesion powder is used for preventing the adhesion between the neodymium iron boron magnetic sheets in the high-temperature heat treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the particle size is controlled within 80 mu m.
The mass percent of the diffusion coating and the composite alloy powder is 60%, the mass percent of the glue is 13%, the mass percent of the auxiliary agent is controlled to be 0.5%, and the mass percent of the anti-adhesion powder is controlled to be 2%.
A diffusion treatment method of high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate for 15 minutes at the temperature of 80 ℃, cooling to room temperature and discharging.
(4) And (3) heat treatment: tempering the sintered NdFeB substrate after surface drying at 850 ℃ for 5 hours, cooling to room temperature, tempering at 450 ℃ for 5 hours, cooling to room temperature, discharging, and completing diffusion treatment.
Example 2
A preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
S2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely dispersing the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder for 20min under the condition of nitrogen protection and oxygen content less than or equal to 0.005% under the stirring condition of 1500rpm of a high-speed dispersing machine, taking out from the nitrogen protection environment, and continuously stirring for 1h under the condition of 2000rpm by adopting the high-speed dispersing machine to prepare the diffusion coating.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
The alloy powder is prepared by smelting, hydrogen breaking and air flow grinding processes, and the grain sizes of M0M1 and M2H, M Fe are controlled to be 1 mu M, 3 mu M and 1.5 mu M respectively through smelting, hydrogen breaking and air flow grinding.
The mass percentages of the M0M1 and the M2H, M Fe alloy powder are 45%, 50% and 20% respectively.
The resin is mainly selected from polyethylene glycol, and the solvent is mainly selected from 1 or more of terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and propylene glycol butyl ether acetate.
The viscosity of the resin is controlled to be 10 seconds, and the mass percentage of the resin in the glue is 85%.
The auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-epoxypropoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
The anti-adhesion powder is used for preventing the adhesion between the neodymium iron boron magnetic sheets in the high-temperature heat treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the grain diameter is controlled within 120 mu m.
The mass percent of the diffusion coating and the composite alloy powder is 85%, the mass percent of the glue is 35%, the mass percent of the auxiliary agent is controlled to be 1.5%, and the mass percent of the anti-adhesion powder is controlled to be 5%.
A diffusion treatment method of high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate at 130 ℃ for 45 minutes, cooling to room temperature and discharging.
(4) And (3) heat treatment: and tempering the surface-dried sintered NdFeB substrate for 35h at 950 ℃, cooling to room temperature, tempering for 10h at 680 ℃, cooling to room temperature, discharging, and finishing the diffusion treatment.
Example 3
A preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
s2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely dispersing the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder for 25 minutes under the condition of nitrogen protection and oxygen content less than or equal to 0.005% under the stirring condition of 1250rpm of a high-speed dispersing machine, taking out from the nitrogen protection environment, and continuously stirring for 1.5 hours under the condition of 1750rpm by adopting the high-speed dispersing machine to prepare the diffusion coating.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
The alloy powder is prepared by smelting, hydrogen breaking and air flow grinding processes in sequence, and the grain sizes of M0M1 and M2H, M Fe are respectively controlled by the smelting, hydrogen breaking and air flow grinding processes. 0.7 μm, 2 μm, 1 μm.
The mass percentages of the M0M1 and the M2H, M Fe alloy powder are 33%, 43% and 17%, respectively.
The resin is mainly selected from polyvinyl pyrrolidone, and the solvent is mainly terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate, or 1 or more combinations of propylene glycol butyl ether acetate.
The viscosity of the resin is controlled to be 6 seconds, and the mass percentage of the resin in the glue is 73%.
The auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-epoxypropoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
The anti-adhesion powder is used for preventing the adhesion between the neodymium iron boron magnetic sheets in the high-temperature heat treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the grain size is controlled within 100 mu m.
The diffusion coating comprises 73% of composite alloy powder by mass, 24% of glue by mass, 1% of auxiliary agent by mass and 3.5% of anti-adhesion powder by mass.
A diffusion treatment method of high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate for 30 minutes at 105 ℃, cooling to room temperature and discharging.
(4) And (3) heat treatment: and tempering the sintered NdFeB substrate after surface drying at 900 ℃ for 20 hours, cooling to room temperature, tempering at 565 ℃ for 7.5 hours, cooling to room temperature, discharging, and finishing diffusion treatment.
