CN115159960A - Preparation method of high-resistivity ITO target material - Google Patents
Preparation method of high-resistivity ITO target material Download PDFInfo
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- CN115159960A CN115159960A CN202210594915.4A CN202210594915A CN115159960A CN 115159960 A CN115159960 A CN 115159960A CN 202210594915 A CN202210594915 A CN 202210594915A CN 115159960 A CN115159960 A CN 115159960A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013077 target material Substances 0.000 title claims description 19
- 239000000843 powder Substances 0.000 claims abstract description 74
- 239000002699 waste material Substances 0.000 claims abstract description 42
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000007873 sieving Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 12
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 4
- 210000001161 mammalian embryo Anatomy 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 238000011084 recovery Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 239000010453 quartz Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002309 gasification Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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Abstract
The invention belongs to the technical field of target recycling and discloses a preparation method of an ITO target with high resistivity. The preparation method comprises the steps of sequentially crushing, crushing and sieving the waste ITO target blank, carrying out heat treatment on the obtained waste ITO target blank powder at 400-600 ℃ to remove additives contained in the waste ITO target blank powder, carrying out mixed ball milling on the waste ITO target blank powder and indium oxide powder to obtain primary ball milled powder, adding pure water, uniformly mixing, granulating, sieving, carrying out primary calcination at 1450 ℃, carrying out secondary ball milling on the calcined powder, adding pure water, uniformly mixing, granulating and sieving; and tabletting and molding the obtained powder, and sintering at the temperature of 1300-1550 ℃ to obtain the ITO target. The method directly converts the waste ITO target blank into the ITO material which can be directly used for production, has the advantages of simple process, short consumed time and environmental protection, and meanwhile, the metal recovery rate in the waste target blank is obviously improved, the waste of resources is reduced and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of target recycling, and particularly relates to a preparation method of a high-resistivity ITO target.
Background
In the background of the current industrial production, the improvement of the production benefit should not be limited to the updating of the production equipment, but should be optimized to the existing production link. A large amount of loss is generated in the production process of the ITO target material, and particularly in the target blank forming process, the generation of a large amount of waste target blanks not only reduces the utilization rate of powder, but also increases the production cost of the target material. The existing recovery technology is usually to purify the oxide in the waste target blank for secondary production. The production technology not only increases the production cost of enterprises, but also causes the waste of resources.
Patent CN 113149611A discloses ITO powder and target material prepared by recycling ITO waste target blanks and a preparation method thereof, wherein the ITO waste target blanks after CIP or CP are subjected to coarse crushing treatment, then are subjected to fine crushing and sieving, are placed into a muffle furnace and are heated to 200-600 ℃ for heat treatment, and the obtained powder is added with pure water, an antifoaming agent, a binder and a dispersing agent to be uniformly mixed and then is subjected to ball milling treatment to obtain slurry, and then is subjected to spray drying treatment, mixing and sieving to obtain ITO powder. Carrying out hydraulic forming on the obtained ITO powder, and carrying out cold isostatic pressing treatment to obtain an ITO target blank; and heating the obtained ITO target blank to 400-600 ℃ at a first heating rate, preserving heat for 4.5-5.5 h, then heating to 1400-1600 ℃ at a second heating rate, and preserving heat for 7.5-8.5 h to obtain the ITO target. However, this patent technology can only obtain a target material from which ITO powder components (indium oxide/tin oxide = 90/10) are recovered, and cannot obtain a target material having other component ratios.
Patent CN 107129277A discloses a method for preparing ITO target material from ITO waste target recovery powder, which comprises using vaporized recovery ITO powder as raw material, adding tin oxide and/or indium oxide powder with mass not less than 0.5% of the raw material as sintering activity enhancer, and distributing in ITO powder; adding water and a dispersing agent into the mixed powder, ball-milling, spray-drying, putting into a die, gradually pressurizing in stages, keeping for a certain time after each pressure rise, pressing into a primary blank, gradually pressurizing in stages, keeping for a certain time after each pressure rise, carrying out cold isostatic pressing to obtain a blank, carrying out heat preservation and degreasing on the prepared blank, and then sintering in an oxygen atmosphere to obtain the ITO target. Patent CN 112960690A discloses a method for recycling waste ITO targets efficiently, which comprises the following steps: s1, cleaning: wiping the surface of the ITO waste target with acetone, cleaning the ITO waste target with ultrasonic waves, and drying the ITO waste target for later use; s2, arc gasification: putting the cleaned ITO waste target into a direct current arc gasification reaction chamber, and introducing an electric arc generated by 100-200V direct current voltage to melt and gasify the ITO waste target; s3, powder recovery: and (3) quenching the gasified ITO waste target, and then passing through a grading powder collecting system to obtain ITO powder.
The method for recovering the ITO powder through gasification has the defect of high energy consumption.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of an ITO target material with high resistivity. The method directly converts the waste ITO target blank into ITO powder which can be directly used for production, has the advantages of simple process, short consumed time and environmental protection, obviously improves the metal recovery rate in the waste target blank, reduces the waste of resources and reduces the production cost.
