Recycling and remanufacturing of ito waste target and method

Abstract

The application belongs to the technical field of target material recycling, and discloses a method for recycling and preparing target material from ITO waste target. The method comprises the following steps: acid pickling, heating and evaporating, cooling and powder collecting of the ITO waste target to obtain powder, mixing and grinding the powder and pure water to obtain slurry one, wherein the mass ratio of the powder and the pure water is 0.4-0.6:1, then adding a binder to the slurry one and stirring, wherein the mass ratio of the added amount of the binder and the slurry one is 2-5:100, and finally spray granulating, pressing and sintering the slurry two to obtain the target material prepared from the ITO waste target. The target material prepared from the ITO waste target by the method has a relatively low cracking rate, a relatively high relative density and a relatively high resistivity. In addition, the application also discloses a target material prepared from ITO waste target.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of target material recycling, and particularly relates to an ITO waste target recycling and target material preparation method. BACKGROUND

[0002] Indium is a semiconductor rare metal, and its reserves in nature are relatively small. With the development of the electronic industry, the demand for indium is increasing, so the recycling of indium is becoming more and more important. ITO target material is the main consumer of indium, and has accounted for more than 75% of the total consumption of indium. However, the utilization rate of ITO target material sputtering film is generally about 60%, and the rest is waste target, so the recycling of ITO waste target material is particularly important, which not only realizes resource recycling, but also has huge economic benefits.

[0003] Chinese patent application 202110242917.2 discloses a high-efficiency ITO waste target recycling method, which comprises the following steps: S1, cleaning: wiping the surface of the ITO waste target with acetone, then cleaning with ultrasonic waves, and drying for standby; S2, arc gasification: placing the cleaned ITO waste target into a direct current arc gasification reaction chamber, and introducing an arc generated by a 100□200V direct current to melt and gasify the ITO waste target; S3, powder recovery: quenching the gasified ITO waste target, and then passing through a grading powder recovery system to obtain ITO powder; the scheme adopts a direct current arc method to gasify the waste target material and then recycle and reuse it. This method does not need to go through any metal separation and refining process, the ITO waste target is directly converted into nano ITO powder, in addition, the direct current arc method does not cause waste of the noble metals In and Sn, is environmentally friendly and energy-saving, and the directly generated ITO alloy powder can be directly used to manufacture ITO target material. The ITO waste target is melted and gasified, and after quenching, ITO powder is obtained through rapid nucleation, crystallization and growth. In the recycling process, no other impurities are introduced, the purity of the ITO powder depends on the original purity of the ITO waste target, so the recovery rate of In is relatively high, generally more than 98%;

[0004] It can be seen that the scheme discloses how to recycle ITO waste targets and how to prepare ITO powder, but it can be seen from the scheme that the scheme does not specifically explain how to use the recycled powder to prepare a target.

[0005] Chinese patent application 201511032741.9 discloses a preparation method of high relative density low resistivity indium tin oxide target material, which takes indium, tin tetrachloride and nitric acid as raw materials, and cetyltrimethylammonium bromide as dispersing agent. The addition amount of indium and tin tetrachloride is based on the mass ratio of In2O3: SnO2 = 90: 10 in the mixed solution. Indium tin oxide composite powder is prepared by chemical co-precipitation method. The chemical co-precipitation method refers to dissolving indium in nitric acid and dissolving tin tetrachloride in deionized water. After indium is completely dissolved, the two solutions are mixed to obtain a mixed solution. The mixed solution is added to the mixed solution to obtain indium tin hydroxide precipitate by co-precipitation with alkaline neutralizing agent. Impurity ions are washed, solid-liquid separation, drying, calcination of indium tin hydroxide to obtain indium tin oxide composite powder. Then, the composite sintering aid is added to the indium tin oxide composite powder and ball milled, and then the binder is added for granulation and drying. The granulated powder is first molded into a green body, and then the green body is cold isostatic pressed to obtain a blank. Finally, the blank is sintered in an oxygen atmosphere to obtain an indium tin oxide target material.

