CN119703242A - Brazing method of graphite target - Google Patents
Brazing method of graphite target Download PDFInfo
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- CN119703242A CN119703242A CN202411830328.6A CN202411830328A CN119703242A CN 119703242 A CN119703242 A CN 119703242A CN 202411830328 A CN202411830328 A CN 202411830328A CN 119703242 A CN119703242 A CN 119703242A
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Abstract
本发明涉及一种石墨靶材的钎焊方法，所述钎焊方法包括如下步骤：(1)对石墨靶材的焊接面进行喷砂，得到喷砂后的石墨靶材；(2)对所述喷砂后的石墨靶材的焊接面进行真空磁控溅射镀钛，得到具有钛膜的石墨靶材；(3)分别将背板和具有钛膜的石墨靶材进行加热，并对加热后的石墨靶材和背板进行钎焊。本发明通过对石墨靶材进行喷砂和真空磁控溅射镀钛处理，改善了石墨靶材表面的焊料浸润性差的问题，极大降低了石墨靶材使用过程中脱焊的风险，降低了生产的成本，提高产品的生产效率，同时，将背板与具有钛膜的石墨靶材进行钎焊，可以极大地提高石墨靶材的拉伸强度。
The present invention relates to a brazing method for a graphite target material, the brazing method comprising the following steps: (1) sandblasting the welding surface of the graphite target material to obtain a sandblasted graphite target material; (2) vacuum magnetron sputtering titanium plating the welding surface of the sandblasted graphite target material to obtain a graphite target material with a titanium film; (3) heating a back plate and the graphite target material with the titanium film respectively, and brazing the heated graphite target material and the back plate. The present invention improves the problem of poor solder wettability on the surface of the graphite target material by sandblasting and vacuum magnetron sputtering titanium plating on the graphite target material, greatly reduces the risk of desoldering during the use of the graphite target material, reduces the production cost, and improves the production efficiency of the product. At the same time, brazing the back plate and the graphite target material with the titanium film can greatly improve the tensile strength of the graphite target material.
Description
Technical Field
The invention relates to the technical field of semiconductor electronics, in particular to a brazing method of a graphite target.
Background
Graphite materials are widely used in the fields of nuclear reactors, aviation and aviation structural materials, electrode materials, drill bits for special purposes, corrosion-resistant crucibles for chemical experiments, semiconductor materials and the like due to the characteristics of high temperature resistance, corrosion resistance, self lubrication and the like. Graphite targets are commonly used in the semiconductor field as substrates for silicon carbide in chips. The graphite target material is required to be connected with the backboard in a brazing mode and is used together on equipment in a sputtering mode, as the wettability of the graphite surface and the welding flux is poor, the surface is not treated, the welding combination rate with the backboard is low, and the risk of desoldering in the using process is also easy to cause.
The sputtering film plating technology generally utilizes gas discharge to generate gas ionization, and positive ions bombard a cathode target material at high speed under the action of an electric field to knock out atoms or molecules of the cathode target material and fly to the surface of a plated substrate to deposit a film. The current sputtering technology comprises radio frequency sputtering, three-stage sputtering and magnetron sputtering technology, and the magnetron sputtering has higher coating speed compared with other sputtering technologies, and the magnetron sputtering is one of the mainstream technology of coating. With the rapid development of terminal application markets such as artificial intelligence, 5G technology and consumer electronics, the market scale of semiconductor chips is increasingly enlarged, and the application range of magnetron sputtering technology is also increasingly wider.
Brazing refers to a welding process in which after brazing filler metal below the melting point of a welding piece and the welding piece are heated to the melting temperature of the brazing filler metal at the same time, liquid brazing filler metal is used for filling gaps of solid workpieces to connect metal materials. In the magnetron sputtering process, the brazing layer connection structure of the target assembly prepared by brazing is adopted, so that the connection interface of the target and the backboard has good heat conduction performance, the heat dissipation performance of the target assembly can be effectively improved, and after the magnetron sputtering is finished, the brazing layers of the target and the backboard can be melted by adopting proper temperature, thereby recycling the backboard and saving the preparation cost of the target.
CN117248203a discloses a binding method of a graphite target and a back plate, by performing sand blasting and chemical nickel plating treatment on a welding surface of the graphite target, wettability of the graphite target is improved, then, by combining brazing with the back plate, welding strength of the target and the back plate is improved, a desoldering risk in a target use process is reduced, a chemical nickel plating process is relatively complex, special equipment and chemical reagents are required to be used, production cost is too high, waste water and waste gas are also generated in the chemical nickel plating process, and if the waste is not properly treated, adverse effects on environment are caused.
