CN114032517A - Preparation method of rare earth ion doped ITO target material - Google Patents
Preparation method of rare earth ion doped ITO target material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention provides a preparation method of a rare earth ion doped ITO target, belonging to the field of ITO targets, wherein the ITO target powder is prepared by vacuum powder feeding, coarse powder grinding, fine powder grinding, nano-scale powder sanding, slurry glue preparation, spray granulation, mixing and sieving, and then dry pressing and cold isostatic pressing molding, biscuit turning, sintering, machining and binding detection are carried out.
Description
Technical Field
The invention relates to the field of ITO target materials, in particular to a preparation method of rare earth ion doped ITO target materials.
Background
Indium Tin Oxide (ITO) target films are widely used in the fields of solar energy, liquid crystal displays, touch panels, semiconductor display devices, and the like, due to their excellent characteristics of high transmittance, low impedance, high weatherability, and the like. The ITO target material is a main raw material for preparing an ITO film material by magnetron sputtering. The ITO target material film required by the solar cell industry needs to have the characteristics of low resistivity, high carrier mobility, high light transmittance, good film uniformity and the like. ITO target materials with different proportions can be prepared by adjusting the proportions of indium oxide and tin oxide, so that the performance control of the ITO film, such as square resistance, transmittance, carrier concentration, carrier mobility and the like, can be realized. However, as the content of tin oxide in the ITO target material is reduced, the difficulty of sintering the target material to be dense is higher and higher because the melting point of tin oxide is lower than that of indium oxide. Rare earth oxide powder including but not limited to Pr2O5, Y2O3 and the like can be added in the preparation of the ITO target, so that the thin carrier mobility of the ITO target can be effectively improved, the density of the target can be improved, the cracking rate can be reduced, and the yield of products can be improved. At present, corresponding process methods are lacked for doping rare earth ions into ITO target materials, and a preparation method of rare earth ion doped ITO target materials is needed.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a rare earth ion doped ITO target, which comprises the steps of carrying out vacuum powder feeding, coarse powder grinding, fine powder grinding, nano-scale powder sanding, slurry glue preparation, spray granulation, mixing and sieving to prepare powder of the ITO target, then carrying out dry pressing and cold isostatic pressing forming, turning processing, sintering, machining and binding detection on a biscuit, and by adding rare earth oxide powder, the problems of low density and easiness in cracking of the ITO target with a high indium-tin ratio are solved, the carrier mobility of a film is improved, the ITO target can be better applied to the solar cell industry, and the problems in the background technology are solved.
The invention aims to provide a preparation method of rare earth ion doped ITO target material,
the method comprises the following steps: adding a certain amount of water into a premixing tank, wherein the ratio of indium oxide powder to tin oxide powder is 90-97: 3-10, adding 0.1-1.0wt.% of rare earth oxide powder, and then pouring into a vacuum feeder for automatic feeding;
step two: after the feeding is finished, starting a stirring paddle of the premixing tank to perform coarse grinding; after the coarse grinding is finished, beating the slurry into a first sand grinding storage tank, starting a main machine of a fine grinding sand grinder, and performing self-circulation fine grinding; after the fine grinding is finished, pumping the ITO slurry into a second storage tank by using a diaphragm pump, starting a nanoscale sand mill for nanoscale sand grinding, and adding a dispersing agent;
step four: after sanding, sieving with a sieve mesh number of 200 meshes and 400 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, stirring for 2H at a stirring speed of 400 rpm/min;
step five: after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size;
step six: carrying out molding treatment on the powder, and carrying out dry pressing and cold isostatic pressing molding on the powder by putting the powder into a mold; turning the formed biscuit to a specified shape;
step seven: putting the processed biscuit into a sintering furnace for degreasing and sintering at normal pressure to obtain a target material, and then machining the target material: cutting, edging and grinding the inner circle and the outer circle.