[0006] At the same time, it can be seen from the specification of the scheme that the binder can be selected from polyvinyl alcohol, polybutyl methacrylate and polyvinyl butyral. Further observation of the embodiments of the scheme shows that the above three binders are used separately, and the relative density of the target material is between 93-99.60%, the resistivity is between 1.75*10 -4 ~ 13.5*10 -4 Ω·cm, and from the comparison between embodiments 6-8 of the scheme, it can be seen that the relative density and resistivity of the target material change significantly under the same use of b group powder. It can be seen from the results presented in the embodiments of the scheme that the type of binder is not necessarily the key factor determining the relative density and resistivity of the target material, and the scheme does not use the binder for compounding.

[0007] The problem to be solved by the present scheme is: how to provide an ITO waste target recycling and target material preparation method, and the method can prepare ITO target material with high relative density under the premise of low cracking rate. SUMMARY

[0008] The purpose of the present application is to provide an ITO waste target recycling and target material preparation method, and the method can prepare ITO target material with high relative density under the premise of low cracking rate.

[0009] To achieve the above purpose, the present application discloses a method for recycling and preparing ITO waste target material, which comprises the following steps:

[0010] Step 1: acid washing, heating evaporation, cooling and powder collecting of ITO waste target to obtain powder;

[0011] Step 2: mix the powder prepared in step 1 with pure water and grind to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4-0.6:1;

[0012] Step 3: add a binder to the slurry one prepared in step 2 and stir to obtain slurry two, wherein the mass ratio of the binder to the slurry one is 2-5:100;

[0013] Step 4: spray granulate, press and sinter the slurry two prepared in step 3 to obtain the ITO waste target recycled target material.

[0014] In step 3, the binder includes polyvinyl alcohol, polyacrylamide and polyethylene glycol, and the mass ratio of polyvinyl alcohol, polyacrylamide and polyethylene glycol is 1-10:3-8:4-7.

[0015] Preferably, the molar ratio of indium to tin in the ITO waste target is 85-95:5-15.

[0016] Preferably, step 1 specifically includes the following steps:

[0017] Step A1: soak the ITO waste target in a hydrochloric acid or nitric acid solution with a concentration of 5-10% for 12-24 hours, and then rinse the ITO waste target with pure water to obtain the pickled ITO waste target;

[0018] Step A2: put the pickled ITO waste target prepared in step A1 into an electric arc furnace, heat the pickled ITO waste target by an electric arc generated by a 100V direct current, the heating temperature is 2300-2800℃, melt and gasify the pickled ITO waste target, cool and re-agglomerate the gasified ITO waste target, collect the powder using a cloth bag to obtain the powder.

[0019] Preferably, in step 2, the grinding time is 12-24 hours, and the D90 of the slurry one is less than 5um.

[0020] Preferably, in step 2, a dispersant is also added, and step 2 specifically includes: mix the powder prepared in step 1 with pure water and a dispersant and grind to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4-0.6:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water is 1-5:100.

[0021] Preferably, in step 4, the pressing specifically includes a cold pressing stage and a cold isostatic pressing stage, the pressure of the cold pressing stage is 20-50MPa, and the duration is 60-180s, the pressure of the cold isostatic pressing stage is 200-400MPa, and the duration is 60-180s.

[0022] The sintering temperature in step 4 is 1300-1600 DEG C, and the sintering time is 8-16 hours.

[0023] Preferably, the target material prepared by the method for recycling ITO waste target to prepare target material has a cracking rate less than or equal to 1.5%.

[0024] In addition, the application also discloses a target material prepared by recycling ITO waste target, which is prepared by the method for recycling ITO waste target to prepare target material.

[0025] The method for recycling ITO waste target to prepare target material disclosed by the application reduces the cracking rate of the prepared target material by controlling the parameters in the recycling process of ITO waste target and compounding the binder in the process of preparing target material, and the prepared target material also has high relative density and low resistivity, thereby improving the utilization rate of the sputtering target material, and the low resistivity of the target material also improves the conductivity and sputtering performance of the target material. DETAILED DESCRIPTION

[0026] The application will be described clearly and completely in combination with the embodiments of the application. In the description of the application, it should be noted that the specific conditions not mentioned in the embodiments are carried out according to the conventional conditions or the recommended conditions of the manufacturer. The reagents or instruments not mentioned by the manufacturer are conventional products that can be purchased in the market.

