CN118064847A - Low-oxygen-content alloy target and preparation method thereof - Google Patents
Low-oxygen-content alloy target and preparation method thereof Download PDFInfo
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- CN118064847A CN118064847A CN202410394793.3A CN202410394793A CN118064847A CN 118064847 A CN118064847 A CN 118064847A CN 202410394793 A CN202410394793 A CN 202410394793A CN 118064847 A CN118064847 A CN 118064847A
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- 238000004519 manufacturing process Methods 0.000 claims description 6
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Abstract
The invention relates to the technical field of alloy targets, and provides a low-oxygen-content alloy target and a preparation method thereof, wherein the low-oxygen-content alloy target comprises the following steps: preparing alloy powder; uniformly mixing the alloy powder and the binder to form a mixture; placing the mixture into a mould for warm isostatic compaction to form a biscuit; performing catalytic degreasing treatment on the biscuit to form a preform; and (3) carrying out vacuum sintering on the preform to obtain the low-oxygen alloy target. According to the preparation method of the low-oxygen alloy target, the alloy powder and the binder are subjected to temperature isostatic pressing to form the biscuit, and then the biscuit is subjected to catalytic treatment, so that the binder in the biscuit is cracked and removed, metal elements are prevented from being oxidized due to high-temperature degreasing, a low-oxygen prefabricated body can be obtained, and finally the low-oxygen prefabricated body is subjected to vacuum sintering, so that the low-oxygen alloy target can be formed, the formation of air holes can be reduced, and the compactness and the conductivity of a target finished product can be improved.
Description
Technical Field
The invention belongs to the technical field of alloy targets, and particularly relates to a low-oxygen-content alloy target and a preparation method thereof.
Background
For targets, the purity and density of the target are critical to the performance of the target coating. The purity of the target material can directly influence the uniformity and stability of the coating film and the poisoning degree of the target surface in the sputtering process, thereby influencing the service life of the target material. The high-purity alloy target material has requirements for the content of elements such as C, N, O, S besides the content of cationic impurity elements. Oxygen is a common impurity element, which affects the performance and quality of the alloy target. In the process of preparing the alloy target material by adopting powder metallurgy, particularly in the forming process, oxidizing substances can be brought in, so that the oxygen content in the alloy target material exceeds the standard. At present, two methods are commonly used for controlling the oxygen content of an alloy, one is to select a raw material with ultra-low oxygen content and high purity, and the other is to add specific alloying elements to absorb oxygen elements in the manufacturing process. However, the selection of high purity raw materials with ultra-low oxygen content can only be guaranteed in the raw material link, but oxygen still exists in the manufacturing link. By adding specific alloying elements to absorb oxygen elements, these elements can lead to impurity formation. Therefore, how to control the low oxygen content of the alloy target material in the manufacturing link is very critical.
The properties of the green body directly affect the properties of the final product, so in order to achieve good molding when manufacturing alloy targets by powder metallurgy, and assist metal powder to fill a mold, the green body with high density, uniformity and high strength is molded, and commonly used binders such as polyvinyl alcohol (PVA), polyethylene glycol (PEG), paraffin, cellulose and the like are usually required to be added into the powder. However, the addition of the above-mentioned conventional binders to the green body requires a high temperature of 500-600 ℃ air treatment to burn out the green body, which can lead to oxidation of the metal powder during the process, resulting in an increase in oxygen content.
Therefore, there is a need to develop a method for preparing low oxygen content alloy targets.
Disclosure of Invention
The invention aims to provide an alloy target with low oxygen content and a preparation method thereof, and aims to solve the problem that the alloy target prepared by the existing preparation method of the alloy target has high oxygen content.
In order to achieve the above purpose, the invention adopts the following technical scheme:
In a first aspect, the present invention provides a method for preparing a low oxygen content alloy target, comprising the steps of:
preparing alloy powder;
Uniformly mixing the alloy powder and the binder to form a mixture;
placing the mixture into a die for warm isostatic compaction to form a biscuit;
Carrying out catalytic degreasing treatment on the biscuit to form a preform;
And carrying out vacuum sintering on the preform to obtain the low-oxygen alloy target.