The further improvement lies in that: the sintering in the seventh step is as follows:
(1) heating to 600 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2-5h, and introducing oxygen at a flow rate of 8L/min;
(2) heating to 1250-;
(3) heating to 1600 ℃ and 1650 ℃ at the heating rate of 0.3 ℃/min, and keeping the temperature for 10-20h, wherein the flow rate of the introduced oxygen is 16L/min;
(4) the temperature is reduced to 1250-;
(5) then stopping introducing oxygen, and naturally cooling to room temperature.
The further improvement lies in that: the diameter of the coarse grinding zirconium beads is 5-10mm, the grinding time is 4-20 hours, and the speed of a stirrer is 50-100 rpm.
The further improvement lies in that: the diameter of the fine grinding zirconium beads is 0.8-1.0mm, the rotating speed of a main machine is 1000-.
The further improvement lies in that: the diameter of the zirconium beads of the nano-level sand mill for nano-level sand grinding is 0.05-0.1mm, the rotating speed of a main machine is 1600rpm, and the flow rate of a feeding pump is 500-.
The further improvement lies in that: binding the machined target material, detecting the quality, performing magnetron sputtering coating on the target material with qualified quality detection, and testing the carrier mobility of the characteristic film.
The further improvement lies in that: performing magnetron sputtering coating on the qualified target material, wherein the coating conditions are as follows: (1) coating power: 100W; (2) film coating pressure: 0.5 Pa; (3) coating time: and 20 min.
The invention has the beneficial effects that: by adding the rare earth oxide powder, the problems of low density and easy cracking of the ITO target with high indium tin ratio are solved, the carrier mobility of the film is improved, and the film can be better applied to the solar cell industry; according to the invention, through coarse grinding, fine grinding and nano-level sanding, the prepared powder has high uniformity and high dispersibility, and through the designed sintering process, the sintered target material has high density, ensures large size, high density and high density uniformity and has no cracking phenomenon; the invention also carries out quality detection after the target material is processed and bound, and carries out magnetron sputtering coating on the target material with qualified quality detection to test the carrier mobility of the characterization film.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a preparation method of a rare earth ion doped ITO target, which comprises the following steps:
s1: mixing indium oxide and tin oxide powder according to the weight ratio of 97: 3, and then adding 0.5wt.% of rare earth oxide powder; then, coarse grinding is carried out, the diameter of the zirconium beads is 7mm, the grinding time is 10 hours, and the speed of a stirrer is 70 rpm; after coarse grinding, self-circulation fine grinding is carried out, the diameter of the fine grinding zirconium beads is 1.0mm, the rotating speed of a main machine is 1100rpm, and the flow rate of a feeding pump is 1000L/min; carrying out nano-grade sanding after fine grinding, wherein the diameter of zirconium beads of the nano-grade sanding machine is 0.1mm, the rotating speed of a main machine is 1600rpm, the flow of a feed pump is 550L/min, and meanwhile, a dispersing agent is added; then, sieving the slurry with the sieve mesh number of 300 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, and stirring for 2H at the stirring speed of 400 rpm/min; after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size; obtaining nanoscale RE ITO powder;
s2: putting the powder prepared in the step S1 into a die, carrying out cold isostatic pressing under the pressure of 300MPa, and keeping the pressure for 30min to obtain a RE ITO biscuit;
s3: turning the biscuit of S2 to set size and properties;
s4: and (3) putting the biscuit processed by the S3 into a sintering furnace for degreasing and sintering at normal pressure. The sintering process comprises the following steps: firstly, heating to 600 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, and introducing oxygen at a flow rate of 8L/min;
secondly, heating to 1250 ℃ at the heating rate of 1.5 ℃/min, preserving the heat for 8 hours, and introducing oxygen at the flow rate of 12L/min;
thirdly, heating to 1650 ℃ at the heating rate of 0.3 ℃/min, preserving the heat for 15h, and introducing oxygen with the flow rate of 16L/min;
fourthly, reducing the temperature to 1250 ℃ at the cooling rate of 5 ℃/min, and introducing oxygen at the flow rate of 16L/min;
fifthly, stopping introducing oxygen, and naturally cooling to room temperature; preparation of 97: 3, RE is ITO target material with unchanged shape and relative density up to 99.0%;
s5: binding the RE ITO target material of S4 on the outer surface of the titanium tube and carrying out ultrasonic flaw detection;
s6: carrying out magnetron sputtering coating on the target material of S5 under the following coating conditions: coating power: 100W; film coating pressure: 0.5 Pa; coating time: 20 min; the prepared film was subjected to a hall effect test, and the carrier mobility was measured to be 8.9cm 2/(Vs).
