CN116165036B - A method for preparing ultrafine metal powder cross-section specimen - Google Patents
A method for preparing ultrafine metal powder cross-section specimenInfo
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- CN116165036B CN116165036B CN202211643730.4A CN202211643730A CN116165036B CN 116165036 B CN116165036 B CN 116165036B CN 202211643730 A CN202211643730 A CN 202211643730A CN 116165036 B CN116165036 B CN 116165036B
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention provides a preparation method of a superfine metal powder section sample, belongs to the technical field of metallographic structure inspection, and aims to solve the technical problems that powder adhesion fastness is low, falling is easy, and dynamic hardness measurement is biased in the superfine metal powder section sample prepared by the existing method. The method comprises the steps of dispersing metal superfine powder in a dispersing agent to obtain a dispersion liquid, dripping the dispersion liquid on a carrying platform, drying to disperse the metal superfine powder on the carrying platform, adopting an electric soldering iron to heat a welding wire to carry out drip welding on the metal superfine powder dispersed on the carrying platform, then pressing the welding drip into welding blocks, inlaying the welding blocks by a thermal inlaying process to obtain an inlaid sample, and polishing the inlaid sample to obtain the superfine metal powder section sample. The sample powder prepared by the invention has low shedding rate, uniform powder dispersion and high phase contrast, can be used for observing microstructure in powder, and can be used for measuring dynamic hardness of the powder.
Description
Technical Field
The invention belongs to the technical field of metallographic structure inspection, and particularly relates to a preparation method of a superfine metal powder section sample.
Background
The metal bond diamond grinding tool has the advantages of strong abrasive grain bonding capability, good toughness, high bearing property, low price of raw materials, stable production process, high forming rate and the like, is suitable for manufacturing various products with complex shapes, and is widely applied to the fields of forming grinding, precision and ultra-precision grinding of complex profiles of brittle and hard materials. The metal bond diamond tool is consumed in a far greater amount than the diamond tool of the resin bond and the ceramic bond, which plays an irreplaceable role in the diamond tool. The copper-based bonding agent system is one of main metal bonding agent systems, the copper-tin bonding agent is the most common copper-based bonding agent, and the copper-tin bonding agent has good heat conductivity, can reduce grinding temperature and prevent surface burn, and is mostly applied to the fields of diamond grinding tools, stone cutting saw blades and the like.
The performance of the alloy powder as a core key raw material directly influences the quality of the metal bond superhard grinding tool. Therefore, observation of the powder structure and hardness measurement become extremely important. If a block metallographic mosaic sample preparation method is adopted, fine particle metal powder is extremely difficult to fix firmly through thermosetting resin mosaic, because the interface binding force of metal and an organic mosaic material is usually weak, the smaller the mosaic metal sample is, the larger the specific surface area is, and the more interface weak areas are, the more easily the mosaic metal sample is dropped. Therefore, a metal powder with an extremely large specific surface area cannot obtain a firm and reliable metallographic sample by a traditional thermosetting inlaying method. The method for embedding the metal superfine powder with firm particle fixation and high lining degree can enable the dynamic hardness measurement and the microstructure observation of the powder to be more accurate and convenient, and can provide guidance for the production of copper-tin alloy by researching the change rule of the mechanical properties of different particle sizes of the powder through the observation of the phase content and distribution in the microstructure of the powder and the dynamic hardness difference of different particle sizes. Therefore, the method for preparing the superfine metal powder section sample for dynamic hardness measurement has certain engineering value and practical significance.
At present, two powder embedding methods are mainly adopted, and patent publication No. CN202210321829 describes a preparation method of a ceramic powder section embedding sample, wherein ceramic powder and tin powder are added into deionized water for mixing, then ultrasonic oscillation is carried out, and drying and pressing are carried out, but the method is not suitable for metal alloy powder due to higher hardness of the metal alloy powder. The patent with the publication number of CN20190764739 describes a display method of a microstructure of a section of fine powder, wherein the fine powder and the hot inlaid powder are mixed and then are prepared and polished, but the method is simple in method, the powder falling rate is high, certain requirements are imposed on the particle size of the powder, the powder utilization rate is low, and the firmness of bonding and the related inlaid powder can influence the dynamic hardness.