In a second aspect, the invention provides a low-oxygen content alloy target, which is prepared by the preparation method of the low-oxygen content alloy target provided by the invention, and the oxygen content of the alloy target is lower than 100ppm.
Compared with the prior art, the invention has the following beneficial effects:
If the oxygen content of the copper gallium or copper indium gallium target preform is higher before vacuum sintering, pores are easily generated in the vacuum sintering stage, the density and strength of the target are affected, the oxidized copper gallium or copper indium gallium in the target preform is reduced to remove oxygen at a very high temperature, the actual operation is very difficult, and the conductivity of the alloy target is affected. Therefore, the alloy target material prepared by the preparation method provided by the invention has the advantages of low oxygen content, good conductivity, good compactness and high strength.
The low-oxygen-content alloy target provided by the second aspect of the invention is prepared by the preparation method of the low-oxygen-content alloy target provided by the invention, and the oxygen content of the alloy target is lower than 100ppm, so that the alloy target has the advantages of good compactness, high strength, good conductivity, high film forming rate, good film uniformity, long service life of the target and the like.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weights of the relevant components mentioned in the description of the embodiments of the present invention may refer not only to the specific contents of the components, but also to the proportional relationship between the weights of the components, so long as the contents of the relevant components in the description of the embodiments of the present invention are scaled up or down within the scope of the disclosure of the embodiments of the present invention. Specifically, the mass described in the specification of the embodiment of the invention can be a mass unit which is known in the chemical industry field such as mu g, mg, g, kg.
The alloy target material is manufactured by the processes of plasma spraying, smelting and casting, hot pressing, hot isostatic pressing, vacuum sintering and the like. For alloy targets (such as CuGa, cuInGa and the like), the targets are easily oxidized when plasma spraying, smelting and casting are adopted; hot pressing or hot isostatic pressing makes it difficult to manufacture long large-sized rotary targets; when a longer large-size rotary target is manufactured by adopting vacuum sintering, a binder needs to be added first to form a high-strength biscuit, then the binder is removed at high temperature, and finally the target is formed by vacuum sintering, however, the binder is removed at high temperature (500-600 ℃) to oxidize metal elements (such as Cu, in, ga and the like) of the biscuit, so that the oxygen content of the biscuit is high, pores are easily generated In the biscuit with high oxygen content In the vacuum sintering stage, the compactness and strength of the target are influenced, the oxygen In the biscuit is difficult to burn out, the oxygen content of the alloy target is high, and the conductivity is poor.
The embodiment of the invention provides a preparation method of a low-oxygen-content alloy target, which comprises the following steps:
s01: preparing alloy powder;
s02: uniformly mixing the alloy powder and the binder to form a mixture;
S03: placing the mixture into a mould for warm isostatic compaction to form a biscuit;
s04: performing catalytic degreasing treatment on the biscuit to form a preform;
s05: and (3) carrying out vacuum sintering on the preform to obtain the low-oxygen alloy target.
If the oxygen content of the copper gallium or copper indium gallium target preform is higher before vacuum sintering, pores are easily generated in the vacuum sintering stage, the density and strength of the target are affected, the oxidized copper gallium or copper indium gallium in the target preform is reduced to remove oxygen at a very high temperature, the actual operation is very difficult, and the conductivity of the alloy target is affected. Therefore, the alloy target material prepared by the preparation method provided by the invention has the advantages of low oxygen content, good conductivity, good compactness and high strength.
In the above step S01, the step of preparing the alloy powder may include: putting the metal sources into a smelting furnace according to a certain proportion, and smelting under vacuum or inert atmosphere at 600-1200 ℃ to obtain alloy melt; and forming alloy powder from the alloy melt by utilizing gas atomization. Wherein, the oxygen content of the metal source is less than 50ppm, and concretely can comprise copper, indium, gallium blocks and the like with the oxygen content less than 50 ppm.