CN115770922a discloses a method for brazing graphite target, which increases wettability of solder on the surface of the graphite target by arranging a metal film on the welding surface of the graphite target, and then, brazes the graphite target and the back plate to improve welding combination rate of the graphite target and the back plate, so as to avoid cracking of the graphite target caused by the brazing process, and the welding surface of the graphite target is not treated, and the metal film is directly arranged on the welding surface of the graphite target, so that the risk of desoldering exists in the subsequent use process.
In summary, there is a need to develop a method for brazing graphite targets, which reduces the risk of desoldering during target use.
Disclosure of Invention
In order to solve the technical problems, the invention provides a brazing method of a graphite target, which can effectively improve the welding combination rate and welding strength of the graphite target, reduce the risk of desoldering in the use process of the target, reduce the production cost and improve the production efficiency of products.
To achieve the purpose, the invention adopts the following technical scheme:
The invention provides a brazing method of a graphite target, which comprises the following steps:
(1) Performing sand blasting on the welding surface of the graphite target material to obtain the graphite target material after sand blasting;
(2) Carrying out vacuum magnetron sputtering titanium plating on the welding surface of the graphite target after sand blasting to obtain a graphite target with a titanium film;
(3) And respectively heating the back plate and the graphite target material with the titanium film, and brazing the heated graphite target material and the back plate.
The invention aims at the graphite target, unlike the conventional metal or metal alloy target, the graphite target has great welding difficulty with a metal backboard or metal alloy backboard due to the problem of great compatibility between the graphite target and the metal or metal alloy material, and the wettability of the surface of the graphite target to welding flux is very poor, especially when the process of hot isostatic pressing and the like is not adopted, the brazing process is only adopted, and the high-efficiency and high-strength welding of the graphite target and the backboard is intended to be realized with great difficulty. In the invention, the surface roughness of the graphite target is enhanced by carrying out sand blasting treatment on the graphite target, and then vacuum magnetron sputtering titanium plating treatment is adopted, so that a titanium film is firmly attached to the surface of the graphite target, the problem of poor solder wettability of the surface of the graphite target is solved, and the welding combination rate and welding strength of the graphite target are effectively improved; furthermore, the invention carries out heating treatment on the graphite target and the back plate before brazing, can lead the graphite target and the back plate to reach temperature balance before brazing, reduces the thermal stress generated by temperature difference in the welding process, thereby reducing the deformation generated by temperature difference in the welding process, improving the welding quality, greatly reducing the risk of desoldering in the using process of the graphite target, reducing the production cost and improving the production efficiency of products by combining the specific steps, and simultaneously, can greatly improve the tensile strength of the graphite target by brazing the back plate and the graphite target with a titanium film.
In a preferred embodiment of the present invention, the pressure of the blasting in the step (1) is 0.3 to 0.4MPa, for example, 0.3MPa, 0.32MPa, 0.34MPa, 0.36MPa, 0.38MPa or 0.4MPa, but the blasting is not limited to the values listed, and other values not listed in the above-mentioned numerical ranges are equally applicable.
Preferably, the sand-blasted sand mold is white corundum.
Preferably, the model number of the white corundum comprises any one or at least two of 24# and 46# or 60# and typical but non-limiting combinations include 24# and 46# combinations, 24# and 60# combinations, 46# and 60# combinations and 24# and 46# and 60# combinations.
The roughness of the welded surface of the graphite target after blasting is preferably 11 to 14 μm, and may be, for example, 11 μm, 11.5 μm, 12 μm, 12.5 μm, 13 μm, 13.5 μm or 14 μm, but is not limited to the values listed, and other values not listed in the above-mentioned numerical ranges are equally applicable.
According to the invention, the roughness of the welding surface of the graphite target after sandblasting is limited to be 11-14 mu m, so that the welding strength of the graphite target and the backboard is optimal, if the roughness of the welding surface of the graphite target after sandblasting is less than 11 mu m, the welding strength is lower, the risk of desoldering is possible, and if the roughness of the welding surface of the graphite target after sandblasting is greater than 14 mu m, the welding strength is almost zero, and the risk of desoldering is larger.
In a preferred embodiment of the present invention, the vacuum degree of the vacuum magnetron sputtering titanium plating in the step (2) is 4.0X10 -3-8.0×10-3 Pa, for example, 4.0X10 -3Pa、5.0×10-3Pa、6.0×10-3Pa、7.0×10-3 Pa or 8.0X10 -3 Pa, but the invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are applicable.
Preferably, the sputtering voltage of the vacuum magnetron sputtering titanium plating is 80-120V, for example, 80V, 90V, 100V, 110V or 120V, but the sputtering voltage is not limited to the listed values, and other non-listed values in the above-mentioned value range are equally applicable.