Example 4
A preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
S2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely under the protection of inert gas, dispersing and stirring the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder at a high speed for 15min by a high-speed stirring device, and then taking out the mixture from the inert gas protection environment, and continuing to stir at a high speed for 0.5h by a secondary stirring mechanism to prepare the diffusion coating.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
The alloy powder is prepared by smelting, hydrogen breaking and air flow grinding processes, and the grain sizes of M0M1 and M2H, M Fe are controlled to be 0.5 mu M, 1 mu M and 0.5 mu M respectively through smelting, hydrogen breaking and air flow grinding.
The mass percentages of the M0M1, the M2H, M Fe three alloy powders are respectively 20 percent 5 percent, 35 percent and 15 percent.
The resin is mainly selected from polyvinyl alcohol, and the solvent is mainly selected from 1 or more of terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and propylene glycol butyl ether acetate.
The viscosity of the resin is controlled to be 2 seconds, and the mass percentage of the resin in the glue is 60%.
The auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-epoxypropoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
The anti-adhesion powder is used for preventing the adhesion between the neodymium iron boron magnetic sheets in the high-temperature heat treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the particle size is controlled within 80 mu m.
The diffusion coating comprises 60% of composite alloy powder by mass, 13% of glue by mass, 0.5% of auxiliary agent by mass and 2% of anti-adhesion powder by mass.
A diffusion treatment method of high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate for 15 minutes at the temperature of 80 ℃, cooling to room temperature and discharging.
(4) And (3) heat treatment: tempering the sintered NdFeB substrate after surface drying at 850 ℃ for 5 hours, cooling to room temperature, tempering at 450 ℃ for 5 hours, cooling to room temperature, discharging, and completing diffusion treatment.
As shown in fig. 2-5, the preparation of the diffusion coating adopts a high-speed stirring device, the high-speed stirring device comprises a tank body 1, a primary stirring mechanism 2, a secondary stirring mechanism 3 and a discharge valve 4, the top of the tank body 1 is provided with a nitrogen gas inlet 11, a feeding hole 12 and a gas outlet 13, the bottom of the protected tank body 1 is provided with a discharge hole 14, the discharge valve 4 is arranged on the discharge hole 14, the primary stirring mechanism 2 is arranged in the tank body 1, and the secondary stirring mechanism 3 is arranged at the discharge hole of the discharge valve 5.
The primary stirring mechanism 2 comprises a connecting rod 21, a driving gear 22, a driven gear 23 and a rotating motor 24, wherein the rotating motor 24 is arranged outside the tank body 1, the output end of the rotating motor 24 penetrates through the tank body 1 and extends to the inside of the tank body 1, the driving gear 22 is arranged on the output end of the rotating motor 24, the driven gear 23 is arranged on the outer side wall of a connecting rod 21, the driving gear 22 and the driven gear 23 are meshed with each other, a first stirring rod 25 arranged in multiple layers is arranged on the side wall of the connecting rod 21, hemispherical stirring blades 26 are formed at the tail end of one stirring rod 25, grooves 261 are formed in the hemispherical stirring blades 26, a second stirring rod 27 is arranged at the bottom of the connecting rod 21 in an array along the axial direction, the connecting rod 21 is hollow, an air inlet pipe 27 is fixedly connected to the nitrogen inlet 11 of the tank body 1, a sealing bearing 271 is fixedly connected at the tail end of the air inlet 27, the outer ring of the sealing bearing 271 is fixedly connected with the air inlet pipe 27, the inner ring of the sealing bearing 271 is fixedly connected with the outer side wall of the connecting rod 21, the second stirring rod 27 is of a hollow structure, the second stirring rod 27 is mutually communicated with the connecting rod 25, and the top of each second stirring rod 27 is provided with the air outlet 271.
