Method for reusing residual molybdenum target

Abstract

The present invention belongs to the technical field of sputtering target materials, and specifically relates to a method for recycling molybdenum residual targets, the method comprising the following steps: (1) cutting the molybdenum residual targets into molybdenum blocks; (2) performing surface pretreatment on the molybdenum blocks obtained in step (1); (3) performing vacuum plasma spraying on the molybdenum blocks obtained in step (2); (4) mixing the molybdenum blocks obtained in step (3) with molybdenum powder and loading them into a rubber sleeve mold for compression molding; (5) sintering the compressed molybdenum blank obtained in step (4); (6) thermoplastic deformation of the sintered molybdenum blank obtained in step (5) to obtain a molybdenum metal product. The method for recycling molybdenum residual targets of the present invention has a molybdenum residual target recovery rate of more than 95%, and the purity of the prepared molybdenum metal product reaches more than 99.95wt%, which meets the index requirements of target material preparation, realizes the recycling of target materials, and has a simple process and low cost, which meets the requirements of industrial promotion and use.

Description

Technical Field

[0001] The invention belongs to the technical field of sputtering target materials, and in particular relates to a method for recycling molybdenum residual targets. Background Art

[0002] Molybdenum is a precious and rare refractory metal with excellent physical and chemical properties such as high thermal conductivity, high electrical conductivity, low thermal expansion coefficient, high high temperature strength, good wear resistance, strong corrosion resistance and stable chemical properties. Molybdenum metal plays a pivotal role in the electronics, information industry and glass coating fields, such as integrated circuits, information storage, liquid crystal displays, solar cells, laser storage, electronic control devices, etc. In these fields, molybdenum metal is mainly used as a target for sputtering thin films.

[0003] Molybdenum targets are usually used by magnetron sputtering, and the targets after use are called residual targets. Due to the influence of magnetic field distribution, the consumption of molybdenum target surface is very uneven, which ultimately results in a very low utilization rate of the target, about 40%. Molybdenum, as a rare and refractory metal, is a strategic resource, and its reasonable development and reuse are of great significance.

[0004] The Chinese invention patent application with publication number CN114395700A discloses a molybdenum blank and its preparation method and application. The preparation method comprises the following steps: cleaning the target material scraps in sequence and performing vacuum electron beam melting at least twice to obtain the molybdenum blank. The purity of the molybdenum blank is ≥99.95%. The preparation method provided by the invention is simple and highly operable. The molybdenum scraps of the target material can be effectively treated by organically combining the cleaning process with the vacuum electron beam melting process, fully realizing the utilization value of the molybdenum scraps and realizing the recycling of molybdenum resources. However, the patent uses molybdenum target scraps to prepare molybdenum blanks through pickling, water washing, soaking, drying and vacuum electron beam melting. The melting point of molybdenum is 2620°C. The energy consumption of electron beam melting is extremely high, and multiple meltings are required to ensure the purity of the product, and the production cost is extremely high. In addition, the size of the prepared molybdenum blank is limited by the crucible and can only be cylindrical, which is inconvenient for later processing and difficult to promote industrialization.

[0005] A Chinese patent with announcement number CN110331368B discloses a method for producing a beveled circular molybdenum target, including particle size analysis, bulk density and purity detection of high-purity molybdenum powder, screening of molybdenum powder, mixing of molybdenum powder, filling and tightening of molds, cold isostatic pressing, demolding, sintering, hot rolling, machining, cleaning and packaging. The method for producing a beveled circular molybdenum target of the invention has high purity, high density and finer grains. However, the invention adopts the traditional powder metallurgy method to prepare the molybdenum target, and the raw materials are all raw molybdenum powder, which has a high production cost, which is different from the reuse of molybdenum residual targets in the present application, and is limited to the preparation of beveled circular molybdenum targets, and its industrial application is limited. Summary of the invention

[0006] In order to overcome the above-mentioned defects, the purpose of the present invention is to provide a method for recycling molybdenum residual targets, which has high recovery rate and high purity, realizes the recycling of target materials, and has simple process and low cost, and can be promoted and used industrially.