[0027] Embodiment 1

[0028] Step 1:

[0029] Step A1: the ITO waste target with a molar ratio of indium element to tin element of 90:10 is immersed in a 5% hydrochloric acid or nitric acid solution for 12 hours, and then the ITO waste target is washed with pure water after the immersion, to obtain the acid-washed ITO waste target;

[0030] Step A2: the acid-washed ITO waste target prepared in step A1 is put into an electric arc furnace, and the acid-washed ITO waste target is heated by an electric arc generated by a 100V direct current voltage, the heating temperature is 2300 DEG C, the acid-washed ITO waste target is melted and gasified, the gasified ITO waste target is cooled and re-agglomerated, the powder is collected by a cloth bag, and the powder is obtained;

[0031] Step 2: the powder prepared in step 1 is mixed with pure water and a dispersing agent, and is ground for 12 hours to obtain slurry one with D90<5um, wherein the mass ratio of the powder to the pure water is 0.4:1, and the mass ratio of the dispersing agent to the total mass of the powder and the pure water is 1:100.

[0032] Step 3: polyvinyl alcohol, polyacrylamide and polyethylene glycol were added into the slurry one prepared in step 2 and stirred, and then slurry two was obtained, wherein the mass ratio of the binder added to the slurry one was 2:100, and the mass ratio of polyvinyl alcohol, polyacrylamide and polyethylene glycol was 1:3:4;

[0033] Step 4: the slurry two prepared in step 3 was sprayed into a centrifugal spray drying tower for spray granulation to obtain powder two, and then the powder two was sequentially subjected to cold pressing and cold isostatic pressing to obtain a target blank, wherein the pressure in the cold pressing stage was 20 MPa, and the time was 60 s, and the pressure in the cold isostatic pressing stage was 200 MPa, and the time was 60 s.

[0034] After the pressing was completed, the target blank was placed into a sintering furnace, the temperature was increased to 1300℃, and the temperature was maintained for 8 h, and then the ITO target material was obtained after the temperature was decreased to room temperature.

[0035] The relative density of the ITO target material prepared was 99.64%, the resistivity was 112 μΩ·cm, and the cracking rate was 1.2%.

[0036] Example 2

[0037] Step 1:

[0038] Step A1: the ITO waste target with a molar ratio of indium element to tin element of 90:10 was immersed in a 10% hydrochloric acid or nitric acid solution for 24 h, and then the ITO waste target was washed with pure water after the immersion was completed to obtain an acid-washed ITO waste target.

[0039] Step A2: the acid-washed ITO waste target prepared in step A1 was placed into an electric arc furnace, and the acid-washed ITO waste target was heated by an electric arc generated by a 100 V direct current voltage, the heating temperature was 2800℃, the acid-washed ITO waste target was melted and gasified, the gasified ITO waste target was cooled and re-agglomerated, the powder was collected using a cloth bag, and then the powder was obtained.

[0040] Step 2: the powder prepared in step 1 was mixed and ground with pure water and a dispersant for 24 h to obtain a D90<5um slurry one, wherein the mass ratio of the powder to the pure water was 0.6:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water was 5:100.

[0041] Step 3: polyvinyl alcohol, polyacrylamide and polyethylene glycol were added into the slurry one prepared in step 2 and stirred, and then slurry two was obtained, wherein the mass ratio of the binder added to the slurry one was 2:100, and the mass ratio of polyvinyl alcohol, polyacrylamide and polyethylene glycol was 1:3:4;

[0042] Step 4: the slurry two prepared in step 3 is punched into a centrifugal spray drying tower for spray granulation to obtain powder two, and then the powder two is sequentially subjected to cold pressing and cold isostatic pressing to obtain a target blank, the pressure in the cold pressing stage is 50 MPa, and the time is 180 s, and the pressure in the cold isostatic pressing stage is 400 MPa, and the time is 180 s

[0043] After the pressing is completed, the target blank is placed into a sintering furnace, the temperature is increased to 1600 ℃, and the temperature is kept for 16 h, and then the ITO target material is obtained after the temperature is decreased to room temperature.