As shown in fig. 5, a blocking structure 28 is arranged above the first stirring rod 25 at the top of the connecting rod 21, the blocking structure 28 comprises a blocking cloth 281, an outer supporting rod 282, an inner supporting rod 283, a first fixing ring 284, a second fixing ring 285, an electric push rod 286 and a push plate 287, the first fixing ring 281 and the second fixing ring 285 are sequentially sleeved on the outer side wall of the connecting rod 21 from top to bottom, the push plate 287 and the first fixing ring 284 are slidably arranged on the connecting rod 21, the push plate 287 and the first fixing ring 284 are fixedly connected, the second fixing ring 285 is fixedly arranged on the connecting rod 21, a plurality of outer supporting rods 282 are arrayed along the circumferential direction of the second fixing ring 285, the outer supporting rod 282 is hinged with the second fixing ring 285, the blocking cloth 281 is arranged at the bottom of the outer supporting rod 282, one end of the inner supporting rod 283 is hinged with the first fixing ring 284, the other end is hinged with the outer supporting rod 282, the motor end of the electric push rod 286 is fixedly arranged on the connecting rod 21, and the push rod end of the electric push rod 286 is fixedly connected with the push plate.
As shown in fig. 2, the secondary stirring mechanism 3 includes a housing 31 and a rotating shaft 32 rotatable in the housing 31, wherein the right end of the rotating shaft 32 is a screw conveying structure, a first ball socket groove 33 is formed at the left end of the rotating shaft 32, a second ball socket groove 34 matched with the first ball socket groove 33 is formed in the housing 31, and the first ball socket groove 33 arranged on the rotating shaft 32 is staggered by R/2 length with the second ball socket groove 34 arranged on the adjacent second housing.
Working principle: when the stirring device is used, as shown in fig. 1-6, nitrogen is pumped into the connecting rod 21 through the nitrogen inlet 11 and then sprayed out of the air outlet 271 of the second stirring rod 27 at the bottom, then materials enter from the feeding port, the rotation of the rotating motor 24 drives the rotation of the driving gear 22 to drive the rotation of the driven gear 23, thereby driving the connecting rod 21 to rotate, the stirring rod is enabled to stir at a high speed, in the stirring process, the hemispherical stirring blades 26 are used for stirring in the ingredients, the hemispherical back forms a movable cavity in the rotating process, the ingredients form a movable vortex flow when filling the grooves, so that the contact reaction between the ingredients is more sufficient, the hemispherical stirring blades can well move in fluid, the mechanical resistance is reduced, the stirring is sufficient, after the stirring is finished, the materials enter into the secondary stirring mechanism 3 through the air outlet, and three-dimensional flow is generated through the first ball socket groove and the second ball socket groove, and the materials are subjected to comprehensive actions of shearing, stripping, coordination, kneading and the like, so that the materials are sufficiently mixed, and the preparation of the diffusion coating is completed, and the stirring efficiency is improved.
From the above table, it is clear that the time required to complete the stirring is the shortest by using the high-speed stirring device.
Example 5
A preparation method of a high-performance sintered NdFeB diffusion coating comprises the following steps:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
s2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely under the protection of inert gas, dispersing and stirring the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder at a high speed for 15min by a high-speed stirring device, and then taking out the mixture from the inert gas protection environment, and continuing to stir at a high speed for 0.5h by a secondary stirring mechanism to prepare the diffusion coating.
Three types of alloy powders, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
The alloy powder is prepared by smelting, hydrogen breaking and air flow grinding processes, and the grain sizes of M0M1 and M2H, M Fe are controlled to be 0.5 mu M, 1 mu M and 0.5 mu M respectively through smelting, hydrogen breaking and air flow grinding.
The mass percentages of the M0M1, the M2H, M Fe three alloy powders are respectively 20 percent 5 percent, 35 percent and 15 percent.
The resin is mainly selected from polyvinyl alcohol, and the solvent is mainly selected from 1 or more of terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and propylene glycol butyl ether acetate.
The viscosity of the resin is controlled to be 2 seconds, and the mass percentage of the resin in the glue is 60%.
The auxiliary agent is mainly selected from 1 or more combinations of gamma- (2, 3-epoxypropoxy), propyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
The anti-adhesion powder is used for preventing the adhesion between the neodymium iron boron magnetic sheets in the high-temperature heat treatment process, and is mainly one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the particle size is controlled within 80 mu m.
The diffusion coating comprises 60% of composite alloy powder by mass, 13% of glue by mass, 0.5% of auxiliary agent by mass and 2% of anti-adhesion powder by mass.
