CN111620367B - Method for recovering ITO powder from ITO residual target/waste target - Google Patents
Method for recovering ITO powder from ITO residual target/waste target Download PDFInfo
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Abstract
The invention provides a method for recovering ITO powder from an ITO residual target/waste target, and relates to the technical field of photoelectric material recycling. The method comprises the steps of cleaning and acid washing the surface of the ITO residual target/waste target, carrying out thermal stress crushing treatment, carrying out ring roller grinding crushing treatment, carrying out airflow crushing treatment and carrying out vibration ball milling treatment, and processing the ITO residual target/waste target into ITO nano powder with the particle size of 100-500 nm. The method provided by the invention processes the ITO residual target/waste target into ITO powder which can be directly used for preparing the ITO target material, and has the advantages of simple process, energy saving, environmental protection, low production cost and suitability for large-scale production; meanwhile, the purity of the recovered ITO powder is high and can reach 99.99%, the recovery rate of the waste target is greatly improved, and the recovery rate of the waste target is more than 98%.
Description
Technical Field
The invention relates to the technical field of photoelectric material recycling, in particular to a method for recycling ITO powder from an ITO residual target/waste target.
Background
Indium Tin Oxide (ITO) films prepared from indium tin oxide as a raw material have the advantages of transparency to visible light, conductivity, high hardness, corrosion resistance and wear resistance, and are widely applied to industry in recent years. However, the utilization rate of the sputtering target is usually low, the utilization rate of the planar target is only about 30%, the utilization rate of the rotary target is high, but the utilization rate is only about 70%, because the raw material of the ITO target is mainly indium oxide, indium is a rare metal, the price is high, and the indium resource is a scarce resource, the recycling of the ITO target is particularly important.
At present, the recovery of the ITO waste target is roughly divided into two categories, one is wet recovery, the rough process flow of the method is to dissolve the ITO waste target by strong acid, and then high-purity indium, tin simple substance or indium-tin alloy is extracted through steps of electrolysis, hydrolysis precipitation, alkaline separation, replacement and the like, the method has the advantages of complex process, longer period, higher cost and serious energy resource consumption, and ITO powder cannot be directly obtained; the other method is to directly prepare the ITO waste target into ITO powder, and the method is a relatively energy-saving recovery method because the process of preparing indium powder into ITO powder is omitted. For example, in chinese patent CN104843771A, an ITO waste target is directly placed in a plasma reaction chamber, and the waste target is directly heated into ITO gas by high-temperature plasma, and then cooled into ITO powder; chinese patent CN105366709A, the ITO waste target is heated by electric arc generated by electrode discharge to form ITO gas, and then the gas is rapidly condensed into ITO powder; the two preparation methods are characterized in that waste targets are atomized and then solidified into ITO powder, the ITO powder can be directly used for preparing ITO targets, but the ITO waste targets belong to ceramic materials, and huge energy is needed for gasifying the waste targets, so that the two methods still have serious energy consumption, high production cost and expensive equipment.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for collecting ITO powder from an ITO residual target/waste target. The method provided by the invention processes the ITO residual target/waste target into ITO powder which can be directly used for preparing the ITO target material, and has the advantages of simple process, energy conservation, environmental protection, low production cost and suitability for large-scale production.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recovering ITO powder from an ITO residual target/waste target, which comprises the following steps:
(1) acid washing the ITO residual target/waste target with the cleaned surface by adopting strong acid to obtain an indium-removing target material;
(2) heating and insulating the indium-removing target material under the condition of introducing oxygen, and then soaking the insulated target material into water for quenching to carry out thermal stress crushing to obtain ITO particles with the particle size of 5-10 mm;
(3) performing ring rolling crushing treatment on the ITO particles with the particle size of 5-10 mm to obtain ITO powder with the particle size of 0.5-1 mm;
(4) carrying out airflow crushing treatment on the ITO powder with the particle size of 0.5-1 mm, and screening to obtain ITO powder with the particle size of less than or equal to 5 micrometers;
(5) and carrying out vibration ball milling treatment on the ITO powder with the particle size of less than or equal to 5 microns to obtain the ITO powder with the particle size of 100-500 nm.