Preferably, the sputtering current of the vacuum magnetron sputtering titanium plating is 10-30mA, for example, 10mA, 15mA, 20mA, 25mA or 30mA, but the sputtering current is not limited to the listed values, and other values not listed in the above-mentioned value range are equally applicable.
The invention ensures the thickness uniformity of the titanium film by limiting the sputtering voltage of 80-120V and the sputtering current of 10-30mA of vacuum magnetron sputtering titanium plating.
Preferably, the sputtering time of the vacuum magnetron sputtering titanium plating is 3-5h, for example, 3h, 3.5h, 4h, 4.5h or 5h, but the method is not limited to the listed values, and other non-listed values in the above-mentioned value range are equally applicable.
The thickness of the titanium plating layer of the graphite target having a titanium film is preferably 2 to 5 μm, and may be, for example, 2 μm, 2.5 μm,3 μm, 3.5 μm, 4 μm, 4.5 μm or 5 μm, but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
The invention can achieve the best infiltration effect by limiting the thickness of the titanium plating layer to be 2-5 mu m, is favorable for subsequent welding, is unfavorable for the infiltration of the surface of the graphite target material if the thickness of the titanium plating layer is less than 2 mu m, thereby influencing the final welding result, and has little influence on the infiltration of the surface of the graphite target material if the thickness of the titanium plating layer is greater than 5 mu m, but greatly increases the sputtering time and the production cost.
The roughness of the titanium plating layer of the graphite target having a titanium film is preferably 10 to 12 μm, and may be, for example, 10 μm, 10.5 μm, 11 μm, 11.5 μm or 12 μm, but is not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
According to the invention, the roughness of the titanium plating layer of the graphite target with the titanium film is limited to be 10-12 mu m, so that the welding strength of the graphite target and the backboard is optimal, if the roughness of the titanium plating layer of the graphite target with the titanium film is smaller than 10 mu m, the welding strength is lower, the risk of desoldering is possible, and if the roughness of the titanium plating layer of the graphite target with the titanium film is larger than 12 mu m, the welding strength is almost zero, and the risk of desoldering is larger.
As a preferred embodiment of the present invention, the material of the back plate in the step (3) includes any one or a combination of at least two of Al, cu, and Mo, wherein typical but non-limiting combinations include a combination of Al and Cu, a combination of Al and Mo, a combination of Cu and Mo, and a combination of Al, cu, and Mo.
Preferably, the target temperature of the heating is 200-220 ℃, such as 200 ℃, 205 ℃, 210 ℃, 215 ℃, or 220 ℃, but is not limited to the recited values, and other non-recited values within the above range are equally applicable.
Preferably, the heating rate is 2-5 ℃ per minute, for example, 2 ℃, 2.5 ℃,3 ℃, 3.5 ℃, 4 ℃, 4.5 ℃ or 5 ℃ per minute, but not limited to the recited values, and other non-recited values within the recited values are equally applicable.
As a preferable technical scheme of the invention, the brazing in the step (3) sequentially comprises infiltration, lamination, hot pressing and cooling.
As a preferred technical scheme of the invention, the wetting comprises the steps of independently placing solder on the welding surface of the graphite target material with the titanium film and the welding surface of the backboard respectively for wetting.
Preferably, the method of infiltration comprises ultrasonic infiltration.
Preferably, the welding surface of the back plate is treated by adopting a rigid brush before the infiltration treatment.
Preferably, the infiltration time of the welding surface of the graphite target material with the titanium film is 10-20min, for example, 10min, 12min, 14min, 16min, 18min or 20min, but not limited to the listed values, and other non-listed values in the above-mentioned value range are equally applicable.
Preferably, the soaking time of the welding surface of the back plate is 10-15min, for example, 10min, 11min, 12min, 13min, 14min or 15min, but not limited to the listed values, and other values not listed in the above-mentioned value range are equally applicable.
Preferably, the material of the solder includes indium solder.
In the invention, the material of the solder comprises indium solder, so that the surface of the solder and the surface of the graphite target are difficult to infiltrate, and therefore, sand blasting and titanizing processes are needed to be adopted first, so that the infiltration effect is improved.
According to the preferable technical scheme, the bonding comprises the steps of manufacturing a solder groove on the welding surface of the backboard, placing a copper wire in the solder groove, and bonding the welding surface of the graphite target material with the welding surface of the backboard.
Preferably, the depth of the solder bath is 3-5mm, for example, 3mm, 3.5mm, 4mm, 4.5mm or 5mm, but not limited to the values recited, and other values not recited in the above ranges are equally applicable.
Preferably, the length and width of the solder grooves are the same as those of the back plate.
The welding combination rate in the welding process can be ensured by limiting the specific size of the welding groove, if the size of the welding groove is too small, the used welding flux is too small, the subsequent welding is not facilitated, the welding combination rate is reduced, if the size of the welding groove is too large, the used welding flux is too much, the welding flux is not easy to remove after the welding, and the labor cost is increased.