A diffusion treatment method of high-performance sintered NdFeB diffusion coating comprises the following steps:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: and leveling and drying the sprayed sintered NdFeB substrate for 15 minutes at the temperature of 80 ℃, cooling to room temperature and discharging.
(4) And (3) heat treatment: tempering the sintered NdFeB substrate after surface drying at 850 ℃ for 5 hours, cooling to room temperature, tempering at 450 ℃ for 5 hours, cooling to room temperature, discharging, and completing diffusion treatment.
As shown in fig. 7, the hydrogen breaking step adopts a hydrogen breaking device 7, the hydrogen breaking device 7 comprises a frame 70, a lifting feeding mechanism 72, a hydrogen breaking overturning mechanism 74, an M0M1 alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 71, an M2H alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 75, an M3Fe high-efficiency cooling hydrogen breaking mechanism 76, an M0M1 alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 71, a M2H alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 75, a hydrogen breaking transferring mechanism 73 is arranged above the M3Fe high-efficiency cooling hydrogen breaking mechanism 76, the M2H alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 75, the M3Fe high-efficiency cooling hydrogen breaking mechanism 76 and the M0M1 alloy strip-casting sheet high-efficiency cooling hydrogen breaking mechanism 71 have the same structure, the M0M1 alloy strip casting sheet high-efficiency cooling hydrogen breaking mechanism 71 comprises a workbench 711, a hydrogen breaking furnace body 712, a heating furnace 713, a bottom spray pipe 714, a water collecting tank 715 and a side spray pipe 716, wherein the workbench 711 is arranged on a frame 70, the hydrogen breaking furnace body 712 is horizontally placed at the top of the workbench 711, the water collecting tank 715 is arranged at the bottom of the hydrogen breaking furnace body 712 and is fixed on the workbench 711, the bottom spray pipe 714 is arranged on the water collecting tank 715, the side spray pipe 716 is positioned at two sides of the hydrogen breaking furnace body 712, the heating furnace 713 comprises a first half furnace body 717 and a second half furnace body 718 which are used for clamping the hydrogen breaking furnace body 712 in opposite directions, sliding blocks 719 are arranged at the bottoms of the first half furnace body 717 and the second half furnace body 718, sliding rails 720 are arranged on the workbench 711, and the sliding blocks 719 slide on the sliding rails 720 are provided with water outlets.
As shown in fig. 8, the bottom of the side spray pipe 716 is provided with a rotating shaft 72, the bottom of the spray pipe 716 penetrates through the rotating shaft 72, one side of the rotating shaft 72 is rotationally connected with a workbench 711, the other side is fixedly connected with a turnover motor 721, the motor end of the turnover motor 721 is fixedly connected with the side wall of the workbench 711, the bottom of the workbench 711, which is positioned at the sliding block 719, is provided with a containing cavity 722 capable of containing the side spray pipe 716, the side spray pipe is provided with more than three side spray pipes in an array on the rotating shaft, the bottom of the side spray pipe is connected with a hose, the turnover is facilitated, the side spray pipe is close to one side of the hydrogen breaking furnace, and a water spray hole is formed in the upper part of the bottom spray pipe.
As shown in fig. 7, the hydrogen breaking furnace transferring mechanism 73 includes a top plate 731 disposed above the workbench, a transferring slide rail 732 is disposed at the bottom of the top plate 731, a first slide plate 733 is disposed at the bottom of the transferring slide rail 732, a distance adjusting slide rail 735 is disposed at the bottom of the slide plate 733, the distance adjusting slide rail 735 is perpendicular to the sliding direction of the transferring slide rail 732, a second slide plate 736 is disposed at the bottom of the distance adjusting slide rail 735, hooks 734 are disposed at the bottom of the second slide plate 736, two hooks 734 are disposed at two ends of the hydrogen breaking furnace body 712 and correspond to each other, a hook electric push rod 737 is disposed between the hooks 734 and the second slide plate 736, a motor end of the hook electric push rod 737 is fixedly connected with the second slide plate 736, and a push rod end of the hook electric push rod 737 is fixedly connected with the hooks 734.