[0007] To achieve the above object, the present invention adopts the following technical solution:

[0008] A method for recycling a residual molybdenum target comprises the following steps:

[0009] (1) Cutting the molybdenum residual target into molybdenum blocks;

[0010] (2) performing surface pretreatment on the molybdenum block obtained in step (1);

[0011] (3) vacuum plasma spraying the molybdenum block obtained in step (2);

[0012] (4) mixing the molybdenum block obtained in step (3) with the molybdenum powder and placing it into a rubber sleeve mold for compression molding;

[0013] (5) sintering the pressed molybdenum blank obtained in step (4);

[0014] (6) The sintered molybdenum blank obtained in step (5) is thermoplastically deformed to obtain a molybdenum metal product.

[0015] Preferably, the purity of the molybdenum residual target in step (1) is ≥99.95wt%, and the density is ≥99%.

[0016] Preferably, the dimensions of the molybdenum block in step (1) are: thickness 5-30 mm, width 5-100 mm, and length 5-500 mm.

[0017] Preferably, the surface pretreatment described in step (2) includes: surface passivation and surface cleaning. First, the surface passivation is performed, and the molybdenum block is subjected to surface sandblasting, and the sand particle size used for the sandblasting is -400 mesh; then the surface cleaning is performed, that is, the molybdenum block is subjected to alkali washing, acid washing and drying in sequence, and the alkali washing is performed using a 3-5% concentration of sodium hydroxide solution for cleaning, and then washed with water for neutralization; the acid washing is performed using a 1-2% concentration of nitric acid or hydrochloric acid solution for cleaning, and then washed with water for neutralization; the drying temperature is 80-90°C, and the time is 1-3h.

[0018] Preferably, the vacuum plasma spraying in step (3) is to spray a high-purity molybdenum film layer with a thickness of 0.1-0.3 mm on the surface of the molybdenum block by a vacuum plasma spraying device.

[0019] Preferably, the purity of the molybdenum powder in step (4) is ≥99.95% and the particle size is 2.5-4 μm.

[0020] Preferably, the mass ratio of the molybdenum block to the molybdenum powder in step (4) is 5-25:75-95.

[0021] Preferably, the pressing process described in step (4) comprises: firstly, loading the molybdenum block and the molybdenum powder into the rubber mold in sequence, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and then performing cold isostatic pressing. The cold isostatic pressing process conditions are: pressing pressure 200-230MPa, holding time 5-10min, and finally releasing the pressure and demolding to obtain a pressed molybdenum blank with the molybdenum block wrapped in the middle.

[0022] Preferably, the sintering in step (5) comprises: high-temperature sintering the pressed molybdenum billet in a vacuum or hydrogen protective atmosphere, wherein the high-temperature sintering temperature is 1830-1980° C. and the holding time is 6-12 hours.

[0023] Preferably, the thermoplastic deformation in step (6) is forging and / or rolling, and the total deformation amount of the plastic deformation is 45-80%.

[0024] Molybdenum is a scarce and key strategic resource. Pure molybdenum metal products include molybdenum targets, molybdenum plates, molybdenum rods, molybdenum wires, molybdenum special-shaped parts, etc., which are widely used in the fields of electronic information, solar photovoltaics, high-temperature thermal fields, rare earth permanent magnets, aerospace, etc. At present, most pure molybdenum products are prepared through pressing, demolding, sintering, and thermoplastic deformation process steps, and there is no public disclosure of the relevant technology for recycling waste after use. The organizational properties of molybdenum plates, molybdenum rods, molybdenum wires, and molybdenum special-shaped parts change after use, and the purity and shape are also uneven. The cost of recycling is high and the value is low. Molybdenum residual target refers to the target material of the molybdenum target material after use by magnetron sputtering. The organization and purity of the molybdenum target material after use do not change, and it remains in a good state. The main change is the surface morphology, so the recycling value is high. The present invention directly cuts the molybdenum residual target into pieces for recycling and preparation of molybdenum metal products, and the following positive and beneficial effects are achieved:

[0025] 1. The surface passivation of the present invention is to perform surface sandblasting on the molybdenum block, and the surface of the molybdenum block is passivated by the process of surface sandblasting. After the sandblasting, the surface is cleaned. The surface cleaning is to perform alkali washing, acid washing and drying on the molybdenum block in sequence to remove residual impurities on the surface of the molybdenum block. After the surface pretreatment, it is beneficial to improve the bonding strength between the molybdenum film layer and the molybdenum block substrate during vacuum plasma spraying. The formed molybdenum film layer plays the role of an intermediate bonding layer. Its wetting bonding with molybdenum powder is greater than the direct bonding between molybdenum powder and molybdenum block, which greatly improves the diffusion rate during the sintering process, and it is easy to realize the strong bonding of molybdenum powder and molybdenum block atoms into one. In addition, vacuum plasma spraying further avoids the introduction of impurities during the reuse of molybdenum residual targets, thereby ensuring the purity of the final molybdenum metal product.