Preferably, the flow rate of the oxygen introduced in the step (2) is 100-120L/min; the heating and heat preservation temperature is 1200-1400 ℃, and the heat preservation time is 2-5 h.
Preferably, after the step (2) of performing thermal stress cracking, the method further comprises taking out the ITO particles obtained by cracking from water and drying.
Preferably, the ring roll mill crushing treatment in the step (3) is performed in a vertical ring roll mill; the rotating speed of the main shaft of the vertical ring roller mill is 180-200 r/min.
Preferably, after the ring-roll milling crushing treatment in step (3), the method further comprises acid-washing the ITO powder obtained after crushing with strong acid.
Preferably, after the step (1) or the step (3) is acid-washed, the method independently further comprises sequentially performing ultrasonic washing and drying on the acid-washed ITO product; the ultrasonic cleaning adopts water as a cleaning agent.
Preferably, the airflow crushing treatment in the step (4) is performed in an impact airflow crusher; the impact plate of the impact type jet mill is an ITO plate.
Preferably, the vibratory ball milling treatment in the step (5) is carried out in a vibratory ball mill; the vibration frequency of the vibration ball mill is 800-1200 times/min, and the ball milling time is 18-24 hours.
Preferably, ITO grinding balls are adopted in the vibration ball milling treatment, and the ball-to-material ratio is 3-5: 1.
Preferably, the ITO grinding ball comprises a large ball, a middle ball and a small ball; the diameter of the big ball is 8-10 mm, the diameter of the middle ball is 5-8 mm, and the diameter of the small ball is 3-5 mm; the mass ratio of the big balls to the medium balls to the small balls is 1:1: 2.
The invention provides a method for recovering ITO powder from an ITO residual target/waste target, which comprises the steps of cleaning and acid washing the surface of the ITO residual target/waste target, carrying out thermal stress crushing treatment, carrying out ring-rolling crushing treatment, carrying out airflow crushing treatment and carrying out vibration ball milling treatment, and processing the ITO residual target/waste target into ITO nano powder with the particle size of 100-500 nm. The method processes the ITO residual target/waste target into ITO nano powder which can be directly used for preparing the ITO target material, does not need to carry out a large number of links of metal separation and purification, and has simple process, economy and environmental protection; according to the invention, in the process of preparing ITO powder, the ITO target does not need to be atomized, so that the energy consumption and the equipment cost are reduced, and the energy-saving and environment-friendly effects are achieved. Therefore, the method provided by the invention processes the ITO residual target/waste target into ITO powder which can be directly used for preparing the ITO target material, has the advantages of simple process, energy conservation, environmental protection and low production cost, and is suitable for large-scale production.
In addition, the invention adopts aerobic heating and heat preservation in the stage of thermal stress crushing treatment, avoids the thermal decomposition of the ITO target in the heating process, and improves the purity of the ITO powder, and further, the ITO powder is pickled after the ring roller grinding treatment, the ITO plate is used as an impact plate in the process of airflow crushing treatment, and the ITO grinding balls are used in the process of vibration ball grinding treatment, thereby avoiding the pollution of the device to the powder in the refining process, and further improving the purity of the ITO powder. Therefore, the ITO powder recovered by the method provided by the invention has high purity which can reach 99.99%, and meanwhile, the recovery rate of the waste target is greatly improved and is more than 98%.
Drawings
FIG. 1 is a schematic diagram showing a residue target of ITO in example 1;
FIG. 2 is a physical diagram of an ITO particle after thermal stress crushing in example 1;
FIG. 3 is a diagram showing a natural stacking state of ITO powder after the ring-roller mill crushing treatment in example 1;
FIG. 4 is a scanning electron micrograph of ITO powder after jet milling in example 1;
FIG. 5 is a graph showing a distribution of particle sizes of ITO powder obtained after ball milling in example 1.