Disclosure of Invention
Aiming at the technical problems that the powder adhesion fastness is low, the powder is easy to fall off and the dynamic hardness measurement is biased in the superfine metal powder section sample prepared by the existing method, the invention provides the preparation method of the superfine metal powder section sample.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
The preparation method of the superfine metal powder section sample mainly comprises the following steps:
step 1, selecting metal superfine powder, namely selecting low-melting-point welding wires, wherein the metal superfine powder is metal powder such as copper powder, copper-tin alloy powder or high-entropy alloy powder.
Step 1.1, the preparation method of the metal superfine powder comprises the steps of atomizing to prepare powder, wherein the particle size of the powder is less than 60 mu m.
Step 1.2, the selected welding wire has the hardness close to that of the superfine metal powder and good wettability, preferably a lead-tin welding wire, wherein the mass fraction of lead is 33%, the mass fraction of tin is 67%, or an Ag-Sn welding wire.
Step 2, cleaning and dispersing the metal superfine powder by using an ultrasonic resonance dispersing instrument;
And 2.1, dispersing agent used in the cleaning and dispersing process is ethanol, propanol or acetone, the dispersing time of an ultrasonic resonance dispersing instrument is 3-5min, so as to obtain dispersion liquid, dispersing liquid is dripped on a carrying platform, the dispersing agent is dried, and the dried metal superfine powder is dispersed on the carrying platform, wherein the carrying platform is a glass slide.
The concentration of the metal superfine powder in the dispersion liquid is 0.1-0.5 g.mL -1.
Step 3, heating the welding wire by using an electric soldering iron, performing drip welding on the dispersed metal superfine powder, dripping molten welding drip on the metal superfine powder to enable the metal superfine powder to be adhered and embedded on the surface of the welding drip, and then pressing the drip welded metal superfine powder;
And 3.1, paying attention to the consumption and the position of a welding drop in the process of drop welding, selecting the position with higher dispersity of the metal superfine powder as much as possible for welding, and immediately pressing the welding drop by using a hot press under the pressure of 80KN for 8-10s.
Step 4, after the welding blocks are cooled, inlaying the welding blocks by using inlay powder, and heating and melting to prepare an inlay sample;
And 4.1, paying attention to the orientation of the powder in the welding block in the embedding process so that the surface with the powder faces downwards, wherein the embedded powder is conventional metallographic embedded powder in the market, preferably bakelite powder or jade powder, and can also be combined embedded powder of other types. The mosaic temperature is 145-155 ℃ and the mosaic time is 10-15min.
Polishing the thermally inlaid sample, and polishing by using water sand paper with different granularities;
and 5.1, the welded welding blocks are softer, and the attention and the order of sand paper are needed in the polishing process.
Step 6, polishing the thermal mosaic sample, and polishing by using diamond grinding liquid with different abrasive particle sizes;
And 6.1, selecting the diamond polishing solution as the polishing solution, and gradually reducing the granularity of the polishing solution.
Finally, the superfine metal powder section sample is prepared. The sample can be directly used for dynamic hardness measurement and microstructure observation, but in order to clearly observe the microstructure of the superfine metal powder, the sample with the section of the superfine metal powder can be corroded by adopting corrosive liquid, and then the microstructure observation is observed, wherein the corrosive liquid is selected according to the type of the superfine metal powder.
The invention has the beneficial effects that:
(1) The invention adopts a drip welding mode to inlay the metal superfine powder on the surface of a welding drip, the prepared sample can be used for observing the microstructure in the powder, and can carry out dynamic hardness measurement on the powder, thereby providing a new method for preparing the metallographic sample of the metal superfine powder and measuring the dynamic hardness of the powder;
(2) The sample powder prepared by the invention has low shedding rate, uniform powder dispersion and high phase contrast, and is used for data stabilization and smooth force-displacement curve during dynamic hardness measurement.
(3) The hardness of the selected welding wire is relatively close to that of the powder, the sample preparation and grinding are more convenient, the powder is saved, and the metallographic sample can be obtained by only dispersing a small amount of powder.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of the preparation method of the invention.
Fig. 2 shows the microstructure under copper-tin alloy mirror conditions.
Fig. 3 is a dynamic hardness indentation of copper-tin alloy powder.
Fig. 4 is a force-displacement curve during dynamic hardness measurement.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the superfine metal powder section sample has a flow shown in figure 1 and comprises the following steps:
The method is characterized in that copper-tin alloy powder with the particle size smaller than 60 mu m is prepared before experiments, the mass fraction of copper is 85%, the mass fraction of tin is 15%, and the powder appearance is spherical as a whole. The copper-tin alloy powder needs to be dried before being inlaid, and the welding wires are lead-tin welding wires with the mass fraction of lead being 33%, electric soldering iron, alcohol and hot inlaid powder, and the equipment used comprises an ultrasonic vibration dispersing instrument, a hot press, a hot inlaid machine and a metallographic grinding and polishing machine.