[0026] 2. In the pressing process of the present invention, the molybdenum block and the molybdenum powder are sequentially loaded into the rubber mold to ensure that the molybdenum block is distributed in the middle of the molybdenum powder and is completely wrapped by the molybdenum powder. The molybdenum block replaces a part of the molybdenum powder raw material, reducing the production cost. Since the molybdenum block is a dense body, the shrinkage of the molybdenum powder and the molybdenum block mixture during the pressing process will become smaller, so it is more advantageous for the size control of the pressed blank, and the size of the rubber sleeve mold can be reduced, which is convenient for pressing; the cold isostatic pressing pressure is 200-230MPa, and the holding time is 5-10min, so that the molybdenum film layer on the surface of the molybdenum block and the molybdenum powder first form a preliminary physical bond, which provides the necessary foundation for the atomic diffusion to form an overall interface bond during the high-temperature sintering process. Then, high-temperature sintering is used to make the interface between the molybdenum film layer and the molybdenum powder fully diffuse, and form a strong interface diffusion bond. The integral sintered molybdenum blank finally prepared has a density that can meet the subsequent thermoplastic deformation requirements, avoid crack defects, and finally obtain a molybdenum metal product to meet the requirements of industrial promotion and application.

[0027] 3. The method for recycling molybdenum residual targets of the present invention does not require complex processes such as oxidation treatment, roasting, ammonia immersion, and evaporation, and has a short flow and simple process. The present invention directly cuts into molybdenum blocks, and also avoids the cumbersome steps of re-preparing into molybdenum powder and the problem of low recovery rate of re-preparing into molybdenum powder. The molybdenum residual targets can be recycled through surface pretreatment, vacuum plasma spraying, compression molding, sintering, and thermoplastic deformation, thereby improving the use value of the molybdenum residual targets, reducing the preparation cost of the target material and improving the use value of the target material, avoiding excessive waste of molybdenum resources, and achieving a comprehensive recovery rate of more than 95%, with a high recovery rate. Moreover, the purity of the prepared molybdenum metal product reaches more than 99.95wt%, which meets the index requirements of target material preparation and realizes the recycling of target materials. At the same time, the equipment investment is small, the cost is low, there is no environmental pollution and high energy consumption problems, and it is more in line with the needs of industrial promotion. DETAILED DESCRIPTION

[0028] The present invention is further described below in conjunction with some specific embodiments.

[0029] Example 1

[0030] A method for recycling a residual molybdenum target comprises the following steps:

[0031] (1) Cutting a molybdenum residual target with a purity of ≥99.95wt% and a density of ≥99% into molybdenum blocks with a size of 8mm*25mm*200mm;

[0032] (2) The molybdenum block obtained in step (1) is subjected to surface pretreatment, firstly, the surface is passivated, and the surface of the molybdenum block is subjected to surface sandblasting, wherein the sand particle size used for the sandblasting is -400 mesh; then the surface is cleaned, and alkali washing, acid washing and drying are performed in sequence to obtain a clean molybdenum block; the alkali washing is performed by using a 3% sodium hydroxide solution for cleaning, and then washing and neutralizing with water; the acid washing is performed by using a 1% hydrochloric acid solution for cleaning, and then washing and neutralizing with water; the drying temperature of the molybdenum block is 80° C., and the time is 1 hour;

[0033] (3) spraying a layer of high-purity molybdenum film with a thickness of 0.1 mm on the surface of the molybdenum block obtained in step (2) through a vacuum plasma spraying device, wherein the purity is ≥ 99.95 wt %;

[0034] (4) putting the molybdenum block obtained in step (3) together with molybdenum powder into a rectangular rubber mold, wherein the purity of the molybdenum powder is ≥99.95% and the particle size is 4 μm, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and the weight ratio of the molybdenum block to the molybdenum powder is 10:90, and then pressing and molding by cold isostatic pressing, finally releasing the pressure and demolding, the pressing pressure is 210 MPa, and the pressure holding time is 5 min;

[0035] (5) sintering the pressed molybdenum blank obtained in step (4) at a high temperature in a hydrogen atmosphere at a sintering temperature of 1830° C. for a holding time of 10 h to finally obtain a sintered molybdenum blank;

[0036] (6) The sintered molybdenum billet obtained in step (5) is hot rolled at a rolling temperature of 1280° C. and a total deformation of 60%.