In an embodiment, the step of uniformly mixing the alloy powder and the binder may include: the step of uniformly mixing the alloy powder and the binder comprises the following steps: and (3) placing the alloy powder and the binder in vacuum or inert atmosphere, firstly carrying out low-speed stirring treatment, then starting to heat to a target temperature, converting into high-speed shearing treatment when the temperature is raised to a preset temperature, finally starting to cool from the target temperature, converting into low-speed stirring treatment when the temperature is lowered to the preset temperature, and stopping stirring until the temperature is lowered to below 30 ℃ to obtain the mixture. According to the embodiment of the invention, the alloy powder and the binder are placed under vacuum or inert atmosphere, the low-speed stirring treatment is carried out firstly, then the temperature is raised to dissolve the binder to generate viscosity, and the high-speed shearing treatment is carried out, so that the binder can be prevented from agglomerating, the binder and the alloy powder are well mixed uniformly, finally the binder is solidified through cooling and low-speed stirring to form the material particles of the binder coated alloy powder, the oxidation of the alloy powder can be effectively prevented, the formation of the alloy target with low oxygen content is facilitated, and the difficult problem that the binder is difficult to mix uniformly due to small amount of the binder can be solved.
In a specific embodiment, the step of uniformly mixing the alloy powder and the binder may include: vacuumizing the power mixing device to a slight negative pressure, then introducing N 2 to normal pressure, adding alloy powder and a binder into the power mixing device, simultaneously introducing and discharging N 2 for a period of time, stopping discharging N 2, and continuously introducing N 2 to maintain normal pressure; stirring at a low speed for 10-30 min under the conditions of 500-1500 rpm of dispersing speed, 5-15 rpm of revolution speed and 20-40 rpm of rotation speed, then heating at a speed of 3-5 ℃/min, regulating the dispersing speed to 2500-4000 rpm when the temperature is raised to 140-150 ℃, continuously heating to 200-250 ℃ at the revolution speed of 30-40 rpm and 70-90 rpm of rotation speed, cooling at a speed of 3-5 ℃/min after shearing at a high speed of 20-60 min, regulating the dispersing speed to 500-1500 rpm when the temperature is reduced to 150 ℃, stirring at a low speed when the revolution speed is 5-15 rpm and the rotation speed is 5-15 rpm, and stopping stirring until the temperature is reduced to 20-30 ℃ to obtain the mixture. According to the embodiment of the invention, the adhesive is dissolved to generate viscosity by low-speed stirring and mixing, and then the adhesive is heated to generate high-speed shearing, so that the adhesive can be prevented from agglomerating, the adhesive and the alloy powder are fully and uniformly mixed, finally the adhesive is solidified by cooling and low-speed stirring, the adhesive coated alloy powder material particles can be formed, the alloy powder can be effectively prevented from being oxidized, the alloy target with low oxygen content can be formed, and the difficult problem that the adhesive is less in amount and difficult to uniformly mix can be solved.
In the embodiment, the alloy powder component contains copper and gallium, the mass ratio of the copper to the gallium can be (20-90)/(10-80), specifically, according to the mass ratio of the copper block to the gallium block of 90/10, 60/40, 20/80 and the like, the copper block and the gallium block are put into a smelting furnace to be smelted under vacuum or inert atmosphere at 600-1200 ℃ to obtain copper-gallium alloy melt, and the copper-gallium alloy melt is utilized to form the copper-gallium alloy powder by gas atomization.
In the embodiment, the alloy powder component contains copper, indium and gallium, the mass ratio of copper, indium and gallium can be (20-90)/(5-30)/(5-50), specifically, according to the mass ratio of copper block, indium block and gallium block of 90/5/5, 60/10/30, 20/30/50 and the like, the copper block, indium block and gallium block are put into a smelting furnace, and are smelted under vacuum or inert atmosphere at 600-1200 ℃ to obtain copper indium gallium alloy melt, and the copper indium gallium alloy melt is utilized for forming the copper indium gallium alloy powder by gas atomization.