The diameter of the copper wire is preferably 0.2-0.5mm, and may be, for example, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm or 0.5mm, but is not limited to the recited values, and other non-recited values within the above-mentioned ranges are equally applicable.
As a preferable technical scheme of the invention, the hot pressing comprises the steps of placing a buffer pad on the bonded graphite target material and placing a pressing block on the buffer pad.
Preferably, the temperature of the cushion is 200-220 ℃, such as 200 ℃, 205 ℃, 210 ℃, 215 ℃, or 220 ℃, but is not limited to the recited values, and other non-recited values within the recited ranges are equally applicable.
Preferably, the cushion comprises a silica gel pad or a wood block.
The pressure of the briquette is preferably 0.3 to 0.5MPa, and may be, for example, 0.3MPa, 0.35MPa, 0.4MPa, 0.45MPa or 0.5MPa, but is not limited to the values recited, and other values not recited in the above-mentioned numerical ranges are equally applicable.
As a preferred embodiment of the present invention, the target temperature of the cooling is 25 ℃.
Preferably, the cooling rate is 1-2 ℃ per minute, and may be, for example, 1 ℃, 1.2 ℃, 1.4 ℃, 1.6 ℃, 1.8 ℃, or 2 ℃, although not limited to the recited values, other non-recited values within the above ranges are equally applicable.
According to the invention, the welding strength of the graphite target and the backboard can be ensured by limiting the cooling rate to 1-2 ℃ per minute, if the cooling rate is smaller than 1 ℃ per minute, the cooling time is increased, the production cost is increased, and if the cooling rate is larger than 2 ℃ per minute, the temperature difference between the target and the heating table is larger, deformation is likely to occur, and meanwhile, for a brittle target, the target is likely to crack due to deformation.
As a preferable technical scheme of the invention, the brazing method comprises the following steps:
(1) Carrying out sand blasting on the welding surface of the graphite target by using white corundum, wherein the pressure of the sand blasting is 0.3-0.4MPa, and the graphite target with the roughness of 11-14 mu m is obtained;
(2) Vacuum magnetron sputtering titanium plating is carried out on the welding surface of the graphite target after sand blasting under the vacuum degree of 4.0X10 -3-8.0×10-3 Pa, the thickness of the titanium plating layer is 2-5 mu m, and the graphite target with the titanium film and the roughness of 10-12 mu m is obtained;
(3) Heating the back plate and the graphite target material with the titanium film to a target temperature of 200-220 ℃ at a heating rate of 2-5 ℃ per minute, placing molten solder on the welding surface of the graphite target material with the titanium film, infiltrating the welding surface of the graphite target material with an ultrasonic welder for 10-20min, infiltrating the back plate with a manual steel brush and the ultrasonic welder for 10-15min, manufacturing a solder tank with a depth of 3-5mm on the welding surface of the back plate, placing copper wires with a diameter of 0.2-0.5mm in the solder tank, bonding the welding surface of the graphite target material with the welding surface of the back plate, placing a buffer cushion on the bonded graphite target material, placing a pressing block with a pressure of 0.3-0.5MPa on the buffer cushion, cooling the bonded graphite target material and the back plate to 25 ℃ at a cooling rate of 1-2 ℃ per min after welding, and removing the pressing block, thereby completing the brazing of the graphite target material and the back plate.
Compared with the prior art, the invention has at least the following beneficial effects:
According to the invention, the titanium film is firmly attached to the surface of the graphite target by carrying out sand blasting and vacuum magnetron sputtering titanium plating treatment on the graphite target, so that the problem of poor solder wettability on the surface of the graphite target is solved, the welding combination rate of the graphite target obtained by brazing and the back plate reaches more than 99.6%, the combination strength can reach more than 8.3MPa, meanwhile, the problem of desoldering in the use process of the graphite target is solved, the production cost is reduced, the production efficiency of a product is improved, and meanwhile, the back plate and the graphite target with the titanium film are brazed, so that the tensile strength of the graphite target can be greatly improved.