The invention also aims to provide the high-resistivity ITO target prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-resistivity ITO target material comprises the following preparation steps:
(1) Crushing the waste ITO target blank by using a crusher, and then crushing and sieving by using a ceramic crusher to obtain waste target blank powder;
(2) Carrying out heat treatment on the waste target embryo powder obtained in the step (1) at 400-600 ℃ to remove additives contained in the waste target embryo powder;
(3) Mixing and ball-milling the waste target blank powder subjected to heat treatment in the step (2) and indium oxide powder to obtain primary ball milled powder, adding pure water, uniformly mixing, granulating and sieving;
(4) Calcining the granulated powder in the step (3) at 1400-1500 ℃ for one time;
(5) Performing secondary ball milling on the calcined powder in the step (4), adding pure water, uniformly mixing, granulating and sieving;
(6) And (4) tabletting and forming the powder treated in the step (5), and sintering at the temperature of 1300-1550 ℃ to obtain the high-resistivity ITO target.
Further, the particle size of the crushed particles in the step (1) is 1-5 cm, and the crushing and sieving refers to sieving through a 80-mesh sieve.
Further, the heat treatment in the step (2) is carried out in a muffle furnace, the heat treatment time is controlled to be 20-40 h, and the content of C after the heat treatment is controlled to be 50-100 ppm.
Further, indium oxide in the waste target blank powder after the heat treatment in the step (3) accounts for 90wt%, and the mass ratio of the waste target blank powder to the indium oxide powder is 1:1.
Further, the rotation speed of the mixing ball mill in the step (3) is 40-70 rpm, and the ball milling time is 6-10 h.
Further, the adding amount of the pure water in the step (3) is 8-10% of the mass of the primary ball milling powder.
Further, the granulation in the step (3) refers to granulation under the pressure of 17-30 MPa, and the sieving refers to sieving by a 0.5mm sieve.
Further, the rotation speed of the secondary ball milling in the step (5) is 40-70 rpm, and the ball milling time is 4-8 h.
Further, the adding amount of the pure water in the step (5) is 5% of the mass of the secondary ball milling powder.
Further, the granulation in the step (5) means granulation under a pressure of 4-10 MPa, and the sieving means sieving by a 0.5mm sieve.
Further, the size of the pellet molding in the step (6) is 25 × 10mm.
The high-resistivity ITO target material is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method can recycle the ITO waste target blank and directly prepare new qualified ITO powder; compared with the mainstream ITO recovery method, the method has the advantages of high production efficiency, low equipment investment, low cost and the like. In addition, by adopting the method, the resource waste can be reduced, the recovery and preparation cost of production enterprises and using enterprises can be reduced, the resistivity of the prepared ITO target meets the requirement, and target cracking is basically avoided when ITO is evaporated.
(2) The invention introduces new indium oxide powder, generates the required phase by primary ball milling and granulation and primary calcination, and then carries out secondary ball milling to facilitate subsequent molding and sintering, thereby obtaining the ITO target with uniform component structure and high resistivity.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Crushing 10kg of formed waste ITO target blank by using a crusher, wherein the particle size of the crushed particles is about 1-5 cm; finely crushing the obtained ITO particles by using a ceramic crusher, screening the ITO particles by using a 80-mesh screen after the fine crushing is finished, and taking undersize products to perform the next step;
(2) And (2) loading the powder obtained in the step (1) into a quartz boat, and then placing the quartz boat into a muffle furnace for heat treatment (removing additives). The heat treatment temperature is 500 ℃, the heat treatment time is 20 hours, and the C content after the heat treatment is 65ppm.
(3) Adding 250g of the heat treatment powder obtained in the step (2) and 250g of indium oxide powder into a ball milling tank for ball milling, wherein the rotating speed of a ball mill is 55rpm, and the ball milling time is 6 hours, so as to obtain ITO (indium tin oxide) primary ball milled powder; adding 40g of pure water into the obtained primary ball milled powder, grinding, and standing for 24 hours; the powder obtained was charged into a die, granulated once under a force of 17MPa for a period of 60s, and then passed through a 0.5mm sieve.
(4) And (4) loading the powder obtained in the step (3) into an alumina quartz boat, and placing the alumina quartz boat into a sintering furnace for primary calcination at 1450 ℃.
(5) Adding the powder obtained in the step (4) into a ball milling tank, and carrying out secondary ball milling, wherein the rotating speed of a ball mill is 55rpm, and the ball milling time is 4 hours; adding 25g of pure water into the powder subjected to secondary ball milling, grinding, and standing for 18h; the powder obtained was granulated at a pressure of 5MPa for a period of 60S, passing through a 0.5mm sieve.
(6) Tabletting and molding the secondary granulated powder obtained in the step (5), wherein the final dimension of the tabletting is phi 25 x 10mm; and sintering the pressed target blank at 1300 ℃ to obtain the ITO target material with high resistivity.
The ITO target obtained in this example was tested to obtain the following data: density 4.148g/cm 3 (ii) a Resistivity 2491 μ Ω · cm; the total impurity result is less than 100ppm, and each impurity result is less than 20ppm; the compositional deviation was less than 0.2%.
