CN113149612A - Method for recycling IZO target material - Google Patents
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- CN113149612A CN113149612A CN202110537592.0A CN202110537592A CN113149612A CN 113149612 A CN113149612 A CN 113149612A CN 202110537592 A CN202110537592 A CN 202110537592A CN 113149612 A CN113149612 A CN 113149612A
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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Abstract
The invention discloses a method for recycling an IZO target, belonging to the field of target recycling. The method for recycling the IZO target comprises the steps of firstly polishing and carrying out heat treatment on the recycled target to remove original crude indium and partial impurities of the target, then crushing the recycled target to micron-level powder, sintering the micron-level powder at high temperature to further purify the micron-level powder, then mixing new powder with the obtained powder, carrying out ball milling on the mixture to a proper size, and finally carrying out spray granulation to obtain the IZO powder which has higher purity and uniform and fine granularity and can be further used for preparing high-density targets; the method has simple operation steps, can implement industrial large-scale production, and has high recycling rate and high economic benefit of the IZO target material; the invention also discloses a method for preparing the IZO target from the IZO powder, and the IZO target prepared by pressing, molding and sintering the IZO powder has higher purity, compactness and relative density of more than 98.5 percent.
Description
Technical Field
The invention relates to the field of target recycling, in particular to a recycling method of an IZO target.
Background
In recent years, with the development of electronic information technology, the amount of target used for depositing IZO thin films is rapidly increased, but in the current industrial production process of bulk IZO targets, the utilization rate of IZO targets is less than 50%, and nearly more than 50% of the target becomes waste in the production process, so that a great resource waste problem exists. In view of this, it is necessary to develop a recycling scheme capable of effectively processing the used IZO target.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide the method for recycling the IZO target, the method comprises the steps of removing impurities from the recycled IZO target, heating and ball-milling the recycled IZO target, and finally performing spray granulation and sintering to form high-quality IZO powder and IZO target with high production efficiency; the method has the advantages of simple operation steps, low equipment requirement and low preparation cost.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for recycling IZO target comprises the following steps:
(1) polishing and heat-treating the recovered IZO target material, and crushing the IZO target material into micron-sized particles to obtain precursor powder A;
(2) putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 550-900 ℃, and preserving heat for 6-18 hours to obtain old material powder B;
(3) mixing zinc oxide and indium oxide in proportion, and placing the mixture into a ball mill for ball milling treatment to obtain new material powder C; the mass ratio of the zinc oxide to the indium oxide is 1: (5-15);
(4) uniformly mixing the old material powder B and the new material powder C in the ball mill, simultaneously adding pure water and additives, and carrying out ball milling treatment to obtain ball milling slurry D; the additive comprises a dispersant and a binder, the dispersant comprises at least one of polyvinylpyrrolidone, polycarboxylic acid compounds and polyvinyl acid salts, and the binder comprises at least one of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylate and polyethylene glycol;
(5) and (4) carrying out spray granulation on the ball-milling slurry D obtained in the step (4) to obtain IZO powder.
When the ball-milling slurry D is prepared, the used dispersing agent and the binder are mild and stable soluble additives, and the prepared powder product can be easily removed during subsequent recovery heat treatment, so that the recycling is convenient.
By adding the dispersing agent and the binder, the powder can be uniformly dispersed during ball milling, and the prepared slurry has no obvious agglomeration phenomenon.
The method for recycling the IZO target comprises the steps of firstly polishing and carrying out heat treatment on the recycled target to remove original crude indium and partial impurities of the target, then crushing the recycled target to micron-level powder, sintering the micron-level powder at high temperature to further purify the micron-level powder, then mixing new powder with the obtained powder, carrying out ball milling on the mixture to a proper size, and finally carrying out spray granulation to obtain the IZO powder which has higher purity and uniform and fine granularity and can be further used for preparing high-density targets; the method has simple operation steps, can implement industrial large-scale production, and has high recycling rate and high economic benefit of the IZO target material.
Preferably, the temperature of the heat treatment in the step (1) is 200-300 ℃, and the time is 4-12 h.
Original impurities on the surface of part of the target can be removed through specific high-temperature pretreatment conditions, and the impurity removal efficiency of subsequent sintering is improved.
Preferably, the precursor powder of step (1) has a particle size of less than 150 μm after being pulverized to micron-sized particles.
Preferably, the precursor powder A in the step (2) is placed in a sintering furnace, heated to 570-660 ℃ and kept warm.
In the preferable heat preservation range, the excessive impurities and crude metals in the recovered powder can be further effectively removed.