[0044] The relative density of the finally measured ITO target material is 99.62%, the resistivity is 110 μΩ·cm, and the cracking rate is 1.5%.

[0045] Example 3

[0046] Step 1:

[0047] Step A1: the ITO waste target with a molar ratio of indium element to tin element of 90:10 is soaked in a hydrochloric acid or nitric acid solution with a concentration of 8% for 18 h, and then the ITO waste target is washed with pure water after the soaking is completed to obtain the ITO waste target after pickling;

[0048] Step A2: the ITO waste target after pickling prepared in step A1 is put into an electric arc furnace, and the ITO waste target after pickling is heated by an electric arc generated by a 100 V direct current voltage, the heating temperature is 2500 ℃, the ITO waste target after pickling is melted and gasified, the gasified ITO waste target is cooled and re-agglomerated, the powder is collected by using a cloth bag, and the powder is obtained;

[0049] Step 2: the powder prepared in step 1 is mixed with pure water and a dispersing agent, and is ground for 18 h to obtain a slurry one with D90<5 um, wherein the mass ratio of the powder to the pure water is 0.5:1, and the mass ratio of the dispersing agent to the total mass of the powder and the pure water is 3:100;

[0050] Step 3: polyvinyl alcohol, polyacrylamide and polyethylene glycol are added to the slurry one prepared in step 2 and are stirred, and then a slurry two is obtained, wherein the mass ratio of the additive amount of the binder to the slurry one is 4:100, and the mass ratio of polyvinyl alcohol, polyacrylamide and polyethylene glycol is 5:6:5;

[0051] Step 4: the slurry two prepared in step 3 is punched into a centrifugal spray drying tower for spray granulation to obtain powder two, and then the powder two is sequentially subjected to cold pressing and cold isostatic pressing to obtain a target blank, the pressure in the cold pressing stage is 50 MPa, and the time is 180 s, and the pressure in the cold isostatic pressing stage is 400 MPa, and the time is 180 s

[0052] After the pressing is completed, the target blank is placed into a sintering furnace, the temperature is increased to 1600 ℃, and the temperature is kept for 16 h, and then the ITO target material is obtained after the temperature is decreased to room temperature.

[0053] The relative density of the prepared ITO target material is 99.86%, the resistivity is 103 μΩ·cm, and the cracking rate is 0.8%.

[0054] Example 4

[0055] Step 1:

[0056] Step A1: ITO waste targets with a molar ratio of indium element to tin element of 85:15 are immersed in a 5% hydrochloric acid or nitric acid solution for 12-24 h. After the immersion is completed, the ITO waste targets are washed with pure water to obtain the acid-washed ITO waste targets;

[0057] Step A2: The acid-washed ITO waste targets prepared in step A1 are placed in an electric arc furnace, and the acid-washed ITO waste targets are heated by an electric arc generated by a 100 V direct current voltage. The heating temperature is 2300°C. The acid-washed ITO waste targets are melted and gasified. The gasified ITO waste targets are cooled and re-agglomerated. The powder is collected using a cloth bag to obtain the powder.

[0058] Step 2: The powder prepared in step 1 is mixed with pure water and a dispersant, and is ground for 12 h to obtain slurry one. The mass ratio of the powder to the pure water is 0.4:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water is 1:100.

[0059] Step 3: Polyvinyl alcohol, polyacrylamide, and polyethylene glycol are added to the slurry one prepared in step 2 and are stirred to obtain slurry two. The mass ratio of the binder to the slurry one is 2:100, and the mass ratio of polyvinyl alcohol, polyacrylamide, and polyethylene glycol is 1:3:4.

[0060] Step 4: The slurry two prepared in step 3 is fed into a centrifugal spray drying tower for spray granulation to obtain powder two. Subsequently, the powder two is sequentially subjected to cold pressing and cold isostatic pressing to obtain a target blank. The pressure in the cold pressing stage is 20 MPa, and the time is 60 s. The pressure in the cold isostatic pressing stage is 200 MPa, and the time is 60 s.

[0061] After the pressing is completed, the target blank is placed in a sintering furnace, the temperature is raised to 1300°C, and the temperature is maintained for 8 h. After the temperature is lowered to room temperature, the ITO target material is obtained.