Drawings
FIG. 1 is a flow chart of the process of brazing a graphite target and backing plate of example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
Example 1
The embodiment provides a brazing method of a graphite target, referring to fig. 1, the brazing method includes the following steps:
(1) Wiping a surface to be sandblasted of the graphite target with ethanol, drying, and then sandblasting a welding surface of the graphite target with 24# white corundum, wherein the pressure of sandblasting is 0.35kPa, so as to obtain the graphite target with the roughness of 12 mu m;
(2) Vacuum magnetron sputtering titanium plating is carried out on the welding surface of the graphite target after sand blasting under the vacuum degree of 6.0X10 -3 Pa, the sputtering voltage of the vacuum magnetron sputtering titanium plating is 100V, the sputtering current is 20mA, the sputtering time is 4h, the thickness of the titanium plating layer is 4 mu m, and the graphite target with the titanium film with the roughness of 11 mu m is obtained;
(3) Heating an Al backboard and a graphite target material with a titanium film to a target temperature of 210 ℃ at a temperature rising rate of 3 ℃ per minute, placing molten solder on the welding surface of the graphite target material with the titanium film, infiltrating the welding surface of the graphite target material with an ultrasonic welder for 15 minutes, infiltrating the Al backboard with a manual steel brush and the ultrasonic welder for 12 minutes, manufacturing a welding groove with a depth of 4mm on the welding surface of the Al backboard, placing copper wires with a diameter of 0.3mm in the welding groove, bonding the welding surface of the graphite target material and the welding surface of the Al backboard, placing a silica gel pad with a pressure of 0.4MPa on the bonded graphite target material, cooling the bonded graphite target material and the Al backboard to 25 ℃ at a cooling rate of 1.5 ℃ per minute after the welding is completed, and removing the pressing block to finish the brazing of the graphite target material and the Al backboard.
Example 2
The embodiment provides a brazing method of a graphite target, which comprises the following steps:
(1) Wiping a surface to be sandblasted of the graphite target with ethanol, drying, and then sandblasting a welding surface of the graphite target with 46# white corundum, wherein the pressure of sandblasting is 0.3MPa, so as to obtain the graphite target with the roughness of 11 mu m;
(2) Vacuum magnetron sputtering titanium plating is carried out on the welding surface of the graphite target after sand blasting under the vacuum degree of 4.0X10 -3 Pa, the sputtering voltage of the vacuum magnetron sputtering titanium plating is 80V, the sputtering current is 30mA, the sputtering time is 5h, the thickness of the titanium plating layer is 5 mu m, and the graphite target with the titanium film with the roughness of 10 mu m is obtained;
(3) Heating a Cu backboard and a graphite target material with a titanium film to a target temperature of 200 ℃ at a heating rate of 2 ℃ per minute, placing molten solder on the welding surface of the graphite target material with the titanium film, infiltrating the welding surface of the graphite target material with an ultrasonic welder for 20min, infiltrating the Cu backboard with a manual steel brush and the ultrasonic welder for 15min, manufacturing a welding groove with a depth of 5mm on the welding surface of the Cu backboard, placing copper wires with a diameter of 0.5mm in the welding groove, bonding the welding surface of the graphite target material and the welding surface of the Cu backboard, placing a wood block with a pressure of 0.5MPa on the bonded graphite target material, cooling the welded graphite target material and the Cu backboard to 25 ℃ at a cooling rate of 1 ℃ per min after the welding is completed, and removing the briquetting to finish the brazing of the graphite target material and the backboard.
Example 3
The embodiment provides a brazing method of a graphite target, which comprises the following steps:
(1) Wiping a surface to be sandblasted of the graphite target with ethanol, drying, and then sandblasting a welding surface of the graphite target with 60# white corundum, wherein the pressure of sandblasting is 0.4MPa, so as to obtain the graphite target with the roughness of 14 mu m;
(2) Vacuum magnetron sputtering titanium plating is carried out on the welding surface of the graphite target after sand blasting under the vacuum degree of 8.0 multiplied by 10 -3 Pa, the sputtering voltage of the vacuum magnetron sputtering titanium plating is 120V, the sputtering current is 10mA, the sputtering time is 3h, the thickness of the titanium plating layer is 2 mu m, and the graphite target with the titanium film with the roughness of 12 mu m is obtained;
(3) Heating a Mo backboard and a graphite target material with a titanium film to a target temperature of 220 ℃ at a temperature rising rate of 5 ℃ per minute, placing molten solder on a welding surface of the graphite target material with the titanium film, infiltrating the welding surface of the graphite target material with an ultrasonic welder for 10 minutes, infiltrating the Mo backboard with a manual steel brush and the ultrasonic welder for 10 minutes, manufacturing a welding groove with a depth of 3mm on the welding surface of the Mo backboard, placing copper wires with a diameter of 0.2mm in the welding groove, bonding the welding surface of the graphite target material and the welding surface of the Mo backboard, placing a silica gel pad with a pressure of 0.3MPa on the bonded graphite target material, cooling the bonded graphite target material and the backboard to 25 ℃ at a cooling rate of 2 ℃ per minute after the welding is completed, and removing the briquetting to finish the brazing of the graphite target material and the backboard.
Example 4
This example provides a method for brazing a graphite target, which differs from example 1 only in that the roughness of the titanium plating layer of the graphite target having a titanium film in step (2) is adjusted to 6 μm, and the other steps are the same as in example 1.