Preferably, the rotation speed of the ball milling treatment in the step (3) is 42-48 r/min, and the time is 6-12 h.
Preferably, the mass ratio of the old material powder B to the new material powder C added in the step (4) is 0.9-1.4: 1.
Preferably, the mass content of the solid in the ball-milling slurry D in the step (4) is 40-75%, and the particle size D of the slurry50＜0.5μm，D90＜1μm。
If the solid content is high, the whole powder is easily adhered in the ball mill or is unevenly dispersed in the ball milling process, so that a large amount of powder raw materials are wasted, and even slurry cannot be prepared; if the solid content is too low, the ball milling efficiency is seriously reduced, and the particles of the slurry cannot be reduced to the target size, so that the subsequent spray granulation and the target preparation are negatively influenced.
Preferably, the addition amount of the dispersing agent accounts for 1-15% of the mass content of the fresh material powder C, and the addition amount of the binder accounts for 1-15% of the mass content of the fresh material powder C.
Preferably, the rotation speed of the ball milling treatment in the step (4) is 42-48 r/min, and the time is 24-48 h.
The slurry with ideal granularity and dispersibility can be finally obtained through ball milling and mixing for a specific time, and subsequent efficient granulation is facilitated.
Preferably, the temperature during the spray granulation in the step (5) is 80-110 ℃.
Another object of the present invention is to provide a method for preparing an IZO target from IZO powder recycled from the IZO target, comprising the steps of:
and (3) performing dry pressure and cold isostatic pressing treatment on the IZO powder prepared by the IZO target recycling method, and sintering at normal pressure to obtain the IZO target.
The IZO target material formed by pressing and sintering the IZO powder has high purity, compactness and compactness, and the relative density is more than 98.5 percent.
Preferably, the pressure during the dry pressure treatment is 60 to 100MPa, and the pressure during the cold isostatic pressure treatment is 250 to 350 MPa.
Preferably, the sintering comprises the following specific steps: heating the material to 600-1000 ℃ at the speed of 0.1-1 ℃/min, heating to 1300-1550 ℃ at the speed of 0.1-1 ℃/min, preserving heat for 5-12 h, and cooling to room temperature at the speed of 1 ℃/min.
The invention has the beneficial effects that: the invention provides a recycling method of IZO target material, which comprises the steps of firstly polishing and carrying out heat treatment on the recycled target material to remove original crude indium and partial impurities of the target material, then crushing the crude indium and partial impurities into micron-level powder, sintering the micron-level powder at high temperature for further purification, then mixing new powder with the obtained powder, carrying out ball milling on the mixture to a proper size, and finally carrying out spray granulation to obtain the IZO powder which has higher purity and uniform and fine granularity and can be further used for preparing high-density target materials; the method has simple operation steps, can implement industrial large-scale production, and has high recycling rate and high economic benefit of the IZO target material; the invention also provides a method for preparing the IZO target from the IZO powder, and the IZO target prepared by pressing, molding and sintering the IZO powder has higher purity, compactness and relative density of more than 98.5 percent.
Drawings
Fig. 1 is a schematic flow chart of the recycling method of IZO target according to the present invention.
Detailed Description
For better illustrating the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples, which are intended to be understood in detail, but not intended to limit the present invention.
Example 1
The recycling method of IZO target of the present invention, as shown in fig. 1, includes the following steps:
(1) polishing and heat-treating the recycled IZO target material at 250 ℃ for 6h, and crushing the recycled IZO target material into micron-sized particles (the particle size of the particles is less than 150 mu m) to obtain precursor powder A;
(2) putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 650 ℃, and preserving heat for 8 hours to obtain old material powder B;
(3) 2.5kg of zinc oxide and 22.5kg of indium oxide are mixed according to a proportion and put into a ball mill to be ball-milled for 7 hours at a rotating speed of 45r/min, so as to obtain new material powder C;
(4) mixing 25kg old powder B and new powder C in ball mill, and adding 0.7kg polyvinylpyrrolidone and 2.9kg polyvinyl alcohol to obtain the final productAnd 50kg of pure water, and performing ball milling treatment for 30 hours at the rotating speed of 45r/min to obtain ball milling slurry D; particle size D of the slurry50＝0.427μm，D90＝0.815μm；
(5) And (4) carrying out spray granulation on the ball-milling slurry D obtained in the step (4) at 85-92 ℃ to obtain IZO powder.