[0062] The relative density of the prepared ITO target material is 99.34%, the resistivity is 114 μΩ·cm, and the cracking rate is 1.2%.

[0063] Example 5

[0064] Step 1:

[0065] Step Al: immerse the IT0 waste target with the molar ratio of indium element to tin element being 95:5 in a 5% concentration hydrochloric acid or nitric acid solution for 12 hours, and then rinse the IT0 waste target with pure water to obtain the acid-washed IT0 waste target;

[0066] Step A2: put the acid-washed IT0 waste target obtained in Step Al into an electric arc furnace, heat the acid-washed IT0 waste target by an electric arc generated by a 100V direct current, the heating temperature is 2300℃, melt and gasify the acid-washed IT0 waste target, cool and re-agglomerate the gasified IT0 waste target, collect the powder with a cloth bag to obtain the powder;

[0067] Step 2: mix, grind and agitate the powder obtained in Step 1 with pure water and a dispersant for 12 hours to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water is 1:100;

[0068] Step 3: add polyvinyl alcohol, polyacrylamide and polyethylene glycol to the slurry one obtained in Step 2 and agitate to obtain slurry two, wherein the mass ratio of the binder to the slurry one is 2:100, and the mass ratio of the polyvinyl alcohol, the polyacrylamide and the polyethylene glycol is 1:3:4;

[0069] Step 4: spray granulate the slurry two obtained in Step 3 into a centrifugal spray drying tower to obtain powder two, and then cold press and cold isostatic press the powder two in sequence to obtain a target blank, the pressure in the cold pressing stage is 20MPa, and the time is 60s, the pressure in the cold isostatic pressing stage is 200MPa, and the time is 60s.

[0070] After the pressing is completed, place the target blank into a sintering furnace, raise the temperature to 1300℃, keep the temperature for 8 hours, and then lower the temperature to room temperature to obtain the ITO target material.

[0071] The relative density of the finally measured ITO target material is 99.27%, the resistivity is 118μΩ.cm, and the cracking rate is 1.2%.

[0072] Example 6

[0073] Step 1:

[0074] Step Al: immerse the IT0 waste target with the molar ratio of indium element to tin element being 95:5 in a 5% concentration hydrochloric acid or nitric acid solution for 12 hours, and then rinse the IT0 waste target with pure water to obtain the acid-washed IT0 waste target;

[0075] Step A2: The acid washed ITO waste target prepared in step Al is put into an electric arc furnace, and the acid washed ITO waste target is heated by an electric arc generated by a 100V direct current, the heating temperature is 2300°C, the acid washed ITO waste target is melted and gasified, the gasified ITO waste target is cooled and re-agglomerated, the powder is collected by a cloth bag, and the powder is obtained;

[0076] Step 2: The powder prepared in step 1 is mixed with pure water and a dispersant, and is ground for 12h to obtain a slurry one, wherein the mass ratio of the powder to the pure water is 0.4:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water is 1:100;

[0077] Step 3: Polyvinyl alcohol, polyacrylamide and polyethylene glycol are added to the slurry one prepared in step 2 and are stirred, and a slurry two is obtained after stirring, wherein the mass ratio of the binder to the slurry one is 2:100, and the mass ratio of polyvinyl alcohol, polyacrylamide and polyethylene glycol is 1:3:4;

[0078] Step 4: The slurry two prepared in step 3 is sprayed into a centrifugal spray drying tower for spray granulation to obtain a powder two, and then the powder two is sequentially subjected to cold pressing and cold isostatic pressing to obtain a target blank, the pressure in the cold pressing stage is 20MPa, and the time is 60s, and the pressure in the cold isostatic pressing stage is 200MPa, and the time is 60s.

[0079] After the pressing is completed, the target blank is put into a sintering furnace, the temperature is raised to 1300°C, and the temperature is maintained for 8h, and the ITO target material is obtained after the temperature is lowered to room temperature.

[0080] The relative density of the finally measured ITO target material is 99.25%, the resistivity is 119μΩ.cm, and the cracking rate is 1.4%.