Example 2
The embodiment provides a preparation method of a rare earth ion doped ITO target, which comprises the following steps:
s1: mixing indium oxide and tin oxide powder according to the weight ratio of 95: 5, adding 0.5wt.% of rare earth oxide powder, then carrying out coarse grinding, carrying out coarse grinding on zirconium beads with the diameter of 7mm, carrying out grinding for 10 hours, and carrying out the speed of a stirrer at 70 rpm; after coarse grinding, self-circulation fine grinding is carried out, the diameter of the fine grinding zirconium beads is 1.0mm, the rotating speed of a main machine is 1100rpm, and the flow rate of a feeding pump is 1000L/min; carrying out nano-grade sanding after fine grinding, wherein the diameter of zirconium beads of the nano-grade sanding machine is 0.1mm, the rotating speed of a main machine is 1600rpm, the flow of a feed pump is 550L/min, and meanwhile, a dispersing agent is added; then, sieving the slurry with the sieve mesh number of 300 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, and stirring for 2H at the stirring speed of 400 rpm/min; after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size; obtaining nanoscale RE ITO powder;
s2: putting the powder prepared in the step S1 into a die, carrying out cold isostatic pressing under the pressure of 280MPa, and keeping the pressure for 30min to obtain a RE ITO biscuit;
s3: turning the biscuit of S2 to set size and properties;
s4: and (3) putting the biscuit processed by the S3 into a sintering furnace for degreasing and sintering at normal pressure. The sintering process comprises the following steps:
firstly, heating to 600 ℃ at a heating rate of 5 ℃/min, preserving heat for 3h, and introducing oxygen at a flow rate of 8L/min;
secondly, heating to 1300 ℃ at the heating rate of 1.5 ℃/min, preserving the temperature for 8 hours, and introducing oxygen at the flow rate of 12L/min;
thirdly, heating to 1630 ℃ at the heating rate of 0.3 ℃/min, preserving the temperature for 13h, and introducing oxygen at the flow rate of 16L/min;
fourthly, reducing the temperature to 1300 ℃ at the cooling rate of 5 ℃/min, and introducing oxygen at the flow rate of 16L/min;
fifthly, stopping introducing oxygen, and naturally cooling to room temperature; 95 of preparation: 5, RE is the ITO target material with unchanged shape and relative density reaching 99.2 percent;
s5: binding the RE ITO target material of S4 on the outer surface of the titanium tube and carrying out ultrasonic flaw detection;
s6: carrying out magnetron sputtering coating on the target material of S5 under the following coating conditions: coating power: 100W; film coating pressure: 0.5 Pa; coating time: 20 min; the prepared film was subjected to a hall effect test, and the carrier mobility was measured to be 5.7cm 2/(Vs).