Example 5
This example provides a method for brazing a graphite target, which differs from example 1 only in that the roughness of the titanium plating layer of the graphite target having a titanium film in step (2) is adjusted to 14 μm, and the other steps are the same as in example 1.
Example 6
This example provides a method for brazing a graphite target, which differs from example 1 only in that the method is the same as example 1 except that the brazing bath in step (3) is adjusted to a depth of 2 mm.
Example 7
This example provides a method for brazing a graphite target, which differs from example 1 only in that the method is the same as example 1 except that the depth of the brazing tank in step (3) is adjusted to 6 mm.
Example 8
This example provides a method of brazing a graphite target, which differs from example 1 only in that the cooling rate in step (3) is adjusted to 0.5 ℃ per minute, and the remainder is the same as example 1.
Example 9
This example provides a method of brazing a graphite target, which differs from example 1 only in that the cooling rate in step (3) is adjusted to 3 ℃.
Comparative example 1
The present example provides a method for brazing a graphite target, which differs from example 1 only in that the sand blasting treatment of step (1) is not performed, and the remainder is the same as example 1.
Comparative example 2
This example provides a method for brazing a graphite target, which differs from example 1 only in that the method is the same as example 1 except that the step (2) is performed with electroless titanium plating on the welded surface of the graphite target after the blasting.
Comparative example 3
The present example provides a method for brazing a graphite target, which differs from example 1 only in that the vacuum magnetron sputtering titanizing treatment of step (2) is not performed, and the remainder are the same as example 1.
Comparative example 4
The present example provided a method for brazing a graphite target, which was different from example 1 only in that the procedure (2) was followed by vacuum magnetron sputtering nickel plating treatment of the welded surface of the sandblasted graphite target, and the procedure was the same as example 1.
The welded bonding ratio and bonding strength of the graphite targets and the backing plate obtained by brazing in examples and comparative examples were tested. The welding combination rate is tested by an ultrasonic flaw detector, the combination strength is tested by detecting the tensile strength, namely, the graphite target obtained by brazing is processed into a hollow shape, the hole is deep to the welding combination position, then the graphite target is suspended, the pressure point of pressure equipment with a digital display function is acted on the welding surface, the pressure in the process of desoldering is recorded as the welding combination strength of the material, and whether cracks exist on the surface of the graphite target after brazing is observed, and the obtained result is shown in a table 1.
TABLE 1
The test results can be seen:
(1) According to the brazing method of the graphite target provided by the invention, the titanium film is firmly attached to the surface of the graphite target by carrying out sand blasting and vacuum magnetron sputtering titanium plating treatment on the graphite target, so that the problem of poor solder wettability on the surface of the graphite target is solved, the welding combination rate of the graphite target obtained by brazing and the backboard is up to more than 99.6%, the combination strength can be up to more than 8.3MPa, and meanwhile, the problem of desoldering in the use process of the graphite target is solved.
(2) It can be seen from a combination of examples 1 and 4 to 5 that the roughness of the titanium plating layer of the graphite target having a titanium film in step (2) in example 1 was 11. Mu.m, the bonding strength of the graphite target to the back plate was 9.5MPa, the roughness of the titanium plating layer of the graphite target having a titanium film in example 4 was 6. Mu.m, the bonding strength of the graphite target to the back plate was 99.2%, the bonding strength of the graphite target to the back plate was 3.5MPa, the roughness of the titanium plating layer of the graphite target having a titanium film in example 5 was 14. Mu.m, and the bonding strength of the graphite target to the back plate in example 5 was 99.0% and was 0.5MPa, whereby it was revealed that the bonding strength of the graphite target to the back plate obtained by brazing was 8.3MPa or more by controlling the roughness of the bonding face of the graphite target to be 11 to 14. Mu.m.
(3) It can be seen from the combination of examples 1 and 6-7 that the depth of the solder pot in example 1 in step (3) is 4mm, the welding rate of the graphite target material and the back plate in example 1 is 99.8%, the bonding strength is 9.5MPa, the depth of the solder pot in example 6 is 2mm, the welding rate of the graphite target material and the back plate in example 6 is 98.5%, the bonding strength is 5.0MPa, the depth of the solder pot in example 7 is 6mm, the welding rate of the graphite target material and the back plate in example 7 is 99.6%, and the bonding strength is 8.2MPa, so that the invention can ensure the welding rate in the welding process by controlling the specific size of the solder pot, if the depth of the solder pot is too small, the used solder is unfavorable for subsequent welding, the welding rate is reduced, and if the depth of the solder pot is too large, the used solder is not affected by too much, but the welding rate of the graphite target material and the back plate is not easy to remove after welding, and the labor cost is increased.