(6) Dry pressing (80MPa) and cold isostatic pressing (270MPa) the IZO powder, heating to 750 ℃ at 0.2 ℃/min, heating to 1450 ℃ at 0.3 ℃/min, keeping the temperature for 8h, and then sintering at normal pressure by a sintering procedure of cooling to room temperature at 1 ℃/min to obtain the IZO target material with the relative density of 99.1% and the purity of 99.992%.
Example 2
The recycling method of IZO target of the present invention, as shown in fig. 1, includes the following steps:
(1) polishing and heat-treating the recycled IZO target material at 200 ℃ for 12h, and crushing the recycled IZO target material into micron-sized particles (the particle size of the particles is less than 150 mu m) to obtain precursor powder A;
(2) putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 850 ℃, and preserving heat for 6 hours to obtain old material powder B;
(3) 2.5kg of zinc oxide and 22.5kg of indium oxide are mixed according to a proportion and put into a ball mill to be ball-milled for 6 hours at a rotating speed of 45r/min, so as to obtain new material powder C;
(4) uniformly mixing 25kg of old material powder B and new material powder C in a ball mill, simultaneously adding 0.7kg of polyvinylpyrrolidone, 2.9kg of polyvinyl alcohol and 50kg of pure water, and carrying out ball milling treatment for 45 hours at the rotating speed of 45r/min to obtain ball milling slurry D; particle size D of the slurry50＝0.355μm，D90＝0.716μm；
(5) And (4) carrying out spray granulation on the ball-milling slurry D obtained in the step (4) at 85-92 ℃ to obtain IZO powder.
(6) Dry pressing (60MPa) and cold isostatic pressing (320MPa) the IZO powder, heating to 750 ℃ at 0.2 ℃/min, heating to 1450 ℃ at 0.3 ℃/min, keeping the temperature for 8h, and then sintering at normal pressure by a sintering procedure of cooling to room temperature at 1 ℃/min to obtain the IZO target material with the relative density of 98.9% and the purity of 99.977%.
Example 3
The recycling method of IZO target of the present invention, as shown in fig. 1, includes the following steps:
(1) polishing and heat-treating the recycled IZO target material at 300 ℃ for 4h, and crushing the recycled IZO target material into micron-sized particles (the particle size of the particles is less than 150 mu m) to obtain precursor powder A;
(2) putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 550 ℃, and preserving heat for 10 hours to obtain old material powder B;
(3) 2.5kg of zinc oxide and 22.5kg of indium oxide are mixed according to a proportion and put into a ball mill to be ball-milled for 10 hours at a rotating speed of 45r/min, so as to obtain new material powder C;
(4) uniformly mixing 25kg of old material powder B and new material powder C in a ball mill, simultaneously adding 0.7kg of polyvinylpyrrolidone, 2.9kg of polyvinyl alcohol and 50kg of pure water, and carrying out ball milling treatment for 25 hours at the rotating speed of 45r/min to obtain ball milling slurry D; particle size D of the slurry50＝0.472μm，D90＝0.894μm；
(5) And (4) carrying out spray granulation on the ball-milling slurry D obtained in the step (4) at 85-92 ℃ to obtain IZO powder.
(6) Dry pressing (100MPa) and cold isostatic pressing (250MPa) the IZO powder, heating to 800 ℃ at 0.5 ℃/min, heating to 1500 ℃ at 0.2 ℃/min, keeping the temperature for 10h, and then carrying out normal pressure sintering by a sintering program of cooling to room temperature at 1 ℃/min to obtain the IZO target material with the relative density of 99.0% and the purity of 99.951%.
Comparative example 1
The comparative example only differs from example 1 in that the specific step of step (2) is: putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 450 ℃, and preserving heat for 6 hours to obtain old material powder B;
the comparative example obtained an IZO target having a relative density of 97.1% and a purity of 98.893%.
Comparative example 2
The comparative example only differs from example 1 in that the specific step of step (2) is: putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 550 ℃, and preserving heat for 5 hours to obtain old material powder B;
the comparative example obtained an IZO target having a relative density of 97.3% and a purity of 99.925%.
Comparative example 3
The comparative example differs from example 1 only in that no dispersant is added during the ball milling treatment; the comparative example obtained an IZO target having a relative density of 98% and a purity of 99.974%.
Comparative example 4
The comparative example differs from example 1 only in that no binder is added during the ball milling process; the comparative example obtained an IZO target having a relative density of 98.2% and a purity of 99.968%.