[0037] Example 2

[0038] A method for recycling a residual molybdenum target comprises the following steps:

[0039] (1) Cutting a molybdenum residual target with a purity of ≥99.95wt% and a density of ≥99.5% into molybdenum blocks with a size of 8mm*8mm*150mm;

[0040] (2) The molybdenum block obtained in step (1) is subjected to surface pretreatment, firstly, surface passivation is performed, that is, the molybdenum block is subjected to surface sandblasting treatment, and the sand particle size used for the sandblasting treatment is -400 mesh; then, the surface is cleaned, and alkali washing, acid washing and drying are performed in sequence to obtain a clean molybdenum block; the alkali washing is performed by using a 4% concentration of sodium hydroxide solution for washing, and then washing and neutralizing with water; the acid washing is performed by using a 1.5% concentration of nitric acid solution for washing, and then washing and neutralizing with water; the drying temperature of the molybdenum block is 85° C., and the time is 2 hours;

[0041] (3) spraying a layer of high-purity molybdenum film with a thickness of 0.2 mm on the surface of the molybdenum block obtained in step (2) through a vacuum plasma spraying device, wherein the purity is ≥99.95wt%;

[0042] (4) putting the molybdenum block obtained in step (3) together with molybdenum powder into a rectangular rubber mold, wherein the purity of the molybdenum powder is ≥99.95% and the particle size is 3 μm, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and the weight ratio of the molybdenum block to the molybdenum powder is 20:80, and then pressing and molding by cold isostatic pressing, and finally releasing the pressure and demolding, the pressing pressure is 230 MPa, and the pressure holding time is 8 min;

[0043] (5) sintering the pressed molybdenum blank obtained in step (4) under vacuum conditions at a high temperature of 1870° C. for a holding time of 10 h to finally obtain a sintered molybdenum blank;

[0044] (6) The sintered molybdenum billet obtained in step (5) is forged at a forging temperature of 1260° C. and a total deformation of 70%.

[0045] Example 3

[0046] A method for recycling a residual molybdenum target comprises the following steps:

[0047] (1) Cutting a molybdenum residual target with a purity of ≥99.95wt% and a density of ≥99.5% into molybdenum blocks with a size of 15mm*40mm*250mm;

[0048] (2) The molybdenum block obtained in step (1) is subjected to surface pretreatment, firstly, surface passivation is performed, that is, the molybdenum block is subjected to surface sandblasting treatment, and then the above-mentioned surface cleaning is performed after the sandblasting treatment; the sand particle size used for the sandblasting treatment is -400 mesh; then the surface is cleaned, and alkali washing, acid washing and drying are performed in sequence to obtain a clean molybdenum block; the alkali washing is performed by using a 4.5% concentration of sodium hydroxide solution for washing, and then washing and neutralizing with water; the acid washing is performed by using a 2% concentration of nitric acid solution for washing, and then washing and neutralizing with water; the drying temperature of the molybdenum block is 88° C., and the time is 3 hours;

[0049] (3) spraying a layer of high-purity molybdenum film with a thickness of 0.2 mm on the surface of the molybdenum block obtained in step (2) through a vacuum plasma spraying device, wherein the purity is ≥99.95wt%;

[0050] (4) putting the molybdenum block obtained in step (3) together with molybdenum powder into a rectangular rubber mold, wherein the purity of the molybdenum powder is ≥99.95% and the particle size is 2.5 μm, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and the weight ratio of the molybdenum block to the molybdenum powder is 25:75, and then pressing and molding by cold isostatic pressing, and finally releasing the pressure and demolding, the pressing pressure is 220 MPa, and the pressure holding time is 10 min;

[0051] (5) sintering the pressed molybdenum blank obtained in step (4) at a high temperature in a hydrogen atmosphere at a sintering temperature of 1930° C. for a holding time of 6 h, to finally obtain a sintered molybdenum blank;

[0052] (6) The sintered molybdenum billet obtained in step (5) is hot rolled at a rolling temperature of 1300° C. and a total deformation of 45%.