(4) It can be seen from a combination of examples 1 and examples 8 to 9 that the cooling rate in step (3) in example 1 was 1.5C/min, the weld bonding rate of the graphite target and the back plate in example 1 was 99.8%, the bonding strength was 9.5MPa, the surface of the graphite target was crack-free after brazing, the cooling rate in example 8 was 0.5C/min, the weld bonding rate of the graphite target and the back plate in example 8 was 99.3%, the bonding strength was 8.1MPa, the surface of the graphite target was crack-free after brazing, the cooling rate in example 9 was 3C/min, the weld bonding rate of the graphite target and the back plate in example 9 was 99.1%, the bonding strength is 8.4MPa, and cracks are formed on the surface of the graphite target after brazing, so that the invention can ensure the welding strength of the graphite target and the back plate by controlling the cooling rate to be 1-2 ℃ per minute, if the cooling rate is too small, the welding bonding rate and the bonding strength are not influenced, but the cooling time is increased, the production cost is increased, and if the cooling rate is too large, the temperature difference between the target and the heating table is large, deformation is likely to occur, and meanwhile, for a brittle target, the target is likely to crack due to deformation.
(5) It can be seen from the comprehensive examples 1 and 1 that the welding surface of the graphite target is not subjected to sand blasting treatment before titanium plating in the comparative example 1, the roughness of the welding surface of the graphite target is smaller, the bonding strength of the graphite target obtained by brazing and the backboard is only 0.3MPa, and the graphite target is subjected to desoldering in the use process, so that the roughness of the surface of the graphite target is enhanced by performing sand blasting treatment on the graphite target, and the titanium film can be firmly attached to the surface of the graphite target when vacuum magnetron sputtering titanium plating treatment is performed later, and the desoldering risk of the graphite target in the use process is greatly reduced.
(6) As can be seen from the comprehensive examples 1 and 2, in the comparative example 2, the bonding strength between the welded surface of the graphite target after sand blasting and the back plate obtained by brazing is only 1.0MPa, because factors such as stability, concentration, temperature and the like of the solution may affect the quality and bonding strength of the plating layer in the chemical titanizing process, and the technological parameters are difficult to control, thus showing that the invention can perform titanizing on the welded surface of the graphite target after sand blasting by using the vacuum magnetron sputtering technology, and the formed titanizing layer has good uniformity, and can effectively improve the welding bonding rate and welding strength of the graphite target.
(7) As can be seen from the comprehensive examples 1 and 3, in the comparative example 3, the sandblasted graphite target is directly brazed with the backboard, the brazing bonding rate of the graphite target obtained by brazing and the backboard is 98.0%, and the bonding strength is only 0.2MPa, and meanwhile, the graphite target is subjected to desoldering in the use process, so that the titanium film is firmly attached to the surface of the graphite target by carrying out the vacuum magnetron sputtering titanation treatment on the sandblasted graphite target, the problem of poor solder wettability of the surface of the graphite target is solved, the welding bonding rate and the welding strength of the graphite target are effectively improved, and the desoldering risk of the graphite target in the use process is greatly reduced.
(8) As can be seen from the comprehensive examples 1 and 4, in the comparative example 4, the welding surface of the graphite target after sandblasting is subjected to the vacuum magnetron sputtering nickel plating treatment, the welding combination rate of the graphite target obtained by brazing and the backboard is 99.2%, and the combination strength is 3.5MPa, so that the invention proves that the titanium plating layer with a certain thickness is formed on the welding surface of the graphite target by carrying out the vacuum magnetron sputtering titanium plating treatment on the graphite target after sandblasting, the problem of poor solder wettability of the surface of the graphite target can be solved by the titanium plating layer, and the welding combination rate and the welding strength of the graphite target are effectively improved.
In summary, the invention enhances the roughness of the surface of the graphite target by carrying out sand blasting treatment on the graphite target, and then adopts vacuum magnetron sputtering titanium plating treatment to ensure that the titanium film is firmly attached to the surface of the graphite target, thereby improving the problem of poor solder wettability of the surface of the graphite target, ensuring that the welding combination rate of the graphite target obtained by brazing and the backboard reaches more than 99.6 percent, ensuring that the combination strength can reach more than 8.3MPa, and simultaneously solving the problem of desoldering in the use process of the graphite target.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. A method of brazing a graphite target, the method comprising the steps of:
(1) Performing sand blasting on the welding surface of the graphite target material to obtain the graphite target material after sand blasting;
(2) Carrying out vacuum magnetron sputtering titanium plating on the welding surface of the graphite target after sand blasting to obtain a graphite target with a titanium film;
(3) And respectively heating the back plate and the graphite target material with the titanium film, and brazing the heated graphite target material and the back plate.