Example 3
The embodiment provides a preparation method of a rare earth ion doped ITO target, which comprises the following steps:
s1: mixing indium oxide and tin oxide powder according to the weight ratio of 93: 7, adding 0.5wt.% of rare earth oxide powder, then carrying out coarse grinding, carrying out coarse grinding on zirconium beads with the diameter of 7mm, carrying out grinding for 10 hours, and carrying out the speed of a stirrer at 70 rpm; after coarse grinding, self-circulation fine grinding is carried out, the diameter of the fine grinding zirconium beads is 1.0mm, the rotating speed of a main machine is 1100rpm, and the flow rate of a feeding pump is 1000L/min; carrying out nano-grade sanding after fine grinding, wherein the diameter of zirconium beads of the nano-grade sanding machine is 0.1mm, the rotating speed of a main machine is 1600rpm, the flow of a feed pump is 550L/min, and meanwhile, a dispersing agent is added; then, sieving the slurry with the sieve mesh number of 300 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, and stirring for 2H at the stirring speed of 400 rpm/min; after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size; obtaining nanoscale RE ITO powder;
s2: putting the powder prepared in the S1 into a die, carrying out cold isostatic pressing under the pressure of 250MPa, and keeping the pressure for 30min to obtain a RE ITO biscuit;
s3: turning the biscuit of S2 to set size and properties;
s4: placing the biscuit processed by the S3 into a sintering furnace for degreasing and sintering at normal pressure; the sintering process comprises the following steps: (1) heating to 600 ℃ at the heating rate of 5 ℃/min, preserving the heat for 4h, and introducing oxygen at the flow rate of 8L/min; (2) heating to 1350 ℃ at the heating rate of 1.5 ℃/min, preserving the heat for 8h, and introducing oxygen at the flow rate of 12L/min; (3) heating to 1600 ℃ at the heating rate of 0.3 ℃/min, preserving the heat for 10h, and introducing oxygen at the flow rate of 16L/min; (4) reducing the temperature to 1350 ℃ at a cooling rate of 5 ℃/min, and introducing oxygen at a flow rate of 16L/min; (5) then stopping introducing oxygen, and naturally cooling to room temperature. Preparation of 93: 7, RE is ITO target material with unchanged shape and relative density reaching 99.4%;
s5: binding the RE ITO target material of S4 on the outer surface of the titanium tube and carrying out ultrasonic flaw detection;
s6: carrying out magnetron sputtering coating on the target material of S5 under the following coating conditions: coating power: 100W; film coating pressure: 0.5 Pa; coating time: 20 min; the prepared film was subjected to a hall effect test, and the carrier mobility was measured to be 3.3cm 2/(Vs).
Example 4
The embodiment provides a preparation method of a rare earth ion doped ITO target, which comprises the following steps:
s1: mixing indium oxide and tin oxide powder according to the weight ratio of 90: 10, adding 0.5wt.% of rare earth oxide powder, then carrying out coarse grinding, carrying out coarse grinding on zirconium beads with the diameter of 7mm, carrying out grinding for 10 hours, and carrying out the speed of a stirrer at 70 rpm; after coarse grinding, self-circulation fine grinding is carried out, the diameter of the fine grinding zirconium beads is 1.0mm, the rotating speed of a main machine is 1100rpm, and the flow rate of a feeding pump is 1000L/min; carrying out nano-grade sanding after fine grinding, wherein the diameter of zirconium beads of the nano-grade sanding machine is 0.1mm, the rotating speed of a main machine is 1600rpm, the flow of a feed pump is 550L/min, and meanwhile, a dispersing agent is added; then, sieving the slurry with the sieve mesh number of 300 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, and stirring for 2H at the stirring speed of 400 rpm/min; after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size; obtaining nanoscale RE ITO powder;
s2: putting the powder prepared in the step S1 into a die, carrying out cold isostatic pressing under the pressure of 230MPa, and keeping the pressure for 30min to obtain a RE ITO biscuit;
s3: turning the biscuit of S2 to set size and properties;
s4: placing the biscuit processed by the S3 into a sintering furnace for degreasing and sintering at normal pressure; the sintering process comprises the following steps:
firstly, heating to 600 ℃ at a heating rate of 5 ℃/min, preserving the heat for 5 hours, and introducing oxygen at a flow rate of 8L/min;
secondly, heating to 1400 ℃ at the heating rate of 1.5 ℃/min, preserving the heat for 8 hours, and introducing oxygen at the flow rate of 12L/min;
thirdly, heating to 1600 ℃ at the heating rate of 0.3 ℃/min, preserving the heat for 20 hours, and introducing oxygen at the flow rate of 16L/min;
fourthly, reducing the temperature to 1400 ℃ at the cooling rate of 5 ℃/min, and introducing oxygen at the flow rate of 16L/min;
and fifthly, stopping introducing oxygen, and naturally cooling to room temperature. 90 of the preparation: 10, RE is ITO target material with unchanged shape and relative density reaching 99.4%;
s5: binding the RE ITO target material of S4 on the outer surface of the titanium tube and carrying out ultrasonic flaw detection;
s6: carrying out magnetron sputtering coating on the target material of S5 under the following coating conditions: coating power: 100W; film coating pressure: 0.5 Pa; coating time: 20 min; the prepared film was subjected to a hall effect test, and the carrier mobility was measured to be 1.6cm 2/(Vs).
