CN116715516A - Rare earth doped ITO target and preparation method thereof - Google Patents
Rare earth doped ITO target and preparation method thereof Download PDFInfo
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- CN116715516A CN116715516A CN202310570152.4A CN202310570152A CN116715516A CN 116715516 A CN116715516 A CN 116715516A CN 202310570152 A CN202310570152 A CN 202310570152A CN 116715516 A CN116715516 A CN 116715516A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 33
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000005245 sintering Methods 0.000 claims abstract description 46
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910001195 gallium oxide Inorganic materials 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000013077 target material Substances 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 18
- 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 18
- 239000007921 spray Substances 0.000 claims abstract description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 18
- 238000005469 granulation Methods 0.000 claims abstract description 11
- 230000003179 granulation Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 102220043159 rs587780996 Human genes 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 3
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- 210000001161 mammalian embryo Anatomy 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000036326 tumor accumulation Effects 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 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
- C04B35/453—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 based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—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 based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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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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- 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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
Abstract
The invention relates to the technical field of targets, in particular to a rare earth doped ITO target and a preparation method thereof, wherein the rare earth doped ITO target is prepared by the following preparation method: the method comprises the steps of (1) gallium oxide ball milling, (2) spray granulation, (3) pressure forming, (4) high-temperature sintering and (5) grinding by a grinding machine; the method adopts a mode of pre-ball milling gallium oxide to uniformly mix high-activity nano gallium oxide, indium oxide and tin oxide powder, and sintering is carried out through different temperature sections and different heating rates, so that indium tin gallium oxide fully reacts to obtain the rare earth doped ITO target material with fine grains and high performance.
Description
Technical Field
The invention relates to the technical field of targets, in particular to a rare earth doped ITO target and a preparation method thereof.
Background
Indium Tin Oxide (ITO) target films are widely used in the fields of solar energy, liquid crystal display, touch screens, semiconductor display devices and the like because of excellent characteristics such as high transmittance, low impedance, high weather resistance and the like. And the ITO target is a main raw material for preparing the ITO film material by magnetron sputtering.
The ITO target film required by TFT-LCD industry needs to have the characteristics of low resistivity, high light transmittance, good uniformity of film layers and the like. The performance of the ITO target material determines the quality of the ITO film
In the existing indium tin oxide target, in the magnetron sputtering coating process, the target is easy to have tumor accumulation, and the large number of the tumor accumulation can generate particles attached to the surface of the glass film to influence the film performance. In the magnetron sputtering coating process, the ITO target is taken out from the vacuum coating machine bin to carry out PM (polishing and removing the accumulated tumor on the target), so that the production can be continued, the product yield is reduced, and the production cost is increased.
Disclosure of Invention
In view of the above, the invention aims to provide a rare earth doped ITO target and a preparation method thereof, so as to solve the problem that the existing indium tin oxide target is easy to generate tumor in the magnetron sputtering coating process.
Based on the above purpose, the invention provides a preparation method of a rare earth doped ITO target, which comprises the following steps:
(1) Ball milling of gallium oxide: adding gallium oxide powder into a ball milling tank filled with zirconium beads with phi 1-2mm, adding pure water for the first time, performing ball milling for 16-24 hours to obtain Y slurry, adding indium oxide powder and tin oxide powder, adding pure water for the second time, and performing ball milling for 24-48 hours to obtain Y-ITO slurry;
(2) And (3) spray granulation: drying and granulating the Y-ITO slurry by using a centrifugal spray granulator to obtain Y-ITO powder;
(3) And (3) pressure forming: filling Y-ITO powder into a mould for molding to obtain a blank;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal-pressure oxygen atmosphere, heating up in a gradient way, preserving heat after reaching the sintering temperature, and cooling after the sintering is finished to obtain a sintered target;
(5) Grinding: and processing the sintered target material into a size required by a customer by using a grinding machine to obtain the rare earth doped ITO target material.
Preferably, the weight ratio of the indium oxide powder, the tin oxide powder and the gallium oxide powder in the step (1) is 80-90:13-9:7-1, wherein the BET of the indium oxide powder is: 5-10m 2 Per g, BET of tin oxide powder: 6-11m 2 Per g, BET of gallium oxide powder: 4-10m 2 /g。
Preferably, in the step 1, the weight of the first pure water is equal to the added amount of the gallium oxide powder, and the weight of the second pure water is equal to the added amount of the indium oxide powder plus the tin oxide powder.