As shown in fig. 10, the turnover mechanism 74 for a hydrogen breaking furnace comprises a first up-down sliding rail 741, a second up-down sliding rail 742, a first up-down sliding block 743, a first rotating motor 745, an electric control opening-closing rod 747, an annular clamp 747, and a second rotating motor 748, wherein the first up-down sliding rail 741 and the second up-down sliding rail 742 are disposed on a side wall of the frame 70, the first up-down sliding rail 741 and the second up-down sliding rail 742 are disposed opposite to each other, the annular clamp 747 is disposed between the first up-down sliding rail 741 and the second up-down sliding rail 742, the annular clamp 747 is composed of an upper half ring 740 and a lower half ring 749, an output end of the first rotating motor 745 is fixedly connected with a side wall of the lower half ring 749, a motor end of the first rotating motor 745 is fixedly connected with the first up-down sliding block 743, a motor end of the electric control opening-closing rod is fixedly connected with an output end of the second rotating motor 74748, a motor end of the electric control opening-closing rod 746 is fixedly connected with an output end of the second rotating motor 74748, an electric control opening-closing rod is disposed at an upper end of the electric control opening-closing rod 7461 is fixedly connected with the other end of the electric control opening-closing rod 749, and the electric control opening-closing rod 749 is arranged at the upper end of the upper half ring 7461 is.
As shown in fig. 10-11, the lifting and feeding mechanism 72 comprises a horizontal moving slide rail 721 of a charging tank, an electric hoist 722 and an electric hoist fixing plate 723, the horizontal moving slide rail 721 of the charging tank is arranged at the top of the frame 70, the horizontal moving slide rails 721 of the charging tank are arranged in two, the horizontal moving slide rails 721 of the charging tank are all arranged along the length direction of the frame 70, the electric hoist fixing plate 723 is fixed on the horizontal moving slide rail 721 of the charging tank, the electric hoist 722 is arranged on the electric hoist fixing plate 723, a mounting hole 724 which is convenient for lifting hooks of the electric hoist 722 to move up and down is formed in the electric hoist fixing plate 723, a conveying trolley 77 is arranged at the bottom of the frame 70, the conveying trolley 77 comprises two conveying slide rails 771 which are parallel to each other, a tray 772 is arranged on the conveying slide rail 771 in a sliding manner, a fixing ring 773 is fixed on the tray 772, a supporting frame 774 is arranged in the fixing ring 773, a supporting frame 774 is arranged at the top of the charging tank 775, a forming bottom plate 775 is provided with a lifting hook 776, and the bottom plate 778 is connected with a bottom plate 776, and the bottom plate 776 is provided with a discharge hole 776. The lower half of the canister 775 is tapered.
Working principle: as shown in fig. 7-11, the present invention opens the upper half ring 740 by controlling the opening and closing electric push rod 746 to be short, after the hydrogen breaking furnace moved by the hydrogen breaking furnace transferring mechanism is put in, the upper half ring 740 and the lower half ring 749 are combined by controlling the opening and closing electric push rod 746 to extend upward, so as to clamp the hydrogen breaking furnace, then the first rotary motor 745 and the second rotary motor 748 are operated at the same time by moving the slide rail upward to a certain distance, the ring clamp 747 is turned over, so that the hydrogen breaking furnace is in a vertical state, then the feed inlet is opened manually, then the slide rail 771 is conveyed to the lower part of the frame 70, the electric hoist 722 lifts the bucket lifting hook 779 by moving the slide rail 721 horizontally to the upper part of the hydrogen breaking furnace turning mechanism, then drops into the feed inlet of the hydrogen breaking furnace turned over in a vertical direction, the electric hoist 722 continues to move downwards so as to open the bottom plate 776, so that materials fall into the charging bucket, then the electric hoist 722 moves upwards to seal the bottom of the tank body, then the charging bucket 774 moves back along the charging bucket horizontal movement sliding rail, then is adjusted into the fixed ring, then returns through the conveying sliding rail, lifting charging is completed, manual charging is not needed, after charging is completed, the upper semi-ring is opened by overturning through the first rotating motor 745 and the second rotating motor 748 to be in a horizontal state, the hydrogen breaking furnace transferring mechanism lifts away the hydrogen breaking furnace, moves to the upper part of one M0M1 alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism, then falls onto the workbench of the M0M1 alloy strip throwing piece high-efficiency cooling hydrogen breaking furnace mechanism, the first half furnace body 717 and the second half furnace 718 draw close to the hydrogen breaking furnace along the sliding rail to form a closed gas distribution device, the hydrogen breaking furnace body is vacuumized and filled with hydrogen, heating furnace heats, distribution device carries out dehydrogenation to it, then, distribution device is in the inert gas of rushing into in to the stove courage, afterwards, first half furnace body 717 and second half furnace body 718 separation, remove along respective slide rail and keep away from broken stove of hydrogen, afterwards, bottom spray pipe and side spray pipe all spray water to broken stove of hydrogen, after the cooling, the rotation of upset motor control axis of rotation is hidden in holding the intracavity, broken stove tilting mechanism of broken stove of hydrogen with broken stove of hydrogen transfer mechanism, repeat above-mentioned work, whole process, degree of automation is high, simultaneously can a plurality of broken stoves of hydrogen simultaneous working, improve work efficiency.