Comparative example 1
Mixing indium oxide and tin oxide powder according to the weight ratio of 97: 3, the other steps are the same as the example 1 without adding the rare earth oxide powder; the sintered target material has cracking or machining cracking phenomenon, and the relative density is 98.2%; after the target material was cut, the film was formed under the same film-forming process as in the examples and tested, and the carrier mobility was measured to be 0.8cm 2/(Vs).
Comparative example 2
Mixing indium oxide and tin oxide powder according to the weight ratio of 97: 3, and then adding 0.3wt.% of rare earth oxide powder, wherein the other steps are the same as the first embodiment; the sintered target material has cracking or machining cracking phenomenon, and the relative density is 99.2%. After the target material was cut, the film was formed under the same film-forming process as in the examples and tested, and the carrier mobility was measured to be 7.1cm 2/(Vs).
Comparative example 3
Mixing indium oxide and tin oxide powder according to the weight ratio of 97: 3, and then adding 0.8wt.% of rare earth oxide powder, wherein the other steps are the same as the first embodiment; the sintered target material has cracking or machining cracking phenomenon, and the relative density is 99.5%; after the target material was cut, the film was formed under the same film-forming process as in the examples and tested, and the carrier mobility was measured to be 10.3cm 2/(Vs).
TABLE 1
| In:Sn（wt.%) | Pr2O5（wt.%) | Relative density (%) | μ(cm2V-1s-1) | |
| Example 4 | 90:10 | 0.5 | 99.0 | 8.9 |
| Example 3 | 93:7 | 0.5 | 99.2 | 5.7 |
| Example 2 | 95:5 | 0.5 | 99.4 | 3.3 |
| Example 1 | 97:3 | 0.5 | 99.4 | 1.6 |
| Comparative example 1 | 97:3 | 0 | 98.2 | 0.8 |
| Comparative example 2 | 97:3 | 0.3 | 99.2 | 7.1 |
| Comparative example 3 | 97:3 | 0.8 | 99.5 | 10.3 |
From the results in table 1, it can be found that the higher the content of indium oxide is, the higher the carrier mobility of the thin film prepared by magnetron sputtering coating of the target material is; 97 prepared by adding rare earth oxide: 3, the ITO target material has no crack, and the carrier mobility of the film of the target material after magnetron sputtering is also larger than that of the film prepared without adding rare earth oxide.