[0053] Example 4

[0054] A method for recycling a residual molybdenum target comprises the following steps:

[0055] (1) Cutting a molybdenum residual target with a purity of ≥99.95wt% and a density of ≥99.3% into molybdenum blocks with a size of 7mm*7mm*7mm;

[0056] (2) The molybdenum block obtained in step (1) is subjected to surface pretreatment, firstly, surface passivation is performed, that is, the molybdenum block is subjected to surface sandblasting treatment, and the sand particle size used for the sandblasting treatment is -400 mesh; then the surface is cleaned, and alkali washing, acid washing and drying are performed in sequence to obtain a clean molybdenum block; the alkali washing is performed by using a 4% concentration sodium hydroxide solution for cleaning, and then washing and neutralizing with water; the acid washing is performed by using a 1.2% concentration hydrochloric acid solution for cleaning, and then washing and neutralizing with water; the drying temperature of the molybdenum block is 90° C., and the time is 2 hours;

[0057] (3) spraying a layer of high-purity molybdenum film with a thickness of 0.1 mm on the surface of the molybdenum block obtained in step (2) through a vacuum plasma spraying device, wherein the purity is ≥ 99.95 wt %;

[0058] (4) putting the molybdenum block obtained in step (3) together with molybdenum powder into a rectangular rubber mold, wherein the purity of the molybdenum powder is ≥99.95% and the particle size is 3 μm, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and the weight ratio of the molybdenum block to the molybdenum powder is 5:95, and then pressing and molding by cold isostatic pressing, and finally releasing the pressure and demolding, the pressing pressure is 200 MPa, and the pressure holding time is 10 min;

[0059] (5) sintering the pressed molybdenum billet obtained in step (4) at a high temperature in a hydrogen atmosphere at a sintering temperature of 1980° C. for a holding time of 8 h, to finally obtain a sintered molybdenum billet;

[0060] (6) Forging the sintered molybdenum billet obtained in step (5) at a forging temperature of 1250° C. and a total deformation of 50%.

[0061] Example 5

[0062] A method for recycling a residual molybdenum target comprises the following steps:

[0063] (1) Cutting a molybdenum residual target with a purity of ≥99.95wt% and a density of ≥99.5% into molybdenum blocks with a size of 20mm*60mm*350mm;

[0064] (2) The molybdenum block obtained in step (1) is subjected to surface pretreatment, firstly, surface passivation is performed, that is, the molybdenum block is subjected to surface sandblasting treatment, and then the surface cleaning is performed after the sandblasting treatment; the sand particle size used for the sandblasting treatment is -400 mesh; then the surface is cleaned, and alkali washing, acid washing and drying are performed in sequence to obtain a clean molybdenum block; the alkali washing is performed by using a 5% concentration of sodium hydroxide solution for cleaning, and then washing and neutralizing with water; the acid washing is performed by using a 1.5% concentration of nitric acid solution for cleaning; the drying temperature of the molybdenum block is 90° C., and the time is 2 hours;

[0065] (3) spraying a layer of high-purity molybdenum film with a thickness of 0.3 mm on the surface of the molybdenum block obtained in step (2) through a vacuum plasma spraying device, wherein the purity is ≥ 99.95 wt %;

[0066] (4) putting the molybdenum block obtained in step (3) together with molybdenum powder into a rectangular rubber mold, wherein the purity of the molybdenum powder is ≥99.95% and the particle size is 2.5 μm, the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder, and the weight ratio of the molybdenum block to the molybdenum powder is 22:78, and then pressing and molding are carried out by cold isostatic pressing, and finally the pressure is released and demolding is carried out, the pressing pressure is 210 MPa, and the pressure holding time is 10 min;

[0067] (5) sintering the pressed molybdenum blank obtained in step (4) under vacuum conditions at a high temperature of 1940° C. for a holding time of 12 h to obtain a sintered molybdenum blank;

[0068] (6) The sintered molybdenum billet obtained in step (5) is first forged and then hot rolled, the forging temperature is 1300° C., the hot rolling temperature is 1260° C., and the total deformation is 80%.