When the M0M1 alloy strip casting sheet high-efficiency cooling hydrogen furnace breaking mechanism works, the hydrogen furnace breaking transfer mechanism moves the hydrogen furnace breaking of the M2H alloy strip casting sheet high-efficiency cooling hydrogen furnace breaking mechanism 75 to the hydrogen furnace breaking turnover mechanism for feeding, and when the M2H alloy strip casting sheet high-efficiency cooling hydrogen furnace breaking mechanism works, the M3Fe high-efficiency cooling hydrogen furnace breaking mechanism moves to the hydrogen furnace breaking turnover mechanism for feeding, and always circularly works, so that the three high-efficiency cooling hydrogen furnace breaking mechanisms can adopt one feeding mechanism, and the efficiency is improved.
Claims (10)
1. The preparation method of the high-performance sintered NdFeB diffusion coating is characterized by comprising the following steps of:
s1, preparing alloy powder, namely compounding three alloy powders of M0M1 and M2H, M Fe to obtain composite alloy powder;
s2, preparing glue, namely completely dissolving resin in a solvent under the condition of mechanical stirring to prepare the glue;
s3, preparing the diffusion coating, namely dispersing and stirring the composite alloy powder, the glue, the auxiliary agent and the anti-adhesion powder at a high speed under the protection of inert gas, and then taking out the mixture from the environment protected by the inert gas, continuing stirring at a high speed, and finishing the preparation of the diffusion coating.
2. The method for preparing a high performance sintered neodymium iron boron diffusion coating according to claim 1, wherein three types of alloy powder are used, wherein M0 is 1 or 2 combinations of Pr or Nd; m1 is a combination of 1 or more of Co, ni, al, cu, zn, ga, mo; m2 in M2H is 1 or 2 combinations of Dy or Tb, and H is hydrogen; in M3Fe, M3 is 1 or more combinations of Gd, ho, la, ce.
3. The preparation method of the high-performance sintered NdFeB diffusion coating according to claim 1, wherein the mass percentages of the three alloy powders M0M1 and M2H, M Fe are 20-45%, 35-50% and 15-20%, respectively; the composite alloy powder is prepared by compounding three alloy powders of M0M1 and M2H, M Fe, and the grain sizes of M0M1 and M2H, M Fe are respectively controlled to be 0.5-1 mu M, 1-3 mu M and 0.5-1.5 mu M through smelting, hydrogen breaking and jet milling.
4. The preparation method of the high-performance sintered NdFeB diffusion coating according to claim 1, wherein the diffusion coating comprises, by mass, 60-85% of composite alloy powder, 13-35% of glue, 0.5% -1.5% of auxiliary agent and 2% -5% of anti-adhesion powder.
5. The method for preparing the high-performance sintered neodymium-iron-boron diffusion coating according to claim 1, wherein the resin in the step S2 is mainly selected from polyvinyl butyral, polyethylene glycol, polyvinyl alcohol and polyvinyl pyrrolidone, and the solvent is mainly selected from terpineol, n-butanol, propylene glycol methyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and 1 or more combinations of propylene glycol butyl ether acetate.
6. The method for preparing the high-performance sintered NdFeB diffusion coating according to claim 1, wherein the viscosity of the resin in the step S2 is controlled to be 2-10 seconds, and the mass percentage of the resin is 60% -85%.