In the above step S02, the binder is polyoxymethylene. The mass ratio of the alloy powder to the binder is 100/(0.5 to 1.5), preferably 100/(0.3 to 0.8), more preferably 100/(0.3 to 0.6), and even more preferably 100/(0.3 to 0.4).
In the above step S03, the mold is a flexible resin mold. Specifically, the flexible resin mold can be a mold made of polyurethane, natural rubber, silica gel and the like, and the mold made of the materials is favorable for high-pressure deformation of the mixture powder to form a biscuit.
In some embodiments, the temperature of the warm isostatic compaction is 150-200 ℃ and the pressure is 100-300 MPa. The temperature isostatic pressing temperature range can dissolve the binder in the mixture to generate viscosity, and the alloy powder (CuGa alloy powder or CuInGaalloy powder) without plasticity or viscosity is bonded to form a biscuit.
In the step S04, the step of performing the catalytic degreasing treatment on the green body includes: heating the biscuit to 100-150 ℃ in inert atmosphere, then introducing acid, and cracking and removing the binder in the biscuit; wherein the acid is nitric acid or oxalic acid.
Specifically, the binder is Polyoxymethylene (POM), acid is taken as a catalyst, a metering pump is used for pumping the acid into a furnace, the polyoxymethylene in the biscuit can be rapidly cracked into formaldehyde gas in an acid atmosphere of 100-150 ℃, so that the polyoxymethylene is removed from the biscuit, high-temperature degreasing is not needed, metal elements are prevented from being oxidized due to high temperature, compared with a traditional method for removing the binder by calcining air at high temperature, the oxygen content of a preform can be effectively reduced, air holes generated by vacuum sintering of the preform with low oxygen content can be reduced, the density and strength of a target finished product can be improved, the oxygen content of an alloy target finally prepared can be reduced, and the conductivity of the target can be improved. The cracking equation is as follows:
(CH 2 O) n (acidic solution) →nCH 2 O
The formaldehyde gas is generated by burning CO, CO 2 and H 2 O, and the gases are heated by the tail gas processor, so that the CO can be converted into CO 2 to be discharged, and the discharged gas has no pollution to the atmosphere, thereby realizing green emission.
In some embodiments, the acid flow is 1.0 to 5.0g/min, further may be 4.0 to 5.0g/min; the time for cracking and removing is 1-5 h, and further can be 1.5-2.5 h. When oxalic acid is selected as the acid, oxalic acid with the concentration of 10-20% can be selected. When nitric acid is selected as the acid, nitric acid with a concentration of 70-98% can be selected.
In the above step S04, the vacuum sintering temperature is 500 to 800 ℃, and further may be 600 to 700 ℃ and the vacuum degree is 10 -2～10-3 Pa.
The embodiment of the invention provides a low-oxygen-content alloy target, which is prepared by the preparation method of the low-oxygen-content alloy target provided by the invention, and the oxygen content of the alloy target is lower than 100ppm.
The low-oxygen-content alloy target material provided by the embodiment of the invention is prepared by the preparation method of the low-oxygen-content alloy target material, and the oxygen content of the alloy target material is lower than 100ppm, so that the alloy target material has the advantages of good compactness, high strength, good conductivity, high film forming rate, good film uniformity, long service life of the target material and the like.
The following description is made with reference to specific embodiments.