[0069] GDMS was used to detect the purity of the molybdenum products obtained in Examples 1-5, and the recovery rate of the molybdenum residual target was calculated, wherein the recovery rate of the molybdenum residual target was calculated by dividing the weight M2 of the molybdenum product obtained by sintering by the weight M1 of the initial molybdenum residual target. The recovery rate of the molybdenum residual target was: (M2*A / M1)×100%, where A was the proportion of the doped molybdenum residual target. The results were shown in Table 1 below.

[0070] Table 1 Performance test results of molybdenum metal products in various embodiments of the present invention

[0071]

[0072]

[0073] As can be seen from Table 1, the purity of the molybdenum product prepared by the present invention reaches more than 99.95wt%, which meets the index requirements for target material preparation and can also meet the needs of other industries.

[0074] The present invention reduces the preparation cost of the target material and improves the use value of the target material by recycling the target material, avoids excessive waste of molybdenum resources, and achieves a comprehensive recovery rate of more than 95%. At the same time, the equipment investment is small and the process flow is simple. Compared with the existing technology, there is no environmental pollution and high energy consumption problem, which is more in line with the needs of industrialization.

[0075] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Other modifications or equivalent substitutions made to the technical solution of the present invention by ordinary technicians in the field should be included in the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solution of the present invention.

Claims

1. A method for recycling molybdenum residual targets, characterized in that: The following steps are involved: (1) Cutting the molybdenum residual target into molybdenum blocks; (2) performing surface pretreatment on the molybdenum block obtained in step (1); (3) vacuum plasma spraying the molybdenum block obtained in step (2); (4) mixing the molybdenum block obtained in step (3) with molybdenum powder and placing them into a rubber sleeve mold for pressing; (5) sintering the pressed molybdenum blank obtained in step (4); (6) thermoplastically deforming the sintered molybdenum blank obtained in step (5) to obtain a molybdenum metal product; The purity of the molybdenum residual target in step (1) is ≥99.95wt% and the density is ≥99%; The dimensions of the molybdenum block in step (1) are: thickness 5-30 mm, width 5-100 mm, and length 5-500 mm; The vacuum plasma spraying in step (3) is to spray a layer of high-purity molybdenum film with a thickness of 0.1-0.3 mm on the surface of the molybdenum block by vacuum plasma spraying equipment; The purity of the molybdenum powder in step (4) is ≥99.95% and the particle size is 2.5-4 μm; The mass ratio of the molybdenum block to the molybdenum powder in step (4) is 5-25:75-95; The pressing process described in step (4) comprises: firstly, loading the molybdenum block and the molybdenum powder into the rubber mold in sequence, wherein the molybdenum block is evenly distributed in the molybdenum powder and is completely wrapped by the molybdenum powder; then, cold isostatic pressing is performed; the cold isostatic pressing process conditions are: pressing pressure 200-230 MPa, holding time 5-10 min; finally, releasing the pressure and demolding to obtain a pressed molybdenum blank with the molybdenum block wrapped in the middle.

2. The method for recycling molybdenum target residues according to claim 1, characterized in that: The surface pretreatment described in step (2) includes: surface passivation and surface cleaning. First, the surface passivation is performed, and the molybdenum block is subjected to surface sandblasting treatment, and the sand particle size used for the sandblasting treatment is -400 mesh; then the surface cleaning is performed, that is, the molybdenum block is subjected to alkali washing, acid washing and drying in sequence, and the alkali washing is performed using a 3-5% concentration of sodium hydroxide solution for washing, and then washing and neutralizing with water; the acid washing is performed using a 1-2% concentration of nitric acid or hydrochloric acid solution for washing, and then washing and neutralizing with water; the drying temperature is 80-90°C, and the time is 1-3h.

3. The method for recycling molybdenum target residues according to claim 1, characterized in that: The sintering in step (5) includes: sintering the pressed molybdenum billet at high temperature in a vacuum or hydrogen protective atmosphere, wherein the high temperature sintering temperature is 1830-1980° C. and the holding time is 6-12 hours.

4. The method for recycling molybdenum target residues according to claim 1, characterized in that: The thermoplastic deformation in step (6) is forging and / or rolling, and the total deformation of the thermoplastic deformation is 45-80%.

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