Preferably, the particle diameter D50 of the particles in the Y slurry in the step (1) is less than or equal to 0.25 μm, and the particle diameter D50 of the particles in the Y-ITO slurry is less than or equal to 0.25 μm.
According to the invention, nanometer gallium oxide is uniformly dispersed in indium oxide and tin oxide powder in a pre-grinding mode, the pre-ground gallium oxide particles are fine, the sintering activity is high, and the indium oxide and tin oxide powder is added after the gallium oxide is pre-ground, so that the gallium oxide is uniformly dispersed in the indium oxide and the tin oxide.
Preferably, in the step (2), the air inlet temperature of the centrifugal spray granulator is 200-230 ℃ and the air outlet temperature is 80-110 ℃.
Preferably, the particle size D50=25-50 μm of the Y-ITO powder in the step (2), the bulk density is not less than 1.4g/cm 3 。
Preferably, the step (3) is performed with the following steps: 500-1800mm long by 200-500mm wide, forming pressure: 280-350Mpa.
Preferably, the gradient heating rate in the step (4) is as follows: the temperature rising rate from 650 ℃ to 1100-1300 ℃ is 0.5-0.9 ℃/min, and the temperature rising rate from 1100-1300 ℃ to 1400-1600 ℃ is 0.8-1.2 ℃/min.
The invention calcines the blank by a gradient heating method, wherein the heating rate of 650 ℃ to 1100-1300 ℃ is controlled to be 0.5-0.9 ℃/min, the indium tin gallium oxide target material can be crystallized better by medium-speed heating In the temperature range, the heating rate of 1100-1300 ℃ to 1400-1600 ℃ is controlled to be 0.8-1.2 ℃/min, the Ga3In2O6 phase is formed, and then the air holes In the target material are closed by high-temperature heat preservation, thereby being beneficial to improving the target material density.
Preferably, the sintering temperature in the step (4): the temperature is 1400-1600 ℃ and the heat preservation time is 20-40h, the relative density of the sintered target material is 99.6-99.85%, and the grain size is 3-3.4 mu m.
Furthermore, the invention also provides a rare earth doped ITO target, which is obtained according to the preparation method of the rare earth doped ITO target.
The invention has the beneficial effects that:
the invention adopts domestic gallium oxide powder BET:4-10m 2 The BET of the domestic gallium oxide powder is of a low specific surface, needs to be premilled firstly, has the characteristics of short purchase period and low cost, the BET of the imported gallium oxide is of a high specific surface, can not be premilled firstly, but has the characteristics of long purchase period and high cost, the high-activity nano gallium oxide, the indium oxide and the tin oxide powder are uniformly mixed by adopting a mode of premilled gallium oxide firstly, and sintering is carried out by different temperature sections and different heating rates, so that indium tin gallium oxide fully reacts, and the rare earth doped ITO target with fine grains and high performance is obtained.
Compared with the traditional ITO material, the invention maintains the low resistivity, high transmittance and high hardness of the common ITO film, reduces the incidence rate of target material tumor, reduces the cost of the target material bracket and the baffle, is easy to etch, and has less etching residual sand.
Drawings
FIG. 1 is a scanning electron microscope image of a rare earth doped ITO target section in example 2 of the present invention;
FIG. 2 is a graph showing the grain size of the rare earth doped ITO target in example 2 of the present invention;
FIG. 3 is a diagram showing the elemental distribution of a rare earth doped ITO target in example 2 of the present invention;
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
In the examples of the present invention, the indium oxide powder of the comparative example: 7m 2 Per g, BET of tin oxide powder: 8m 2 Per g, BET of gallium oxide powder: 6m 2 /g。
Example 1
(1) Ball milling of gallium oxide: adding 7g of gallium oxide powder into a ball milling tank filled with phi 1mm zirconium beads, then adding 7g of pure water, and performing ball milling for 16 hours to obtain Y slurry, wherein the particle size D50=0.23 mu m, then adding 80g of indium oxide powder and 13g of tin oxide powder, then adding 93g of pure water, and performing ball milling for 24 hours to obtain Y-ITO slurry, and the particle size D50=0.24 mu m;
(2) And (3) spray granulation: drying and granulating the Y-ITO slurry by using a centrifugal spray granulator, wherein the air inlet temperature is 200 ℃, the air outlet temperature is 80 ℃, and the Y-ITO powder is obtained, D50=25.43 mu m, and the apparent density=1.425 g/cm 3 ；
(3) And (3) pressure forming: filling Y-ITO powder into a die for molding, wherein the molding size is as follows: 500mm long by 200mm wide, forming pressure: 280Mpa to obtain a plain embryo;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1100 ℃ is 0.5 ℃/min, the heating up rate from 1100 ℃ to 1400 ℃ is 0.8 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 20h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: and processing the sintered target material into a size required by a customer by using a grinding machine to obtain the rare earth doped ITO target material.