And dispersing copper-tin alloy powder, namely selecting 5g of powder, putting the copper-tin alloy powder into 50mL of alcohol solution, cleaning and dispersing the powder by using an ultrasonic resonance dispersing instrument, then sucking part of dispersion liquid onto a glass carrier by using a rubber head dropper, and drying alcohol on the glass carrier.
And (3) performing drop welding on the copper-tin alloy powder, namely heating the electric iron to 250 ℃, melting the lead-tin welding wire, enabling molten tin to drop above the copper-tin alloy powder, and rapidly pressing the tin-tin alloy powder by using a hot press, wherein the pressing pressure is 80KN, and the pressing time is 11s. By pressing, the contact area between the copper-tin alloy powder and the soldering liquid drops is increased, so that the soldering liquid drops can be welded to more powder, and meanwhile, the welding strength is improved.
The welding blocks are inlaid by using 25g of hot inlaid powder, wherein the inlaid temperature is 150 ℃ and the inlaid time is 14min. In order to improve the sample grinding success rate during embedding, a plurality of welding blocks can be placed into one thermal embedding sample through thermal embedding, the direction of the welding blocks in the embedding process is noted, and the surface of the welding blocks with powder faces downwards.
The embedded sample is polished, because the hardness of the welding wire is low, the polishing time is required to be paid attention to, the used sand paper is water sand paper, the embedded sample is sequentially polished by adopting the water sand paper with the granularity of 150 meshes, 400 meshes, 800 meshes, 1500 meshes and 2500 meshes, the polishing time of each granularity sand paper is 5min, the water flow is required to be paid attention to in the polishing process, the polishing efficiency is affected by the overlarge water flow, scratches are easy to be generated due to the overlarge water flow, the water flow is controlled to be 100 mL/min -1, and the polishing is carried out until the scratches are basically not seen under an optical microscope.
Polishing the embedded sample, namely sequentially polishing the embedded sample by using diamond grinding liquid with diamond grain diameters of 6 mu m, 3 mu m, 1 mu m and 0.5 mu m for 5min to obtain the superfine metal powder section sample.
Firstly, a dynamic hardness experiment is carried out on a sample with an ultrafine metal powder section, the test pressure is 10gf, the loading time is 30s, the unloading time is 5s, the final measured dynamic hardness (Mars hardness) is 1364.27 N.mm -2, the dynamic hardness indentation of copper-tin alloy powder is shown in figure 2, and the figure 2 shows that the powder indentation is clear, the powder adhesion is good, the phase is uniform, the contrast is high, and the polishing is easy. The force-displacement curve in the dynamic hardness measurement process is shown in fig. 3, and the sample loading curve is stable and the force-displacement curve is smooth as can be known from fig. 3, so that the prepared sample is suitable for dynamic hardness measurement.
In order to further observe the microscopic morphology of the copper-tin alloy powder, the sample with the cross section of the superfine metal powder is corroded, wherein the adopted corrosive liquid is FeCl 3 alcohol solution, the ratio of FeCl 3 to alcohol=5 g to 30ml, and the corrosion time is 10s. The microstructure under the condition of the copper-tin alloy optical lens is shown in fig. 4, and as can be seen from fig. 4, the metallographic sample of the prepared metal superfine powder has low powder falling rate, high lining degree and clear microstructure in the powder in the grinding and polishing process.
Example 2
The preparation method of the superfine metal powder section sample has a flow shown in figure 1 and comprises the following steps:
The method is characterized in that pure copper powder with the particle size of 50-60 mu m is prepared before experiments, and the powder appearance is spherical as a whole. The pure copper powder needs to be dried before being inlaid, and the welding wires are lead-tin welding wires with the mass fraction of lead being 33%, electric soldering iron, acetone and thermal inlaid powder, and the equipment used comprises an ultrasonic vibration dispersing instrument, a hot press, a thermal inlaid machine and a metallographic grinding and polishing machine.
And dispersing copper-tin alloy powder, namely selecting 5g of powder, putting the copper-tin alloy powder into 30mL of acetone solution, cleaning and dispersing the powder by using an ultrasonic resonance dispersing instrument, then sucking part of dispersion liquid onto a glass carrier by using a rubber head dropper, and drying acetone on the glass carrier.