Claims (7)
1. A preparation method of rare earth ion doped ITO target material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adding a certain amount of water into a premixing tank, wherein the ratio of indium oxide powder to tin oxide powder is 90-97: 3-10, adding 0.1-1.0wt.% of rare earth oxide powder, and then pouring into a vacuum feeder for automatic feeding;
step two: after the feeding is finished, starting a stirring paddle of the premixing tank to perform coarse grinding; after the coarse grinding is finished, beating the slurry into a first sand grinding storage tank, starting a main machine of a fine grinding sand grinder, and performing self-circulation fine grinding; after the fine grinding is finished, pumping the ITO slurry into a second storage tank by using a diaphragm pump, starting a nanoscale sand mill for nanoscale sand grinding, and adding a dispersing agent;
step four: after sanding, sieving with a sieve mesh number of 200 meshes and 400 meshes, transferring the sieved slurry into a glue blending tank, adding a binder and a defoaming agent, stirring for 2H at a stirring speed of 400 rpm/min;
step five: after stirring, granulating the ITO slurry, mixing the granulated ITO powder, and sieving by grades to finally obtain ITO powder with primary particle size and secondary particle size;
step six: carrying out molding treatment on the powder, and carrying out dry pressing and cold isostatic pressing molding on the powder by putting the powder into a mold; turning the formed biscuit to a specified shape;
step seven: putting the processed biscuit into a sintering furnace for degreasing and sintering at normal pressure to obtain a target material, and then machining the target material: cutting, edging and grinding the inner circle and the outer circle.
2. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: the sintering in the seventh step is as follows:
(1) heating to 600 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2-5h, and introducing oxygen at a flow rate of 8L/min;
(2) heating to 1250-;
(3) heating to 1600 ℃ and 1650 ℃ at the heating rate of 0.3 ℃/min, and keeping the temperature for 10-20h, wherein the flow rate of the introduced oxygen is 16L/min;
(4) the temperature is reduced to 1250-;
(5) then stopping introducing oxygen, and naturally cooling to room temperature.
3. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: the diameter of the coarse grinding zirconium beads is 5-10mm, the grinding time is 4-20 hours, and the speed of a stirrer is 50-100 rpm.
4. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: the diameter of the fine grinding zirconium beads is 0.8-1.0mm, the rotating speed of a main machine is 1000-.
5. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: the diameter of the zirconium beads of the nano-level sand mill for nano-level sand grinding is 0.05-0.1mm, the rotating speed of a main machine is 1600rpm, and the flow rate of a feeding pump is 500-.
6. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: binding the machined target material, detecting the quality, performing magnetron sputtering coating on the target material with qualified quality detection, and testing the carrier mobility of the characteristic film.
7. The method for preparing the rare earth ion-doped ITO target material according to claim 1, wherein the method comprises the following steps: performing magnetron sputtering coating on the qualified target material, wherein the coating conditions are as follows: (1) coating power: 100W; (2) film coating pressure: 0.5 Pa; (3) coating time: and 20 min.
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| CN116715516A (en) * | 2023-05-19 | 2023-09-08 | 芜湖映日科技股份有限公司 | Rare earth doped ITO target and preparation method thereof |
| CN116813329A (en) * | 2023-05-30 | 2023-09-29 | 芜湖映日科技股份有限公司 | Preparation method of high-density tin-tantalum oxide target |
| CN116813310A (en) * | 2023-06-01 | 2023-09-29 | 先导薄膜材料（广东）有限公司 | Rare earth element doped indium tin gallium oxide target material and preparation method thereof |
| CN116835964A (en) * | 2023-06-12 | 2023-10-03 | 先导薄膜材料（广东）有限公司 | Indium cerium tantalum titanium oxide target material with low zirconium content and preparation method thereof |