Example 2
(1) Crushing 10kg of formed waste ITO target blank by using a crusher, wherein the particle size of the crushed particles is about 1-5 cm; finely crushing the obtained ITO particles by using a ceramic crusher, screening the ITO particles by using a 80-mesh screen after the fine crushing is finished, and taking undersize products to perform the next step;
(2) And (2) loading the powder obtained in the step (1) into a quartz boat, and then placing the quartz boat into a muffle furnace for heat treatment (removing additives). The heat treatment temperature is 500 ℃, the heat treatment time is 20 hours, and the C content after the heat treatment is 58ppm.
(3) Adding 250g of the heat treatment powder obtained in the step (2) and 250g of indium oxide powder into a ball milling tank for ball milling, wherein the rotating speed of a ball mill is 50rpm, and the ball milling time is 8 hours, so as to obtain ITO (indium tin oxide) primary ball milled powder; adding 40g of pure water into the obtained primary ball milled powder, grinding, and standing for 24 hours; the powder obtained was charged into a die, granulated once under a force of 17MPa for a period of 60s, and then passed through a 0.5mm sieve.
(4) And (4) loading the powder obtained in the step (3) into an alumina quartz boat, and placing the alumina quartz boat into a sintering furnace for primary calcination, wherein the calcination temperature is 1450 ℃.
(5) Adding the powder obtained in the step (4) into a ball milling tank, and carrying out secondary ball milling, wherein the rotating speed of a ball mill is 50rpm, and the ball milling time is 6 hours; adding 25g of pure water into the powder subjected to secondary ball milling, grinding, and standing for 18h; the powder obtained was granulated at a pressure of 5MPa for a period of 60S, passing through a 0.5mm sieve.
(6) Tabletting and molding the secondary granulated powder obtained in the step (5), wherein the final tabletting size is phi 25 x 10mm; and sintering the pressed target blank at 1500 ℃ to obtain the high-resistivity ITO target.
The ITO target obtained in this example was tested to obtain the following data: density 4.020g/cm 3 (ii) a The resistivity was 1309 μ Ω · cm; the total impurity result is less than 100ppm, and each impurity result is less than 20ppm; deviation of compositionLess than 0.2%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a high-resistivity ITO target is characterized by comprising the following preparation steps:
(1) Crushing the waste ITO target blank by using a crusher, and then crushing and sieving the crushed waste ITO target blank by using a ceramic crusher to obtain waste target blank powder;
(2) Carrying out heat treatment on the waste target embryo powder obtained in the step (1) at 400-600 ℃ to remove additives contained in the waste target embryo powder;
(3) Mixing and ball-milling the waste target blank powder subjected to heat treatment in the step (2) and indium oxide powder to obtain primary ball milled powder, adding pure water, uniformly mixing, granulating and sieving;
(4) Calcining the granulated powder in the step (3) at 1400-1500 ℃ for one time;
(5) Performing secondary ball milling on the calcined powder in the step (4), adding pure water, uniformly mixing, granulating and sieving;
(6) And (4) tabletting and molding the powder treated in the step (5), and sintering at 1300-1550 ℃ to obtain the high-resistivity ITO target.
2. The method for preparing the ITO target material with high resistivity according to claim 1, wherein the particle size of the crushed particles in the step (1) is 1-5 cm, and the crushing and sieving are performed by using an 80-mesh sieve.
3. The method for preparing the ITO target material with high resistivity according to claim 1, wherein the heat treatment in the step (2) is performed in a muffle furnace, the heat treatment time is controlled to be 20-40 h, and the C content after the heat treatment is controlled to be 50-100 ppm.
4. The method for preparing the ITO target material with high resistivity according to claim 1, wherein the indium oxide in the waste target blank powder after the heat treatment in the step (3) accounts for 90wt%, and the mass ratio of the waste target blank powder to the indium oxide powder is 1:1.
5. The method for preparing the ITO target material with high resistivity according to claim 4, wherein the rotation speed of the mixing ball mill in the step (3) is 40-70 rpm, and the ball milling time is 6-10 h.
6. The method for preparing an ITO target material with high resistivity according to claim 5, wherein the amount of pure water added in the step (3) is 8-10% of the mass of the primary ball mill powder; the granulation refers to granulation under the pressure of 17-30 Mpa, and the sieving refers to sieving by a 0.5mm sieve.
7. The method for preparing the ITO target material with high resistivity according to claim 1, wherein the rotation speed of the secondary ball milling in the step (5) is 40-70 rpm, and the ball milling time is 4-8 h.
8. The method for preparing the ITO target material with high resistivity according to claim 7, wherein the amount of pure water added in the step (5) is 5% of the mass of the secondary ball mill powder; the granulation is carried out under the pressure of 4-10 Mpa, and the sieving is carried out by a sieve of 0.5 mm.
9. The method according to claim 1, wherein the preform molding in step (6) has a dimension of 25 x 10mm.
10. A high resistivity ITO target, characterized by being prepared by the method of any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116332637A (en) * | 2023-02-14 | 2023-06-27 | 芜湖映日科技股份有限公司 | Method for preparing ITO rotary target in solar cell industry |
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