And (3) performing drop welding on the pure copper powder, namely heating the electric iron to 250 ℃, melting the lead-tin welding wire, enabling molten tin welding drops to be above the pure copper powder, and rapidly pressing the tin welding drops by using a hot press, wherein the pressing pressure is 80KN, and the pressing time is 11s. By pressing, the contact area between the pure copper powder and the soldering liquid drops is increased, so that the soldering liquid drops can be welded to more powder, and meanwhile, the welding strength is improved.
The welding blocks are inlaid, namely 25g of hot inlaid powder is used, the inlaid temperature is 145 ℃, and the inlaid time is 10min. In order to improve the sample grinding success rate during embedding, a plurality of welding blocks can be placed into one thermal embedding sample through thermal embedding, the direction of the welding blocks in the embedding process is noted, and the surface of the welding blocks with powder faces downwards.
The embedded sample is polished, because the hardness of the welding wire is low, the polishing time is required to be paid attention to, the used sand paper is water sand paper, the embedded sample is sequentially polished by adopting the water sand paper with the granularity of 150 meshes, 400 meshes, 800 meshes, 1500 meshes and 2500 meshes, the polishing time of each piece of the granularity sand paper is 7min, the water flow is required to be paid attention to in the polishing process, the polishing efficiency is affected by the overlarge water flow, scratches are easy to be generated due to the overlarge water flow, the water flow is controlled to be 300 mL/min -1, and the polishing is carried out until the scratches are basically not seen under an optical microscope.
Polishing the embedded sample, namely sequentially polishing the embedded sample by using diamond grinding liquid with diamond grain diameters of 6 mu m, 3 mu m, 1 mu m and 0.5 mu m for 10min to obtain the superfine metal powder section sample.
The dynamic hardness test is carried out on the superfine metal powder section sample, the test pressure is 10gf, the loading time is 30s, the unloading time is 5s, and the final dynamic hardness (Mars hardness) is 1101.38 N.mm -2.
Example 3
The preparation method of the superfine metal powder section sample has a flow shown in figure 1 and comprises the following steps:
the method is characterized in that copper-tin alloy powder with the particle size smaller than 60 mu m is prepared before an experiment, the mass fraction of copper is 67%, the mass fraction of tin is 33%, and the whole shape of the powder is spherical. The copper-tin alloy powder needs to be dried before being inlaid, and the welding wires are Ag-Sn welding wires, electric soldering irons, propanol and hot inlaid powder (comprising bakelite powder), and the equipment comprises an ultrasonic vibration dispersing instrument, a hot press, a hot inlaid machine and a metallographic grinding and polishing machine.
And dispersing copper-tin alloy powder, namely selecting 5g of powder, putting the copper-tin alloy powder into 10 propanol solution, cleaning and dispersing the powder by using an ultrasonic resonance dispersing instrument, then sucking part of dispersion liquid onto a glass carrier by using a rubber head dropper, and drying propanol on the glass carrier.
And (3) performing drop welding on the copper-tin alloy powder, namely heating the electric iron to 250 ℃, then melting the Ag-Sn welding wire to enable the melted Ag-Sn welding wire to be above the copper-tin alloy powder, and rapidly pressing the tin-tin alloy powder drops by using a hot press, wherein the pressing pressure is 80KN, and the pressing time is 11s. By pressing, the contact area between the copper-tin alloy powder and the soldering liquid drops is increased, so that the soldering liquid drops can be welded to more powder, and meanwhile, the welding strength is improved.
The welding blocks are inlaid by using 25g of hot inlaid powder, wherein the inlaid temperature is 155 ℃ and the inlaid time is 10min. In order to improve the sample grinding success rate during embedding, a plurality of welding blocks can be placed into one thermal embedding sample through thermal embedding, the direction of the welding blocks in the embedding process is noted, and the surface of the welding blocks with powder faces downwards.
The embedded sample is polished, because the hardness of the welding wire is low, the polishing time is required to be paid attention to, the used sand paper is water sand paper, the embedded sample is sequentially polished by adopting the water sand paper with the granularity of 150 meshes, 400 meshes, 800 meshes, 1500 meshes and 2500 meshes, the polishing time of each piece of the granularity sand paper is 10min, the water flow is required to be paid attention to in the polishing process, the polishing efficiency is affected by the overlarge water flow, scratches are easy to be generated due to the overlarge water flow, the water flow is controlled to be 400 mL/min -1, and the polishing is carried out until the scratches are basically not seen under an optical microscope.