Example 1
The embodiment provides a preparation method of a low-oxygen-content CuGa alloy target, which comprises the following steps:
S11: putting a Cu block and a Ga block into a smelting furnace according to the mass ratio of 7/3, smelting at 1050 ℃ in an inert atmosphere to obtain a CuGa alloy melt, and forming the CuGa alloy melt into CuGa alloy powder by utilizing gas atomization, wherein the oxygen content of the Cu block and the Ga block is less than 50ppm;
S12: vacuumizing the power mixing device to a slight negative pressure, then introducing N 2 to normal pressure, adding the CuGa alloy powder and the polyformaldehyde into the power mixing device according to the mass ratio of the CuGa alloy powder to the polyformaldehyde of 100/0.3, and stopping discharging N 2 and continuously introducing N 2 to maintain the normal pressure after introducing and discharging N 2 for a period of time; stirring at a low speed for 20min under the conditions of 1000rpm for dispersing speed, 10rpm for revolution speed and 30rpm for autorotation speed, then heating at a speed of 5 ℃/min, regulating the dispersing speed to 3000rpm for revolution speed and 30rpm for autorotation speed to 80rpm when heating to 150 ℃, continuously heating to 200 ℃, cooling at a speed of 5 ℃/min after high-speed shearing for 30min, regulating the dispersing speed to 1000rpm when cooling to 150 ℃, regulating the revolution speed to 10rpm for revolution speed and stopping stirring at a low speed until cooling to room temperature to obtain a mixture;
s13: placing the mixture into a polyurethane mould, and performing isostatic compaction at the temperature of 180 ℃ and 200MPa to form a biscuit;
S14: placing the biscuit in a furnace in nitrogen atmosphere, heating to 130 ℃, and then introducing oxalic acid for 2.5 hours at a flow rate of 4.0g/min to crack the polyoxymethylene in the biscuit into formaldehyde gas to separate from the biscuit, so as to obtain a preform;
S15: and (3) carrying out vacuum sintering on the preform for 6 hours at the vacuum degree of 10 -3 Pa and the temperature of 650 ℃ to obtain the CuGa alloy target with low oxygen content.
Example 2
The present embodiment provides a method for preparing a low oxygen content CuGa alloy target, which is different from the method in embodiment 1 in that in step S14, the temperature is heated to 100 ℃, and then oxalic acid is introduced for 2 hours at a flow rate of 4.5 g/min.
Example 3
The embodiment provides a preparation method of a low-oxygen-content CuGa alloy target, which is different from the preparation method in embodiment 1 in that in step S14, heating is performed to 140 ℃, and then oxalic acid is introduced for 1.5 hours at a flow rate of 5 g/min.
Example 4
The present embodiment provides a method for preparing a low oxygen content CuGa alloy target, which has a preparation step different from that of embodiment 1 in that nitric acid is introduced in step S14.
Example 5
The preparation method of the CuInGaalloy target with low oxygen content comprises the following steps:
S51: according to the mass ratio of 7/1/2, the Cu block, the In block and the Ga block are put into a smelting furnace, and are smelted under inert atmosphere and 1050 ℃ to obtain CuInGaalloy melt, and the CuInGaalloy melt is formed into CuInGaalloy powder by utilizing gas atomization;
S52: vacuumizing the power mixing device to a slight negative pressure, then introducing N 2 to normal pressure, adding CuInGa alloy powder and polyformaldehyde into the heating device according to the mass ratio of the CuInGa alloy powder to the polyformaldehyde of 100/0.8, simultaneously introducing and discharging N 2 for a period of time, stopping discharging N 2, and continuing introducing N 2 to maintain normal pressure; stirring at a low speed for 20min under the conditions of 1000rpm for dispersing speed, 10rpm for revolution speed and 30rpm for autorotation speed, then heating at a speed of 5 ℃/min, regulating the dispersing speed to 3000rpm for revolution speed and 30rpm for autorotation speed to 80rpm when heating to 150 ℃, continuously heating to 200 ℃, cooling at a speed of 5 ℃/min after high-speed shearing for 30min, regulating the dispersing speed to 1000rpm when cooling to 150 ℃, regulating the revolution speed to 10rpm for revolution speed and stopping stirring at a low speed until cooling to room temperature to obtain a mixture;
s53: placing the mixture into a polyurethane mould, and performing isostatic compaction at the temperature of 180 ℃ and 200MPa to form a biscuit;
s54: placing the biscuit in a furnace in nitrogen atmosphere, heating to 130 ℃, and then introducing oxalic acid for 2.5 hours at a flow rate of 5.0g/min to crack the polyoxymethylene in the biscuit into formaldehyde gas to separate from the biscuit, so as to obtain a preform;
s55: and (3) carrying out vacuum sintering on the preform for 6 hours at the vacuum degree of 10 -3 Pa and the temperature of 650 ℃ to obtain the CuInGaalloy target with low oxygen content.