[0081] Example 7

[0082] Step 1:

[0083] Step Al: An ITO waste target with a molar ratio of indium element to tin element of 80:20 is soaked in a 5% hydrochloric acid or nitric acid solution for 12h, and the ITO waste target is washed with pure water after the soaking is completed to obtain an acid washed ITO waste target;

[0084] Step A2: The acid washed ITO waste target prepared in step Al is put into an electric arc furnace, and the acid washed ITO waste target is heated by an electric arc generated by a 100V direct current, the heating temperature is 2300°C, the acid washed ITO waste target is melted and gasified, the gasified ITO waste target is cooled and re-agglomerated, the powder is collected by a cloth bag, and the powder is obtained;

[0085] Step 2: The powder prepared in step 1 is mixed with pure water and a dispersant, and ground for 12 hours to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4:1, and the mass ratio of the dispersant to the total mass of the powder and the pure water is 1:100;

[0086] Step 3: Polyvinyl alcohol, polyacrylamide and polyethylene glycol are added to the slurry one prepared in step 2 and stirred, and slurry two is obtained after stirring, wherein the mass ratio of the binder to the slurry one is 2:100, and the mass ratio of the polyvinyl alcohol, the polyacrylamide and the polyethylene glycol is 1:3:4;

[0087] Step 4: The slurry two prepared in step 3 is sprayed into a centrifugal spray drying tower for spray granulation to obtain powder two, and then the powder two is sequentially subjected to cold pressing and cold isostatic pressing to obtain a target embryo, wherein the pressure in the cold pressing stage is 20 MPa, and the time is 60 s, and the pressure in the cold isostatic pressing stage is 200 MPa, and the time is 60 s.

[0088] After the pressing is completed, the target embryo is placed in a sintering furnace, the temperature is raised to 1300°C, and the temperature is maintained for 8 hours, and then the temperature is lowered to room temperature to obtain an ITO target material.

[0089] The relative density of the ITO target material prepared is 97.64%, the resistivity is 126 μΩ.cm, and the cracking rate is 1.5%.

[0090] Comparative Example 1

[0091] The comparative example 1 is basically the same as example 1, except that the binder added in step 3 only contains polyvinyl alcohol, and the mass ratio of the binder to the slurry one is 2:100.

[0092] The relative density of the ITO target material prepared is 98.18%, the resistivity is 180 μΩ.cm, and the cracking rate is 1.9%.

[0093] Comparative Example 2

[0094] The comparative example 2 is basically the same as example 1, except that the binder added in step 3 contains polyvinyl alcohol and polyacrylamide, and the total amount of the polyvinyl alcohol and the polyacrylamide added is 2:100 of the mass of the slurry one, and the mass ratio of the polyvinyl alcohol to the polyacrylamide is 1:3.

[0095] The relative density of the ITO target material prepared is 97.38%, the resistivity is 165 μΩ.cm, and the cracking rate is 2.2%.

[0096] Comparative Example 3

[0097] The difference between the example 1 and the example 2 is that the binder added in step 3 includes polyvinyl alcohol, polyethylene glycol, and the total adding amount of polyvinyl alcohol and polyethylene glycol is 2:100 in mass ratio to the slurry 1, and the mass ratio of polyvinyl alcohol and polyethylene glycol is 1:3.

[0098] The relative density of the finally measured IT0 target material is 97.54%, the resistivity is 142 μΩ·cm, and the cracking rate is 2.8%.

[0099] Comparative example 4

[0100] The difference between the example 1 and the example 2 is that the binder added in step 3 includes polyvinyl alcohol, polyethylene glycol, and the total adding amount of polyvinyl alcohol and polyethylene glycol is 2:100 in mass ratio to the slurry 1, and the mass ratio of polyvinyl alcohol and polyethylene glycol is 1:3.

[0101] The relative density of the finally measured IT0 target material is 97.54%, the resistivity is 142 μΩ·cm, and the cracking rate is 2.8%.

[0102] Comparative example 5

[0103] The difference between the example 1 and the example 2 is that the binder added in step 3 includes polyvinyl alcohol, polyethylene glycol, and the total adding amount of polyvinyl alcohol and polyethylene glycol is 2:100 in mass ratio to the slurry 1, and the mass ratio of polyvinyl alcohol and polyethylene glycol is 1:3.