Polishing the embedded sample, namely sequentially polishing the embedded sample by using diamond grinding liquid with diamond grain diameters of 6 mu m, 3 mu m, 1 mu m and 0.5 mu m for 7min to obtain the superfine metal powder section sample.
The dynamic hardness test is carried out on the superfine metal powder section sample, the test pressure is 10gf, the loading time is 30s, the unloading time is 5s, and the final dynamic hardness (Mars hardness) is 1809.30 N.mm -2.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. The preparation method of the superfine metal powder section sample is characterized by comprising the following steps of:
(1) Dispersing the metal superfine powder in a dispersing agent to obtain a dispersion liquid, dripping the dispersion liquid on a glass slide, and drying to disperse the metal superfine powder on the glass slide;
(2) Heating a welding wire by adopting an electric iron to melt the welding wire, dripping the melted welding droplet on the metal superfine powder to enable the metal superfine powder to be adhered and embedded on the surface of the welding droplet, and then rapidly pressing the welding droplet into a welding block by using a hot press;
(3) Embedding the welding blocks by using a thermal embedding process to prepare an embedded sample, wherein the surface of the welding blocks, which is provided with powder, faces downwards when the welding blocks are placed in the thermal embedding process, the embedding temperature is 145-155 ℃, and the embedding time is 10-15 min;
(4) Polishing the inlaid sample to obtain a superfine metal powder section sample;
the grain diameter of the metal superfine powder is less than or equal to 60 mu m;
The concentration of the metal superfine powder in the dispersion liquid is 0.1-0.5 g.mL -1;
the welding wire is a lead-tin welding wire or a silver-tin welding wire.
2. The method for preparing a cross-section sample of ultrafine metal powder according to claim 1, wherein the ultrafine metal powder is prepared by an aerosolization pulverizing process.
3. The method for preparing a cross-section sample of ultrafine metal powder according to claim 1 or 2, wherein the metal ultrafine powder is added to the dispersing agent in the step (1) and dispersed and washed by using an ultrasonic dispersing machine.
4. The method for preparing a cross-section sample of ultrafine metal powder according to claim 3, wherein the dispersant is ethanol, propanol or acetone.
5. The method for preparing a cross-section sample of ultrafine metal powder according to claim 4, wherein the inlaid powder used in the thermal inlaying process is bakelite powder or jade powder.
6. The method for preparing a sample of ultrafine metal powder cross section according to claim 1, wherein the step (4) uses sandpaper to polish the embedded sample, the sandpaper is water sandpaper, and the polishing solution is used to polish the embedded sample after polishing.
7. The method for preparing a sample of ultra-fine metal powder cross section according to claim 1, wherein the sample of ultra-fine metal powder cross section prepared in step (4) is etched with an etching solution.
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| CN110455846A (en) * | 2019-08-19 | 2019-11-15 | 飞而康快速制造科技有限责任公司 | A method for displaying microstructure of fine powder section |
| CN114082965A (en) * | 2021-10-27 | 2022-02-25 | 北京七弟科技有限公司 | Preparation method of metal-based micro-nano particle composite powder, obtained powder and its application in the preparation of composite materials |
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| FR423131A (en) * | 1910-11-29 | 1911-04-08 | Wilhelm Schieber | Welding process of copper, nickel or alloys of these metals |
| JP3529669B2 (en) * | 1999-05-17 | 2004-05-24 | 株式会社神戸製鋼所 | No plating wire for arc welding and arc welding method |
| CN108362695A (en) * | 2018-01-23 | 2018-08-03 | 中国科学院金属研究所 | The metallographic preparation method of ultra-fine titanium alloy powder and the detection method of hollow powder rate |
| CN109093128A (en) * | 2018-09-25 | 2018-12-28 | 大连理工大学 | Device and method for preparing superfine low-melting-point spherical metal powder by droplet-by-droplet atomization method |
| CN114518373A (en) * | 2022-03-30 | 2022-05-20 | 南昌航空大学 | Preparation method of ceramic powder cross-section mosaic sample for electron microscope observation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110455846A (en) * | 2019-08-19 | 2019-11-15 | 飞而康快速制造科技有限责任公司 | A method for displaying microstructure of fine powder section |
| CN114082965A (en) * | 2021-10-27 | 2022-02-25 | 北京七弟科技有限公司 | Preparation method of metal-based micro-nano particle composite powder, obtained powder and its application in the preparation of composite materials |
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