Example 6
The preparation method of the CuInGaalloy target with low oxygen content is different from that of the embodiment 5 in that oxalic acid is introduced into the preparation method in the step S52 according to the mass ratio of 100/0.5 and the flow rate of 4.5g/min in the step S54 for 2h.
Comparative example 1
The preparation method of the CuGa alloy target comprises the following steps:
S1: mixing a Cu block and a Ga block according to the mass ratio of 7/3 to form a CuGa mixture, placing the CuGa mixture in an alumina crucible, vacuumizing a smelting chamber to 3X 10 -2 Pa, filling argon into a furnace washing furnace, vacuumizing again, recharging argon to enable the furnace pressure to be 0.08MPa, heating the CuGa mixture at 600 ℃ for 20min, then heating to 1050 ℃, and refining for 3min at 950 ℃ to obtain a CuGa melt;
S2: preheating a graphite mold and an alumina funnel in an oven at 300 ℃ for 1h, casting a CuGa melt into the graphite mold, naturally cooling to room temperature, and demolding to obtain an ingot;
S3: cutting the cast ingot and polishing to obtain the CuGa alloy target material.
Comparative example 2
The preparation method of the CuGa alloy target comprises the following steps:
S1: putting a Cu block and a Ga block into a smelting furnace according to the mass ratio of 7/3, smelting at 1050 ℃ in an inert atmosphere to obtain a CuGa alloy melt, and forming the CuGa alloy melt into CuGa alloy powder by utilizing gas atomization, wherein the oxygen content of the Cu block and the Ga block is less than 50ppm;
S2: loading CuGa alloy powder into a graphite die for leveling;
S3: putting the powder into a vacuum hot pressing furnace, and cold-prepressing the powder under the pressure of 8 Mpa; vacuumizing the hot-pressing furnace, starting heating when the vacuum degree reaches 0.1pa, heating to 650 ℃ at 4 ℃/min, preserving heat for 1.5 hours, pressurizing at 650 ℃ with the pressure of 55Mpa, maintaining for 2 hours, discharging the pressurized pressure, naturally reducing the pressure at 650 ℃ for 1 hour, cooling at the natural reduced pressure, starting reducing the pressure after the temperature is reduced to 250 ℃, and naturally cooling to below 35 ℃ after the pressure is reduced to 10 MPa;
S3: and (5) after demoulding, carrying out mechanical processing to obtain the CuGa alloy target.
Comparative example 3
The preparation method of the CuGa alloy target comprises the following steps:
s1: according to the mass ratio of 7/3, putting a metal Cu block and a metal Ga block into a smelting furnace, smelting under inert atmosphere and 1050 ℃ to obtain a CuGa alloy melt, and forming the CuGa alloy melt into CuGa alloy powder by utilizing gas atomization;
S2: vacuumizing the power mixing device to a slight negative pressure, then introducing N 2 to normal pressure, adding the CuGa alloy powder and the polyvinyl alcohol into the power mixing device according to the mass ratio of the CuGa alloy powder to the polyvinyl alcohol of 100/0.5, simultaneously introducing and discharging N 2 for a period of time, stopping discharging N 2, and continuously introducing N 2 to maintain the normal pressure; stirring at a low speed for 20min under the conditions of 1000rpm for dispersing speed, 10rpm for revolution speed and 30rpm for autorotation speed, then heating at a speed of 5 ℃/min, regulating the dispersing speed to 3000rpm for revolution speed and 30rpm for autorotation speed to 80rpm when heating to 150 ℃, continuously heating to 200 ℃, cooling at a speed of 5 ℃/min after high-speed shearing for 30min, regulating the dispersing speed to 1000rpm when cooling to 150 ℃, regulating the revolution speed to 10rpm for revolution speed and stopping stirring at a low speed until cooling to room temperature to obtain a mixture;
S3: placing the mixture into a polyurethane mold, and performing cold isostatic pressing molding under 200MPa to form a biscuit;
s4: placing the biscuit in a nitrogen atmosphere at 550 ℃ for degreasing for 24 hours, and burning and removing polyvinyl alcohol in the biscuit to obtain a preform;
S5: and (3) carrying out vacuum sintering on the preform for 6 hours at the vacuum degree of 10 -3 Pa and the temperature of 650 ℃ to obtain the CuGa alloy target with low oxygen content.