| CN117247273A (en) * | 2023-11-17 | 2023-12-19 | 江苏迪纳科精细材料股份有限公司 | Preparation method and device of X-IZO magnetron sputtering target material with high mobility |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054455A (en) * | 2007-04-27 | 2007-10-17 | 南京工业大学 | Nano semi-conductor metal oxide paste composition and preparing process thereof |
| JP2010030824A (en) * | 2008-07-28 | 2010-02-12 | Idemitsu Kosan Co Ltd | Metal phase-containing indium oxide sintered compact and method for producing the same |
| KR20110054863A (en) * | 2009-11-18 | 2011-05-25 | 한국전자통신연구원 | Thermal stability transparent conductive thin film and method for preparing thermal stability transparent conductive thin film |
| JP2012126937A (en) * | 2010-12-13 | 2012-07-05 | Sumitomo Metal Mining Co Ltd | Ito sputtering target and manufacturing method thereof |
| TW201434788A (en) * | 2012-11-09 | 2014-09-16 | Idemitsu Kosan Co | Sputtering target, oxide semiconductor thin film, and methods for producing these products |
| WO2015052927A1 (en) * | 2013-10-09 | 2015-04-16 | 出光興産株式会社 | Sputtering target and method for producing same |
| CN107130217A (en) * | 2017-06-01 | 2017-09-05 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of low cost, the preparation method of high-density ITO targe material |
| CN110797395A (en) * | 2019-09-18 | 2020-02-14 | 华南理工大学 | Doped metal oxide semiconductor, thin film transistor and application |
| CN111592339A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | ITO target material and preparation method thereof |
-
2021
- 2021-10-22 CN CN202111234757.3A patent/CN114032517A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054455A (en) * | 2007-04-27 | 2007-10-17 | 南京工业大学 | Nano semi-conductor metal oxide paste composition and preparing process thereof |
| JP2010030824A (en) * | 2008-07-28 | 2010-02-12 | Idemitsu Kosan Co Ltd | Metal phase-containing indium oxide sintered compact and method for producing the same |
| KR20110054863A (en) * | 2009-11-18 | 2011-05-25 | 한국전자통신연구원 | Thermal stability transparent conductive thin film and method for preparing thermal stability transparent conductive thin film |
| JP2012126937A (en) * | 2010-12-13 | 2012-07-05 | Sumitomo Metal Mining Co Ltd | Ito sputtering target and manufacturing method thereof |
| TW201434788A (en) * | 2012-11-09 | 2014-09-16 | Idemitsu Kosan Co | Sputtering target, oxide semiconductor thin film, and methods for producing these products |
| WO2015052927A1 (en) * | 2013-10-09 | 2015-04-16 | 出光興産株式会社 | Sputtering target and method for producing same |
| CN107130217A (en) * | 2017-06-01 | 2017-09-05 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of low cost, the preparation method of high-density ITO targe material |
| CN110797395A (en) * | 2019-09-18 | 2020-02-14 | 华南理工大学 | Doped metal oxide semiconductor, thin film transistor and application |
| CN111592339A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | ITO target material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 罗民华: "《陶瓷工业节能减排与污染综合治理》", 中国建材工业出版社, pages: 17 - 19 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115745572A (en) * | 2022-10-31 | 2023-03-07 | 芜湖映日科技股份有限公司 | Rare earth doped X-IGZO target material and preparation method thereof |
| CN116715516A (en) * | 2023-05-19 | 2023-09-08 | 芜湖映日科技股份有限公司 | Rare earth doped ITO target and preparation method thereof |
| CN116813329A (en) * | 2023-05-30 | 2023-09-29 | 芜湖映日科技股份有限公司 | Preparation method of high-density tin-tantalum oxide target |
| CN116813310A (en) * | 2023-06-01 | 2023-09-29 | 先导薄膜材料（广东）有限公司 | Rare earth element doped indium tin gallium oxide target material and preparation method thereof |
| CN116835964A (en) * | 2023-06-12 | 2023-10-03 | 先导薄膜材料（广东）有限公司 | Indium cerium tantalum titanium oxide target material with low zirconium content and preparation method thereof |
| CN117247273A (en) * | 2023-11-17 | 2023-12-19 | 江苏迪纳科精细材料股份有限公司 | Preparation method and device of X-IZO magnetron sputtering target material with high mobility |
| CN117247273B (en) * | 2023-11-17 | 2024-02-23 | 江苏迪纳科精细材料股份有限公司 | Preparation method and device of X-IZO magnetron sputtering target material with high mobility |
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