Detailed Description
The invention provides a method for recovering ITO powder from an ITO residual target/waste target, which comprises the following steps:
(1) pickling the ITO residual target/waste target with a clean surface by using strong acid to obtain an indium-removing target material;
(2) heating and insulating the indium-removing target material under the condition of introducing oxygen, and then soaking the insulated target material into water for quenching to carry out thermal stress crushing to obtain ITO particles with the particle size of 5-10 mm;
(3) performing ring rolling crushing treatment on the ITO particles with the particle size of 5-10 mm to obtain ITO powder with the particle size of 0.5-1 mm;
(4) carrying out airflow crushing treatment on the ITO powder with the particle size of 0.5-1 mm, and screening to obtain ITO powder with the particle size of less than or equal to 5 micrometers;
(5) and carrying out vibration ball milling treatment on the ITO powder with the particle size of less than or equal to 5 microns to obtain the ITO powder with the particle size of 100-500 nm.
According to the invention, the ITO residual target/waste target with a clean surface is subjected to acid washing by adopting strong acid, so that the target material after indium removal is obtained. The present invention has no particular requirement on the source of the ITO residual target/waste target, and the ITO residual target/waste target from which the present invention is known to those skilled in the art can be applied to the method of the present invention. In the present invention, the surface cleaning is specifically: and wiping off dust on the surface of the ITO residual target/waste target by using a cleaning cloth.
In the invention, the strong acid is preferably sulfuric acid with the mass concentration of 10-15%, and more preferably sulfuric acid with the mass concentration of 12-13%; according to the invention, indium simple substance generated in the sputtering process of the ITO residual target/waste target or indium simple substance residue used in the binding process is removed through acid washing, and the acid washing time is preferably 10-20 min. After acid washing, the invention also preferably carries out ultrasonic cleaning and drying on the ITO product after acid washing in sequence. In the invention, the cleaning agent adopted for ultrasonic cleaning is preferably water, and the water is preferably deionized water; the ultrasonic cleaning time is preferably 20-30 min; the invention removes the residual acid on the surface of the ITO product after the acid cleaning through ultrasonic cleaning. In the present invention, the temperature and time for the drying are not particularly required, and the moisture can be sufficiently removed.
After the indium-removing target material is obtained, the indium-removing target material is heated and insulated under the condition of introducing oxygen, then the insulated target material is immersed in water for quenching and thermal stress crushing, and ITO particles with the particle size of 5-10 mm are obtained. In the invention, the flow rate of the introduced oxygen is preferably 100-120L/min, and more preferably 110L/min. In the invention, the heat preservation temperature of the heating heat preservation is preferably 1200-1400 ℃, more preferably 1300 ℃, and the heat preservation time is preferably 2-5 h, more preferably 3-4 h. In the present invention, the heat retention is preferably performed in an atmospheric aerobic furnace. The invention adopts aerobic heating and heat preservation in the stage of thermal stress crushing treatment, avoids thermal decomposition of the ITO target material (the ITO target material is easy to lose oxygen and reduce into a metal simple substance at high temperature), and improves the purity of the ITO powder.
In the present invention, the water is preferably normal temperature deionized water; and (3) immersing the heat-insulated target material into water, and crushing the target material into ITO particles with the particle size of 5-10 mm due to thermal stress under the condition of high-temperature shock cooling. After the thermal stress crushing is carried out, the invention also preferably takes out the ITO particles obtained by crushing from water and then carries out drying; the present invention does not require any particular temperature or time for drying, and it is sufficient to remove moisture from the ITO particles.
After ITO particles with the particle size of 5-10 mm are obtained, the ITO particles with the particle size of 5-10 mm are subjected to ring roller grinding and crushing treatment to obtain ITO powder with the particle size of 0.5-1 mm. In the present invention, the ring roll mill crushing treatment is preferably performed in a vertical ring roll mill; the rotating speed of the main shaft of the vertical ring roller mill is 180-200 r/min, and more preferably 190 r/min. The invention has no special requirements on the vertical ring roller mill, and a vertical ring roller mill which is well known to a person skilled in the art can be adopted. ITO particles with the particle size of 5-10 mm are crushed into powder in the ring roller grinding and crushing treatment process, and the particle size is 0.5-1 mm.