[0104] The relative density of the finally measured IT0 target material is 97.54%, the resistivity is 142 μΩ·cm, and the cracking rate is 2.8%.

[0105] Result analysis:

[0106] 1. It can be seen from the example 1 and the examples 3-7 that the finally prepared target material has more excellent relative density and lower resistivity when the molar ratio of indium element and tin element is 90:10 in the disclosed IT0 waste target recycling and target material preparation method.

[0107] 2. It can be seen from the example 1 and the comparative examples 1-3 that the relative density of the target material decreases and the resistivity increases to a certain extent when one or two components are missing in the binder.

[0108] 3. It can be seen from the example 1 and the comparative examples 4-5 that the relative density of the target material decreases and the resistivity increases to a certain extent when a certain component in the binder is greatly adjusted.

[0109] The above examples are the preferred embodiments of the present application, but the embodiments of the present application are not limited to the above examples, and any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present application should be equivalent replacement methods, and all are included in the protection scope of the present application.

Claims

1. A method for recycling and re-preparing a target material from an ITO waste target, characterized by, It comprises the following steps: Step 1: acid washing, heating evaporation, cooling, powder collection of ITO waste target to obtain powder; Step 2: mixing and grinding the powder obtained in step 1 with pure water to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4-0.6:1; Step 3: adding a binder to the slurry one obtained in step 2 and stirring to obtain slurry two, wherein the mass ratio of the binder to the slurry one is 2-5:100; Step 4: spray granulation, pressing and sintering of the slurry two obtained in step 3 to obtain ITO waste target recycling and re-preparation target material; In step 3, the binder comprises polyvinyl alcohol, polyacrylamide and polyethylene glycol, and the mass ratio of the polyvinyl alcohol, the polyacrylamide and the polyethylene glycol is 1-10:3-8:4-7; In the ITO waste target, the molar ratio of indium element to tin element is 85-95:5-15.

2. The method of recycling a waste ITO target into a target material according to claim 1, wherein Step 1 specifically comprises the following steps: Step A1: soaking the ITO waste target in a hydrochloric acid or nitric acid solution with a concentration of 5-10% for 12-24 hours, and then washing the ITO waste target with pure water to obtain the acid-washed ITO waste target; Step A2: putting the acid-washed ITO waste target obtained in step A1 into an electric arc furnace, heating the acid-washed ITO waste target by an electric arc generated by a 100V direct current, and setting the heating temperature to 2300-2800℃, melting and gasifying the acid-washed ITO waste target, cooling and re-agglomerating the gasified ITO waste target, collecting the powder with a cloth bag to obtain the powder.

3. The method of recycling a waste ITO target into a target material according to claim 1, wherein In step 2, the grinding time is 12-24 hours, and the D90 of the slurry one is less than 5um.

4. The method of recycling a waste ITO target into a target material according to claim 1, wherein In step 2, a dispersing agent is also added, and step 2 specifically comprises the following steps: mixing and grinding the powder obtained in step 1 with pure water and a dispersing agent to obtain slurry one, wherein the mass ratio of the powder to the pure water is 0.4-0.6:1; and the mass ratio of the dispersing agent to the total mass of the powder and the pure water is 1-5:

100.

5. The method of recycling a waste ITO target into a target material according to claim 1, wherein In step 4, the pressing specifically comprises a cold pressing stage and a cold isostatic pressing stage, the pressure of the cold pressing stage is 20-50MPa, and the duration is 60-180s, and the pressure of the cold isostatic pressing stage is 200-400MPa, and the duration is 60-180s; In step 4, the sintering temperature is 1300-1600℃, and the sintering time is 8-16 hours.

6. The method of recycling a waste ITO target into a target material according to any one of claims 1 to 5, wherein The cracking rate of the target material prepared by the method for recycling and re-preparing target material from ITO waste target is less than or equal to 1.5%.

7. A method for recycling an ITO waste target into a target material, characterized by, The relative density of the ITO waste target recycling and re-preparing target material prepared by the method for recycling and re-preparing target material from ITO waste target according to any one of claims 1-5 is greater than or equal to 99%, and the resistivity of the ITO waste target recycling and re-preparing target material is less than or equal to 120μΩ·cm.