The alloy targets prepared in examples 1 to 5 and comparative examples 1 to 3 were subjected to tests for purity, relative density, oxygen content and resistivity, and the test results are shown in table 1.
TABLE 1
As is clear from Table 1, the alloy targets produced in examples 1 to 6 of the present invention did not develop cracks, whereas the alloy target produced in comparative example 1 had microcracks, indicating that the method of casting in comparative example 1 was not suitable for producing an alloy target. The oxygen content and the resistivity of the alloy targets prepared In the embodiments 1-6 are obviously lower than those of the alloy targets prepared In the comparative examples 1-3, the density and the purity of the alloy targets prepared In the embodiments 1-6 are obviously higher than those of the alloy targets prepared In the comparative examples 1-3, and the embodiment of the invention is illustrated that the alloy powder and the binder are mixed, then the binder In the mixture is dissolved through warm isostatic pressing to generate viscosity, the CuGa or CuInGaalloy powder without plasticity or viscosity is bonded to form a biscuit, the biscuit is subjected to catalytic treatment to crack and remove the binder, and the Cu, in and Ga metal elements are prevented from being oxidized due to high-temperature degreasing, so that a low-oxygen-content prefabricated body can be formed, and finally the low-oxygen-content prefabricated body is subjected to vacuum sintering, so that the low-oxygen-content alloy targets can be formed, the formation of pores is effectively reduced, and the density and the strength of the alloy targets are improved.
The foregoing description is only of the preferred embodiments of the invention and is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (10)
1. The preparation method of the low-oxygen-content alloy target is characterized by comprising the following steps of:
preparing alloy powder;
Uniformly mixing the alloy powder and the binder to form a mixture;
placing the mixture into a die for warm isostatic compaction to form a biscuit;
Carrying out catalytic degreasing treatment on the biscuit to form a preform;
And carrying out vacuum sintering on the preform to obtain the low-oxygen alloy target.
2. The method of claim 1, wherein the step of uniformly mixing the alloy powder and the binder comprises: and placing the alloy powder and the binder in vacuum or inert atmosphere, firstly carrying out low-speed stirring treatment, then starting to heat to a target temperature, converting into high-speed shearing treatment when the temperature is raised to a preset temperature, finally starting to cool from the target temperature, converting into low-speed stirring treatment when the temperature is lowered to the preset temperature, and stopping stirring until the temperature is lowered to below 30 ℃ to obtain the mixture.
3. The method of claim 1, wherein the step of subjecting the greenbody to catalytic degreasing treatment comprises: heating the biscuit to 100-150 ℃ in inert atmosphere, then introducing acid, and cracking and removing the binder in the biscuit; wherein the acid is nitric acid or oxalic acid.
4. The method according to claim 3, wherein the acid flow rate is 1.0 to 5.0g/min;
The time for cracking and removing is 1-5 h.
5. The preparation method according to claim 1, wherein the mass ratio of the alloy powder to the binder is 100/(0.5-1.5);
And/or the binder is polyoxymethylene.
6. The method according to claim 3, wherein the temperature of the isostatic pressing is 150-200 ℃ and the pressure is 100-300 MPa.
7. The method according to claim 3, wherein the vacuum sintering temperature is 500 to 800 ℃ and the vacuum degree is 10 -2～10-3 Pa.
8. The method according to any one of claims 1 to 7, wherein the alloy powder component contains copper and gallium.
9. The method according to any one of claims 1 to 7, wherein the alloy powder component contains copper, indium and gallium.
10. A low oxygen content alloy target, characterized in that the low oxygen content alloy target is produced by the production method according to any one of claims 1 to 9, and the oxygen content of the alloy target is lower than 100ppm.
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