After the ring-roll mill crushing treatment, the ITO powder obtained after crushing is preferably subjected to acid washing with a strong acid in the present invention. In the invention, the strong acid is preferably sulfuric acid with the mass concentration of 5-10%, and more preferably sulfuric acid with the mass concentration of 6-8%; the pickling time is preferably 10-20 min. According to the invention, the ITO powder obtained after crushing is subjected to acid washing, so that metal simple substances (mainly iron simple substances) generated by abrasion of the ring roller mill can be removed, and the purity of the prepared ITO powder is further improved. After the acid washing, the invention also preferably carries out ultrasonic cleaning and drying on the ITO product after the acid washing in sequence; the ultrasonic cleaning and drying conditions are the same as those in the above scheme, and are not described again here.
After ITO powder with the particle size of 0.5-1 mm is obtained, the ITO powder with the particle size of 0.5-1 mm is subjected to airflow crushing treatment and then screened to obtain ITO powder with the particle size of less than or equal to 5 micrometers. In the present invention, the jet milling treatment is preferably performed in an impact jet mill, and the present invention does not particularly require the configuration of the impact jet mill, and an impact jet mill having a configuration well known to those skilled in the art may be used. In the invention, the impact plate of the impact type jet mill is preferably an ITO plate, and the ITO plate is used as the impact plate, so that the pollution of a jet mill to powder is avoided, and the purity of the ITO powder is further improved.
In the present invention, the screening is preferably carried out by a screen machine, further pulverization and screening by the air current pulverization treatment are carried out to obtain ITO powder having a particle size of 5 μm or less, and the screened ITO powder having a particle size of more than 5 μm is again subjected to the air current pulverization treatment.
After the ITO powder with the particle size of less than or equal to 5 micrometers is obtained, the ITO powder with the particle size of less than or equal to 5 micrometers is subjected to vibration ball milling treatment to obtain the ITO powder with the particle size of 100-500 nm. In the present invention, the vibration ball milling treatment is preferably performed in a vibration ball mill, and the present invention does not particularly require the structure of the vibration ball mill, and a vibration ball mill having a structure well known to those skilled in the art may be used. In the invention, the excitation frequency of the vibration ball mill is preferably 800-1200 times/min, and more preferably 900-1100 times/min; the ball milling time is preferably 18-24 h, and more preferably 20-22 h.
In the invention, ITO grinding balls are preferably adopted in the vibration ball milling treatment, and the ball material ratio is preferably 3-5: 1, and more preferably 4: 1; the ITO grinding ball preferably comprises a large ball, a middle ball and a small ball; the diameter of the large ball is preferably 8-10 mm, more preferably 9mm, the diameter of the middle ball is preferably 5-8 mm, more preferably 7mm, and the diameter of the small ball is preferably 3-5 mm, more preferably 4 mm; the mass ratio of the big balls, the middle balls and the small balls is preferably 1:1: 2. The large balls, the medium balls and the small balls are mixed to carry out vibration ball milling treatment on the ITO powder with the particle size of less than 5 mu m, so that the ball milling efficiency and the ball milling quality can be improved. The invention takes the ITO grinding ball as the grinding ball of the vibrating ball mill, avoids the pollution of a vibrating ball mill to powder and further improves the purity of the ITO powder. And performing vibration ball milling treatment to obtain ITO powder with the particle size of 100-500 nm, and directly using the ITO powder for preparing ITO target materials.
The method processes the ITO residual target/waste target into ITO nano powder which can be directly used for preparing the ITO target material, does not need to carry out a large number of links of metal separation and purification, and has simple process, economy and environmental protection; according to the invention, the ITO target does not need to be atomized in the process of preparing the ITO powder, so that the energy consumption and the equipment cost are reduced, and the energy-saving and environment-friendly effects are achieved. Therefore, the method provided by the invention has the advantages of simple process, energy conservation, environmental protection and low production cost, and is suitable for large-scale production; meanwhile, the purity of the recovered ITO powder is high and can reach 99.99%, the recovery rate of the waste target is greatly improved, and the recovery rate of the waste target is more than 98%.