Example 2
(1) Ball milling of gallium oxide: adding 4g of gallium oxide powder into a ball milling tank filled with phi 1mm zirconium beads, then adding 4g of pure water, and performing ball milling for 20 hours to obtain Y slurry, wherein the particle size D50=0.23 mu m, then adding 85g of indium oxide powder and 11g of tin oxide powder, then adding 96g of pure water, and performing ball milling for 36 hours to obtain Y-ITO slurry, and the particle size D50=0.24 mu m;
(2) And (3) spray granulation: drying and granulating the Y-ITO slurry by using a centrifugal spray granulator, wherein the air inlet temperature is 215 ℃, the air outlet temperature is 95 ℃, and the Y-ITO powder is obtained, d50=37 mu m, and the apparent density=1.59 g/cm 3 ；
(3) And (3) pressure forming: filling Y-ITO powder into a die for molding, wherein the molding size is as follows: length 1100 mm. Width 300mm, forming pressure: 310Mpa to obtain a plain embryo;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 0.7 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 1 ℃/min, keeping the temperature for 30 hours after the green body reaches the sintering temperature, and cooling after the sintering is finished to obtain a sintered target;
(5) Grinding: and processing the sintered target material into a size required by a customer by using a grinding machine to obtain the rare earth doped ITO target material.
Example 3
(1) Ball milling of gallium oxide: adding 1g of gallium oxide powder into a ball milling tank filled with phi 2mm zirconium beads, then adding 1g of pure water, and performing ball milling for 24 hours to obtain Y slurry, wherein the particle size D50=0.21 mu m, then adding 90g of indium oxide powder and 9g of tin oxide powder, then adding 99g of pure water, and performing ball milling for 48 hours to obtain Y-ITO slurry, and the particle size D50=0.23 mu m;
(2) And (3) spray granulation: drying and granulating the Y-ITO slurry by using a centrifugal spray granulator, wherein the air inlet temperature is 230 ℃, the air outlet temperature is 110 ℃, and the Y-ITO powder is obtained, d50=48 mu m, and the apparent density is=1.62 g/cm 3 。；
(3) And (3) pressure forming: filling Y-ITO powder into a die for molding, wherein the molding size is as follows: length 1800mm x width 500mm, forming pressure: 350Mpa to obtain a plain embryo;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1300 ℃ is 0.9 ℃/min, the heating up rate from 1300 ℃ to 1600 ℃ is 1.2 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 40h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: and processing the sintered target material into a size required by a customer by using a grinding machine to obtain the rare earth doped ITO target material.
Comparative example 1
(1) Ball milling of gallium oxide: same as in example 2;
(2) And (3) spray granulation: same as in example 2;
(3) And (3) pressure forming: same as in example 2;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 0.07 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 0.07 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 30h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: as in example 2.
Comparative example 2
(1) Ball milling of gallium oxide: same as in example 2;
(2) And (3) spray granulation: same as in example 2;
(3) And (3) pressure forming: same as in example 2;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 0.07 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 1 ℃/min, keeping the temperature for 30 hours after the green body reaches the sintering temperature, and cooling after the sintering is finished to obtain a sintered target;
(5) Grinding: as in example 2.
Comparative example 3
(1) Ball milling of gallium oxide: same as in example 2;
(2) And (3) spray granulation: same as in example 2;
(3) And (3) pressure forming: same as in example 2;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal pressure oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 1 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 0.07 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 30h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: as in example 2.
Comparative example 4
(1) Ball milling of gallium oxide: same as in example 2;
(2) And (3) spray granulation: same as in example 2;
(3) And (3) pressure forming: same as in example 2;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in an atmospheric oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 1 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 1 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 30h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: as in example 2.