Comparative example 5
The comparative example is different from example 1 only in that the ball-milling slurry D is defoamed, then directly injected into a mold for hydraulic molding for 5h, and then placed into a sintering furnace for normal pressure sintering according to the same sintering procedure as in example 1 to obtain an IZO target with a relative density of 95.5% and a purity of 99.989%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for recycling IZO target is characterized by comprising the following steps:
(1) polishing and heat-treating the recovered IZO target material, and crushing the IZO target material into micron-sized particles to obtain precursor powder A;
(2) putting the precursor powder A obtained in the step (1) into a sintering furnace, heating to 550-900 ℃, and preserving heat for 6-18 hours to obtain old material powder B;
(3) mixing zinc oxide and indium oxide in proportion, and placing the mixture into a ball mill for ball milling treatment to obtain new material powder C; the mass ratio of the zinc oxide to the indium oxide is 1: (5-15);
(4) uniformly mixing the old material powder B and the new material powder C in the ball mill, simultaneously adding pure water and additives, and carrying out ball milling treatment to obtain ball milling slurry D; the additive comprises a dispersant and a binder, the dispersant comprises at least one of polyvinylpyrrolidone, polycarboxylic acid compounds and polyvinyl acid salts, and the binder comprises at least one of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylate and polyethylene glycol;
(5) and (4) carrying out spray granulation on the ball-milling slurry D obtained in the step (4) to obtain IZO powder.
2. The method for recycling IZO target according to claim 1, wherein the heat treatment in the step (1) is performed at a temperature of 200 to 300 ℃ for 4 to 12 hours.
3. The method for recycling the IZO target material as claimed in claim 1, wherein the rotation speed of the ball milling in the step (3) is 42 to 48r/min for 6 to 12 hours.
4. The method for recycling an IZO target according to claim 1, wherein the mass ratio of the old powder B to the new powder C added in the step (4) is 0.9 to 1.4: 1.
5. the method for recycling an IZO target material as claimed in claim 1, wherein the ball-milling slurry D in the step (4) contains 40 to 75% by mass of solids, and has a particle size D of 40 to 75%50＜0.5μm，D90＜1μm。
6. The method for recycling an IZO target material as claimed in claim 5, wherein the dispersant is added in an amount of 1 to 15% by mass based on the mass content of the virgin powder C, and the binder is added in an amount of 1 to 15% by mass based on the mass content of the virgin powder C.
7. The method for recycling the IZO target material as claimed in claim 1, wherein the rotation speed of the ball milling in the step (4) is 42 to 48r/min for 24 to 48 hours.
8. The method for recycling an IZO target material as claimed in claim 1, wherein the temperature in the spray granulation in the step (5) is 80 to 110 ℃.
9. A preparation method of an IZO target is characterized by comprising the following steps: the IZO target material is obtained by subjecting the IZO powder prepared by the method for recovering an IZO target material as defined in any one of claims 1 to 8 to dry pressure and cold isostatic pressing, and then sintering the powder under normal pressure.
10. The method for preparing IZO target according to claim 9, wherein the sintering specifically comprises: heating the material to 600-1000 ℃ at the speed of 0.1-1 ℃/min, heating to 1300-1550 ℃ at the speed of 0.1-1 ℃/min, preserving heat for 5-12 h, and cooling to room temperature at the speed of 1 ℃/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116444269A (en) * | 2023-03-30 | 2023-07-18 | 先导薄膜材料(安徽)有限公司 | Preparation method of doped molybdenum target |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540895A (en) * | 2012-07-10 | 2014-01-29 | 光洋应用材料科技股份有限公司 | Sputtering target and metal oxide thin film |
| CN104710163A (en) * | 2005-07-01 | 2015-06-17 | 出光兴产株式会社 | method for producing IZO sputtering target |
| KR20150120073A (en) * | 2014-04-17 | 2015-10-27 | 삼성코닝어드밴스드글라스 유한회사 | Method of fabricating indium zinc oxide sputtering target |
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| CN104710163A (en) * | 2005-07-01 | 2015-06-17 | 出光兴产株式会社 | method for producing IZO sputtering target |
| CN103540895A (en) * | 2012-07-10 | 2014-01-29 | 光洋应用材料科技股份有限公司 | Sputtering target and metal oxide thin film |
| KR20150120073A (en) * | 2014-04-17 | 2015-10-27 | 삼성코닝어드밴스드글라스 유한회사 | Method of fabricating indium zinc oxide sputtering target |
| CN109320231A (en) * | 2018-09-13 | 2019-02-12 | 江苏比昂电子材料有限公司 | The recovery and treatment method of ITO target |
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| CN116444269A (en) * | 2023-03-30 | 2023-07-18 | 先导薄膜材料(安徽)有限公司 | Preparation method of doped molybdenum target |
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