CN116639956A - High-mobility indium titanium cerium tantalum oxide target and preparation method thereof - Google Patents
High-mobility indium titanium cerium tantalum oxide target and preparation method thereof Download PDFInfo
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- -1 indium titanium cerium tantalum oxide Chemical compound 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 129
- 239000002002 slurry Substances 0.000 claims abstract description 63
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001936 tantalum oxide Inorganic materials 0.000 claims abstract description 26
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 25
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 25
- 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 25
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 24
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000013077 target material Substances 0.000 claims description 37
- 238000001816 cooling Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 238000005086 pumping Methods 0.000 claims description 17
- 238000007873 sieving Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 14
- 230000003179 granulation Effects 0.000 claims description 14
- 239000004576 sand Substances 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims description 2
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 49
- 239000004372 Polyvinyl alcohol Substances 0.000 description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 13
- 239000002202 Polyethylene glycol Substances 0.000 description 12
- 229920001223 polyethylene glycol Polymers 0.000 description 12
- 102220042174 rs141655687 Human genes 0.000 description 10
- 102220043159 rs587780996 Human genes 0.000 description 10
- 235000015895 biscuits Nutrition 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910001460 tantalum ion Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention belongs to the technical field of oxide target preparation, and discloses a high-mobility indium titanium cerium tantalum oxide target and a preparation method thereof. The preparation method comprises the following steps: weighing indium oxide, titanium oxide, cerium oxide and tantalum oxide powder according to the mass ratio of 97.95-98.47:0.23-0.35:0.50-0.75:0.80-1.12; adding the powder into a dispersing agent aqueous solution, stirring, dispersing and grinding to obtain slurry I, and adding a binder for pre-dispersing and grinding to obtain slurry II; granulating the slurry through spraying, mixing and screening to obtain mixed powder; and carrying out heat treatment on the mixed powder after dry pressing and cold isostatic pressing to obtain the high-mobility indium titanium cerium tantalum oxide target. According to the invention, through adjusting each component in the target, the mobility and the conductivity of the target can be obviously improved.
Description
Technical Field
The invention belongs to the technical field of oxide target preparation, and particularly relates to a high-mobility indium titanium cerium tantalum oxide target and a preparation method thereof.
Background
The oxide semiconductor thin film has excellent characteristics of high electron mobility, high light transmittance and low growth temperature, is expected to replace the traditional silicon-based thin film transistor, and becomes a driving device of the next generation of display technology. Solar energy is a clean energy battery, and is widely applied to living and production. The solar cell, in particular, the transparent conductive film (TCO) is added between the electrode of the heterojunction solar cell and the amorphous silicon by doping, so that the collection of carriers can be effectively increased, and the conversion efficiency of the solar cell is improved.
The indium titanium cerium tantalum oxide target film has higher optical transmittance (80% -90%) in the visible light range (380-780 nm), is a film with high mobility and high carrier concentration, and is widely applied to windows of solar cells, photosensitive detectors and other electronic devices. Therefore, the production and the manufacture of the high-performance indium titanium cerium tantalum oxide target material have very important promotion effect on the development of the field.
In our earlier patent application CN 116082045A, a method for preparing indium titanium cerium tantalum oxide powder is disclosed, which comprises the steps of reacting a solution containing indium ions, titanium ions, tantalum ions and cerium ions with an alkaline precipitant, filtering to obtain a precipitate, grinding the precipitate, and calcining to obtain the indium titanium cerium tantalum oxide powder. Carrying out mould pressing and cold isostatic pressing on the indium titanium cerium tantalum oxide powder to obtain a target biscuit; and sintering the target biscuit to obtain the indium titanium cerium tantalum oxide target. The particle size of the indium titanium cerium tantalum oxide precursor is controlled, so that the indium titanium cerium tantalum oxide powder generated after calcination has better particle uniformity. Meanwhile, the concentration of main metal ions is selected, so that the porosity, resistivity and the like of the target material can be effectively controlled. Patent CN 114180938A also discloses a preparation method of indium oxide cerium titanium tantalum powder, which mainly controls the particle size of the indium oxide cerium titanium tantalum powder to be uniform, the particle size distribution is small, the components are uniform, and thus the effects of high density, uniform structure and excellent photoelectric characteristics are achieved. However, the component proportions of the indium titanium cerium tantalum oxide material and the corresponding photoelectric properties, such as mobility, resistivity and the like, still have room for further improvement.
Disclosure of Invention
In order to further improve the performance of the indium titanium cerium tantalum oxide target, the primary aim of the invention is to provide a preparation method of the high-mobility indium titanium cerium tantalum oxide target.
The invention also aims to provide the high-mobility indium titanium cerium tantalum oxide target material prepared by the method.