7. The method for preparing the high-performance sintered neodymium-iron-boron diffusion coating according to claim 1, wherein the auxiliary agent of S3 is mainly selected from 1 or more combinations of gamma- (2, 3-glycidoxy), propyl trimethoxysilane 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl trimethoxysilane and N-phenyl-3-aminopropyl trimethoxysilane.
8. The method for preparing high-performance sintered neodymium-iron-boron diffusion coating according to claim 1, wherein the anti-adhesion powder in the step S3 is one or more of aluminum oxide, silicon carbide, barium sulfate, titanium oxide and titanium nitride, and the particle size is controlled within 80-120 μm, wherein the anti-adhesion powder is used for preventing adhesion between neodymium-iron-boron magnetic sheets in the high-temperature heat treatment process.
9. The preparation method of the high-performance sintered NdFeB diffusion coating according to claim 1 is characterized in that a high-speed stirring device is adopted for preparing the diffusion coating, the high-speed stirring device comprises a tank body (1), a primary stirring mechanism (2), a secondary stirring mechanism (3) and a discharge valve (4), a nitrogen gas inlet (11), a feed inlet (12) and a gas outlet (13) are formed in the top of the tank body (1), a discharge hole (14) is formed in the bottom of the protected tank body (1), the discharge valve (4) is arranged on the discharge hole (14), the primary stirring mechanism (2) is arranged in the tank body (1), and the secondary stirring mechanism (3) is arranged at the discharge hole of the discharge valve (5);
The utility model provides a stirring mechanism (2) including connecting rod (21), driving gear (22), driven gear (23), rotating electrical machines (24) are established outside jar body (1), the output of rotating electrical machines (24) runs through jar body (1) extends to the inside of jar body (1), driving gear (22) are established on the output of rotating electrical machines (24), driven gear (23) are established on the lateral wall of connecting (21) pole, driving gear (22) and driven gear (23) intermeshing, be equipped with first puddler (25) of multilayer setting on the lateral wall of connecting rod (21), the end shaping of a puddler (25) has hemisphere stirring vane (26), set up flutedly (261) on hemisphere stirring vane (26), the bottom of connecting rod (21) is provided with second puddler (27) along the array in axial direction.
10. A diffusion treatment method of a diffusion coating prepared by the preparation method of a high-performance sintered neodymium iron boron diffusion coating according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) Pretreatment: performing ultrasonic degreasing, water washing, ultrasonic water-based, acid washing, water washing, pure water washing and ethanol washing treatment on the sintered NdFeB substrate, and then performing water washing and drying to clean the surface of the sintered NdFeB substrate;
(2) Coating: placing the treated sintered NdFeB substrate on a jig, and coating the diffusion coating on the surface of the sintered NdFeB substrate in a spraying or brushing or rolling way;
(3) Surface drying: leveling and drying the sprayed sintered NdFeB substrate at 80-130 ℃ for 15-45 minutes, cooling to room temperature and discharging;
(4) And (3) heat treatment: tempering the sintered NdFeB substrate after surface drying at 850-950 ℃ for 5-35h, cooling to room temperature, tempering at 450-680 ℃ for 5-10h, cooling to room temperature, discharging, and finishing diffusion treatment.
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| CN202311279167.1A CN117165117A (en) | 2023-10-07 | 2023-10-07 | Preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating |
| JP2024534235A JP2025537049A (en) | 2023-10-07 | 2023-12-28 | Manufacturing method and diffusion treatment method for high-performance sintered neodymium iron boron diffusion paint |
| PCT/CN2023/142573 WO2025073152A1 (en) | 2023-10-07 | 2023-12-28 | Preparation and diffusion treatment method for high-performance diffusion coating used for sintered neodymium-iron-boron magnet |
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| CN202311279167.1A CN117165117A (en) | 2023-10-07 | 2023-10-07 | Preparation and diffusion treatment method of a high-performance sintered NdFeB diffusion coating |
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| CN120236883B (en) * | 2025-05-30 | 2025-09-12 | 江西荧光磁业有限公司 | A high-strength NdFeB magnetic material and its preparation method |
| CN120768068B (en) * | 2025-09-11 | 2025-11-21 | 江西荧光磁业有限公司 | Bonding jig and bonding method for neodymium iron boron magnetic steel |
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| WO2025073152A1 (en) | 2025-04-10 |
| JP2025537049A (en) | 2025-11-14 |
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