The following will describe in detail the method for collecting ITO powder from ITO targets in the present invention with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) The real object diagram of the ITO residual target is shown in figure 1, dust on the surface of the residual target is wiped off by using a clean cloth, the wiped residual target is put into sulfuric acid with the mass concentration of 10% to remove indium simple substance, then the indium-removed residual target is put into an ultrasonic cleaning machine, ultrasonic cleaning is carried out for 30min by using deionized water, and the indium-removed residual target is taken out and dried for standby;
(2) putting the cleaned residual target into a normal-pressure aerobic furnace for heating and heat preservation, wherein the heat preservation temperature is 1400 ℃, the flow of introduced oxygen is 120L/min, and the heat preservation time is 5h, then taking out the heated waste target, putting the waste target into normal-temperature deionized water, performing thermal stress crushing treatment, crushing the waste target into ITO particles with the particle size of 5-10 mm due to thermal stress under the condition of high-temperature shock cooling, and taking out the ITO particles after thermal stress crushing for drying for later use; the physical diagram of the ITO particles after thermal stress crushing is shown in FIG. 2;
(3) placing the dried ITO particles into a vertical ring roller mill for ring roller milling and crushing treatment, wherein the rotating speed of a main shaft of the ring roller mill is controlled at 200r/min, the ITO particles are crushed into powder with the particle size of about 0.5mm after ring roller milling, and a natural stacking state real object diagram of the ITO powder after ring roller milling and crushing treatment is shown in FIG. 3; putting the crushed powder into a dilute sulfuric acid solution with the mass concentration of 5% for acid washing for 20min, then putting the powder into an ultrasonic cleaning machine, ultrasonically cleaning the powder with deionized water for 30min, taking out the powder and drying the powder for later use;
(4) Placing the ITO powder crushed by the ring roller mill into an impact type airflow crusher for further crushing, wherein an impact plate used in the airflow crusher is an ITO plate, a scanning electron microscope image of the ITO powder after airflow crushing is shown in figure 4, and as can be seen from figure 4, after airflow crushing, most of the ITO powder has been crushed to be less than 5 mu m, and only a small amount of powder has larger particle size;
placing the ITO powder after jet milling into a screening machine for screening, carrying out next treatment on the powder with the particle size of less than or equal to 5 microns, and placing the powder with the particle size of more than 5 microns into the jet mill again for secondary milling;
(5) putting the screened ITO powder into a vibration ball mill, wherein the vibration ball mill adopts ITO grinding balls, the ball-material ratio is controlled to be 5:1, the mass ratio of large balls, medium balls and small balls of the grinding balls is 1:1:2, the diameter of the large balls is 10mm, the diameter of the medium balls is 8mm, the diameter of the small balls is 5mm, the excitation frequency of the ball mill is 1200 times/min, the ball milling time is 24h, the particle size distribution diagram of the ITO powder obtained after ball milling is shown in figure 5, and as can be seen from figure 5, the particle size of the ITO powder obtained after ball milling is 100-500 nm, and the average particle size is 237 nm.