2. The brazing method according to claim 1, wherein the pressure of the blasting in step (1) is 0.3 to 0.4MPa;
preferably, the sand mould for sand blasting is white corundum;
preferably, the model of the white corundum comprises any one of 24# or 46# or 60# or a combination of at least two of the models;
Preferably, the roughness of the welding surface of the graphite target after sand blasting is 11-14 mu m.
3. The brazing method according to claim 1 or 2, wherein the vacuum degree of vacuum magnetron sputtering titanation in step (2) is 4.0 x10 -3-8.0×10-3 Pa;
Preferably, the sputtering voltage of the vacuum magnetron sputtering titanium plating is 80-120V;
Preferably, the sputtering current of the vacuum magnetron sputtering titanizing is 10-30mA;
Preferably, the sputtering time of the vacuum magnetron sputtering titanium plating is 3-5h;
preferably, the thickness of the titanizing layer of the graphite target material with the titanium film is 2-5 mu m;
preferably, the roughness of the titanizing layer of the graphite target with the titanium film is 10-12 mu m.
4. A brazing method according to any one of claims 1 to 3, wherein the material of the back plate of step (3) comprises any one or a combination of at least two of Al, cu or Mo;
preferably, the target temperature of heating is 200-220 ℃;
preferably, the heating rate is 2-5 ℃ per minute.
5. The method of brazing according to any one of claims 1 to 4, wherein the brazing in step (3) comprises sequentially dipping, fitting, hot pressing and cooling.
6. The brazing method according to claim 5, wherein the infiltrating includes independently placing solder on the bonding face of the graphite target having the titanium film and the bonding face of the backing plate, respectively, for infiltrating;
preferably, the method of infiltration comprises ultrasonic infiltration;
Preferably, the welding surface of the backboard is treated by adopting a rigid brush before the infiltration treatment;
preferably, the infiltration time of the welding surface of the graphite target material with the titanium film is 10-20min;
Preferably, the infiltration time of the welding surface of the backboard is 10-15min;
preferably, the material of the solder includes indium solder.
7. The brazing method according to claim 5 or 6, wherein the bonding comprises manufacturing a solder tank on the welding surface of the back plate, placing copper wires in the solder tank, and bonding the welding surface of the graphite target material and the welding surface of the back plate;
Preferably, the depth of the solder bath is 3-5mm;
preferably, the length and the width of the solder groove are the same as those of the backboard;
Preferably, the diameter of the copper wire is 0.2-0.5mm.
8. The brazing method according to any one of claims 5 to 7, wherein the hot pressing comprises placing a cushion pad on the bonded graphite target and placing a compact on the cushion pad;
preferably, the temperature of the cushion pad is 200-220 ℃;
preferably, the cushion comprises a silica gel pad or a wood block;
preferably, the pressure of the briquette is 0.3-0.5MPa.
9. Brazing method according to any one of claims 5-8, wherein the target temperature of cooling is 25 ℃;
preferably, the cooling is at a rate of 1-2 ℃ per minute.
10. Brazing method according to any one of claims 1-9, characterized in that the brazing method comprises the steps of:
(1) Carrying out sand blasting on the welding surface of the graphite target by using white corundum, wherein the pressure of the sand blasting is 0.3-0.4MPa, and the graphite target with the roughness of 11-14 mu m is obtained;
(2) Vacuum magnetron sputtering titanium plating is carried out on the welding surface of the graphite target after sand blasting under the vacuum degree of 4.0X10 -3-8.0×10-3 Pa, the thickness of the titanium plating layer is 2-5 mu m, and the graphite target with the titanium film and the roughness of 10-12 mu m is obtained;
(3) Heating the back plate and the graphite target material with the titanium film to a target temperature of 200-220 ℃ at a heating rate of 2-5 ℃ per minute, placing molten solder on the welding surface of the graphite target material with the titanium film, infiltrating the welding surface of the graphite target material with an ultrasonic welder for 10-20min, infiltrating the back plate with a manual steel brush and the ultrasonic welder for 10-15min, manufacturing a solder tank with a depth of 3-5mm on the welding surface of the back plate, placing copper wires with a diameter of 0.2-0.5mm in the solder tank, bonding the welding surface of the graphite target material with the welding surface of the back plate, placing a buffer cushion on the bonded graphite target material, placing a pressing block with a pressure of 0.3-0.5MPa on the buffer cushion, cooling the bonded graphite target material and the back plate to 25 ℃ at a cooling rate of 1-2 ℃ per min after welding, and removing the pressing block, thereby completing the brazing of the graphite target material and the back plate.
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| US5428882A (en) * | 1993-04-05 | 1995-07-04 | The Regents Of The University Of California | Process for the fabrication of aluminum metallized pyrolytic graphite sputtering targets |
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