Comparative example 5
(1) Ball milling: adding 80g of indium oxide powder, 13g of tin oxide powder and 93g of pure water into a ball milling tank filled with phi 1mm zirconium beads, and performing ball milling for 24 hours to obtain ITO slurry with the particle size D50=0.24 mu m;
(2) And (3) spray granulation: same as in example 2;
(3) And (3) pressure forming: same as in example 2;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in an atmospheric oxygen atmosphere, heating up the green body in a gradient way, wherein the heating up rate from 650 ℃ to 1200 ℃ is 1 ℃/min, the heating up rate from 1200 ℃ to 1500 ℃ is 1 ℃/min, after the green body reaches the sintering temperature, preserving the heat for 30h, and cooling after the sintering is finished, thus obtaining the sintered target;
(5) Grinding: as in example 2.
The targets prepared in examples 1-3, comparative examples 1-5 were tested for relative density and grain size, and the results are shown in Table 1.
TABLE 1 relative Density and grain size of the targets prepared in examples 1-3, comparative examples 1-5
Data analysis: as can be seen from examples 1-3, the rare earth doped ITO target prepared by the preparation method provided by the invention has uniform and flat surface color, the relative density of the rare earth doped ITO target is 99.6-99.85%, and the grain size is 3-3.4 mu m.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the rare earth doped ITO target is characterized by comprising the following steps of:
(1) Ball milling of gallium oxide: adding gallium oxide powder into a ball milling tank filled with zirconium beads with phi 1-2mm, adding pure water for the first time, performing ball milling for 16-24 hours to obtain Y slurry, adding indium oxide powder and tin oxide powder, adding pure water for the second time, and performing ball milling for 24-48 hours to obtain Y-ITO slurry;
(2) And (3) spray granulation: drying and granulating the Y-ITO slurry by using a centrifugal spray granulator to obtain Y-ITO powder;
(3) And (3) pressure forming: filling Y-ITO powder into a mould for molding to obtain a blank;
(4) High-temperature sintering: placing the green body into a high-temperature sintering furnace in normal-pressure oxygen atmosphere, heating up in a gradient way, preserving heat after reaching the sintering temperature, and cooling after the sintering is finished to obtain a sintered target;
(5) Grinding: and processing the sintered target material into a size required by a customer by using a grinding machine to obtain the rare earth doped ITO target material.
2. The method for preparing a rare earth doped ITO target according to claim 1, wherein the steps are as follows(1) The weight ratio of the indium oxide powder, the tin oxide powder and the gallium oxide powder is 80-90:13-9:7-1, wherein the BET of the indium oxide powder is as follows: 5-10m 2 Per g, BET of tin oxide powder: 6-11m 2 Per g, BET of gallium oxide powder: 4-10m 2 /g。
3. The method for preparing a rare earth doped ITO target according to claim 1, wherein the weight of pure water added in the first step 1 is equal to the added amount of gallium oxide powder, and the weight of pure water added in the second step is equal to the added amount of indium oxide powder plus tin oxide powder.
4. The method for preparing a rare earth doped ITO target according to claim 1, wherein the particle diameter D50 of particles in the Y slurry in the step (1) is less than or equal to 0.25 μm, and the particle diameter D50 of particles in the Y-ITO slurry is less than or equal to 0.25 μm.
5. The method for preparing a rare earth doped ITO target according to claim 1, wherein the inlet air temperature of the centrifugal spray granulator in the step (2) is 200-230 ℃ and the outlet air temperature is 80-110 ℃.
6. The method for producing a rare earth doped ITO target according to claim 1, wherein the particle diameter D50=25 to 50 μm of the Y-ITO powder in the step (2) is not less than 1.4g/cm in bulk density 3 。
7. The method for preparing a rare earth doped ITO target according to claim 1, wherein the step (3) is a step of forming: 500-1800mm long by 200-500mm wide, forming pressure: 280-350Mpa and molding time of 1-3h.
8. The method for preparing a rare earth doped ITO target material according to claim 1, wherein the gradient heating rate in the step (4) is: the temperature rising rate from 650 ℃ to 1100-1300 ℃ is 0.5-0.9 ℃/min, and the temperature rising rate from 1100-1300 ℃ to 1400-1600 ℃ is 0.8-1.2 ℃/min.
9. The method for preparing a rare earth doped ITO target according to claim 1, wherein the sintering temperature in step (4): the temperature is 1400-1600 ℃, the heat preservation time is 20-40h, the relative density of the sintered target material is 99.6-99.85%, and the grain size is 3-3.4 mu m.
10. A rare earth doped ITO target, characterized in that the rare earth doped ITO target is obtained according to the method of manufacturing a rare earth doped ITO target according to claim 1.
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