Example 2
(1) Wiping off dust on the surface of the ITO residual target by using a clean cloth, putting the wiped residual target into sulfuric acid with the mass concentration of 12% for immersion cleaning for 15min to remove indium simple substances, then putting the indium-removed residual target into an ultrasonic cleaning machine, ultrasonically cleaning for 30min by using deionized water, taking out and drying for later use;
(2) Putting the cleaned residual target into a normal-pressure aerobic furnace for heating and heat preservation, wherein the heat preservation temperature is 1300 ℃, the flow of introduced oxygen is 110L/min, and the heat preservation time is 4h, then taking out the heated waste target, putting the waste target into normal-temperature deionized water, performing thermal stress crushing treatment, crushing the waste target into ITO particles with the particle size of 5-10 mm due to thermal stress under the condition of high-temperature shock cooling, and taking out and drying the ITO particles after thermal stress crushing for later use;
(3) placing the dried ITO particles into a vertical ring roller mill for ring roller grinding and crushing treatment, controlling the rotating speed of a main shaft of the ring roller mill at 180r/min, crushing the ITO particles into powder with the particle size of about 0.5mm after ring roller grinding, placing the crushed powder into a dilute sulfuric acid solution with the mass concentration of 8% for acid washing for 20min, then placing the powder into an ultrasonic cleaning machine, ultrasonically cleaning the powder for 30min by using deionized water, taking out the powder and drying the powder for later use;
(4) the ITO powder crushed by the ring roller mill is put into an impact type airflow crusher for further crushing, an impact plate used in the airflow crusher is an ITO plate, after airflow crushing, most of the ITO powder is crushed to be less than 5 mu m, and only a small amount of powder has larger particle size;
Placing the ITO powder after jet milling into a screening machine for screening, carrying out next treatment on the powder with the particle size of less than or equal to 5 microns, and placing the powder with the particle size of more than 5 microns into the jet mill again for secondary milling;
(5) putting the screened ITO powder into a vibration ball mill, wherein the vibration ball mill adopts ITO grinding balls, the ball-material ratio is controlled to be 5:1, the mass ratio of large balls, medium balls and small balls of the grinding balls is 1:1:2, the diameter of the large balls is 8mm, the diameter of the medium balls is 5mm, the diameter of the small balls is 3mm, the excitation frequency of the ball mill is 1200 times/min, the ball milling time is 24h, the particle size of the ITO powder obtained after ball milling is 100-500 nm, and the average particle size is 245 nm.
Example 3
(1) Wiping off dust on the surface of the ITO residual target by using a clean cloth, putting the wiped residual target into sulfuric acid with the mass concentration of 15% for immersion cleaning for 10min to remove an indium simple substance, then putting the indium-removed residual target into an ultrasonic cleaning machine, ultrasonically cleaning for 30min by using deionized water, taking out and drying for later use;
(2) putting the cleaned residual target into a normal-pressure aerobic furnace for heating and heat preservation, wherein the heat preservation temperature is 1200 ℃, the flow of introduced oxygen is 100L/min, and the heat preservation time is 5h, then taking out the heated waste target, putting the waste target into normal-temperature deionized water, and carrying out thermal stress crushing treatment, wherein the waste target is crushed into ITO particles with the particle size of 5-10 mm due to thermal stress under the condition of high-temperature shock cooling, and then taking out the ITO particles after thermal stress crushing for drying for later use;
(3) Placing the dried ITO particles into a vertical ring roller mill for ring roller grinding and crushing treatment, controlling the rotating speed of a main shaft of the ring roller mill to be 190r/min, crushing the ITO particles into powder with the particle size of about 0.5mm after ring roller grinding, placing the crushed powder into a dilute sulfuric acid solution with the mass concentration of 10% for acid washing for 20min, then placing the powder into an ultrasonic cleaning machine, ultrasonically cleaning the powder for 30min by using deionized water, taking out the powder and drying the powder for later use;
(4) the ITO powder crushed by the ring roller mill is put into an impact type airflow crusher for further crushing, an impact plate used in the airflow crusher is an ITO plate, after airflow crushing, most of the ITO powder is crushed to be less than 5 mu m, and only a small amount of powder has larger particle size;
placing the ITO powder after jet milling into a screening machine for screening, carrying out next treatment on the powder with the particle size of less than or equal to 5 microns, and placing the powder with the particle size of more than 5 microns into the jet mill again for secondary milling;
(5) placing the screened ITO powder into a vibration ball mill, wherein the vibration ball mill adopts ITO grinding balls, the ball-material ratio is controlled to be 5:1, the mass ratio of large balls, medium balls and small balls of the grinding balls is 1:1:2, the diameter of the large balls is 10mm, the diameter of the medium balls is 5mm, the diameter of the small balls is 3mm, the excitation frequency of the ball mill is 1200 times/min, the ball milling time is 24 hours, the particle size of the ITO powder obtained after ball milling is 100-500 nm, and the average particle size is 250 nm.
The ITO powder recovered from the ITO residual target by the methods of the embodiments 1 to 3 has the purity of more than 99.99% and the recovery rate of more than 98%, and the method has the advantages of energy conservation, environmental protection, simple flow, low production cost and suitability for large-scale production in factories.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for recovering ITO powder from an ITO residual target/waste target is characterized by comprising the following steps:
(1) pickling the ITO residual target/waste target with a clean surface by using strong acid to obtain an indium-removing target material;
(2) heating and insulating the indium-removing target material under the condition of introducing oxygen, and then soaking the insulated target material into water for quenching to carry out thermal stress crushing to obtain ITO particles with the particle size of 5-10 mm; the flow rate of the introduced oxygen is 100-120L/min; the heating and heat preservation temperature is 1200-1400 ℃, and the heat preservation time is 2-5 h;
(3) performing ring rolling crushing treatment on the ITO particles with the particle size of 5-10 mm to obtain ITO powder with the particle size of 0.5-1 mm;
(4) Carrying out airflow crushing treatment on the ITO powder with the particle size of 0.5-1 mm, and screening to obtain ITO powder with the particle size of less than or equal to 5 micrometers;
(5) and carrying out vibration ball milling treatment on the ITO powder with the particle size of less than or equal to 5 microns to obtain the ITO powder with the particle size of 100-500 nm.
2. The method according to claim 1, wherein the step (2) comprises drying the ITO particles after removing the ITO particles from the water after the thermal stress cracking.
3. The method according to claim 1, characterized in that the ring roll mill crushing treatment in the step (3) is performed in a vertical ring roll mill; the rotating speed of the main shaft of the vertical ring roller mill is 180-200 r/min.
4. The method of claim 1, wherein the step (3) further comprises acid washing the ITO powder obtained after crushing with a strong acid after the ring roll crushing treatment.
5. The method according to claim 1 or 4, wherein the step (1) or step (3) after acid washing independently further comprises sequentially subjecting the acid-washed ITO product to ultrasonic washing and drying; the ultrasonic cleaning adopts water as a cleaning agent.
6. The method as claimed in claim 1, wherein the air stream-breaking treatment in the step (4) is performed in an impact jet mill; the impact plate of the impact type jet mill is an ITO plate.
7. The method according to claim 1, wherein the vibratory ball milling treatment in step (5) is carried out in a vibratory ball mill; the vibration frequency of the vibration ball mill is 800-1200 times/min, and the ball milling time is 18-24 hours.
8. The method according to claim 7, wherein the vibratory ball milling treatment adopts ITO (indium tin oxide) milling balls, and the ball-to-material ratio is 3-5: 1.
9. The method of claim 8, wherein the ITO grinding balls comprise large balls, medium balls, and small balls; the diameter of the big ball is 8-10 mm, the diameter of the middle ball is 5-8 mm, and the diameter of the small ball is 3-5 mm; the mass ratio of the big balls to the middle balls to the small balls is 1:1: 2.
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| CN112079627A (en) * | 2020-09-16 | 2020-12-15 | 韶关市欧莱高新材料有限公司 | Preparation method for directly crushing ITO waste target to prepare powder and producing ITO target |
| CN112708763B (en) * | 2020-12-15 | 2022-09-06 | 先导薄膜材料（广东）有限公司 | Method for recovering valuable metal from ITO waste target |
| CN112608143A (en) * | 2021-01-19 | 2021-04-06 | 福州大学 | Preparation method of slurry for ITO target slip casting process |
| CN113292345A (en) * | 2021-05-28 | 2021-08-24 | 芜湖映日科技股份有限公司 | Preparation process for recycling residual target after ITO target sputtering |
| CN114275808A (en) * | 2021-07-01 | 2022-04-05 | 芜湖映日科技股份有限公司 | Preparation process of nanoscale ITO powder for TFT-LCD target |
| CN114956162B (en) * | 2022-07-04 | 2023-10-13 | 广东先导稀贵金属材料有限公司 | Recovery method of indium oxide waste |
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