The invention aims at realizing the following technical scheme:
the preparation method of the high-mobility indium titanium cerium tantalum oxide target material comprises the following preparation steps:
(1) Weighing indium oxide powder, titanium oxide powder, cerium oxide powder and tantalum oxide powder according to the mass ratio of 97.95-98.47:0.23-0.35:0.50-0.75:0.80-1.12;
(2) Adding a dispersing agent into water, stirring and dissolving uniformly, adding the oxide powder weighed in the step (1), stirring for pre-dispersing, pumping the pre-dispersed slurry into a sand mill for grinding by a pump to obtain slurry I;
(3) Adding a binder into the slurry I obtained in the step (2) for pre-dispersing, and grinding by a sand mill to obtain slurry II;
(4) Granulating the slurry obtained in the step (3) through spraying, and then mixing and sieving to obtain indium titanium cerium tantalum oxide mixed powder;
(5) Carrying out heat treatment on the indium titanium cerium tantalum oxide mixed powder obtained in the step (4) after dry pressing and cold isostatic pressing to obtain an indium titanium cerium tantalum oxide target material with high mobility;
the heat treatment process in the step (5) is as follows: degreasing treatment is carried out in air atmosphere at 400-600 ℃, then cooling is carried out to room temperature, oxygen is introduced, and normal pressure sintering treatment is carried out by heating to 1300-1550 ℃ in oxygen atmosphere.
Further, the average grain size of the indium oxide powder, the titanium oxide powder, the cerium oxide powder and the tantalum oxide powder in the step (1) is 40-300 μm, and the purity is not lower than 4N.
Further, the dispersing agent in the step (2) is one of polyvinylpyrrolidone (polyvinyl pyrrolidone, PVP for short), sodium dodecyl benzene sulfonate (sodium dodecyl benzene sulfonate, SDBS for short), a polycarboxylic acid compound, a polyvinyl acid salt or sodium hexadecyl benzene sulfonate; the addition amount of the dispersing agent accounts for 1-5% of the total mass of the oxide powder.
Further, the rotational speed of the pre-dispersion in the step (2) is 100-300 rpm, and the time is 20-60 min.
Further, in the step (2), the grinding rotation speed is 800-1800 r/min, and the grinding time is 6-10 h.
Further, the solid content of the slurry I in the step (2) is 30% -75%; the grain diameter D50 of the slurry I is 0.2-0.6 mu m, and the D90 is 0.2-1.2 mu m.
Further, the binder in the step (3) is a mixture of polyvinyl alcohol (PVA) and polyethylene glycol (PEG), PVA or polyvinyl butyral (PVB); the addition amount of the binder is 5-10% of the total mass of the solids in the second slurry.
Further, the pre-dispersing rotating speed in the step (3) is 50-150 rpm, and the time is 20-40 min.
Further, in the step (3), the grinding rotating speed is 800-1600 r/min, and the grinding time is 2-5 h.
Further, the solid content of the second slurry in the step (3) is 45% -75%; the grain diameter D50 of the slurry II is 0.2-0.5 mu m, and the D90 is 0.2-1.2 mu m.
Further, in the step (4), the spray granulation is performed by adopting a flow type spray drying tower, and in the spray granulation process, the air outlet temperature is 68-75 ℃ and the frequency of an atomizer is 120Hz.
Further, the pressure in the dry pressing in the step (5) is 20-95 Mpa, and the molding time is 60-180 s; the pressure during cold isostatic pressing is 200-500 Mpa, and the molding time is 60-180 s.
Further, the temperature rising rate of the degreasing treatment in the step (5) is 0.1-0.5/min, and the heat preservation time is 1-10 h; the temperature rising rate of the sintering treatment is 0.1-1 ℃/min, and the heat preservation time is 8-12 h.
The high-mobility indium titanium cerium tantalum oxide target is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, through adjusting each component in the target, the mobility and the conductivity of the target can be obviously improved.
(2) Under the preparation process conditions, the obtained indium titanium cerium tantalum oxide target material can reach higher relative density.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
(1) 9808g of indium oxide powder, 28g of titanium oxide powder, 52g of cerium oxide powder and 112g of tantalum oxide powder are weighed, and the average grain size of each oxide powder is 40-300 mu m and the purity is 4N for later use.
(2) Adding 4.94kg of pure water and 0.43kg of polyvinylpyrrolidone (PVP) dispersing agent into the slurry barrel to prepare a mixed solution; then adding the powder weighed in the step (1), and pre-dispersing for 60min at a stirring speed of 100 rpm. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 10h, wherein D50=0.458 μm and D90=0.684 μm to obtain slurry I.
(3) Sequentially adding adhesive PVA and PEG into the slurry I obtained in the step (2), and pre-dispersing for 30min at a stirring speed of 100 rpm. Wherein, the mass of PVA and PEG is 4% of the total mass of slurry solid. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 5h, wherein D50=0.312 μm and D90=0.543 μm to obtain a second slurry.
(4) And (3) pumping the slurry II obtained in the step (3) into a parallel-flow spray drying tower for spray granulation, wherein in the spray granulation process, the air outlet temperature is 72 ℃, and the frequency of an atomizer is 120Hz. And then mixing and sieving the powder by adopting a mixer and a sieving machine. The mixed powder after sieving is the powder of the prepared indium titanium cerium tantalum oxide target material.
(5) Sequentially carrying out dry pressing and cold isostatic pressing on the prepared mixed powder to obtain a biscuit of the target, wherein the pressure of the target during dry pressing is 30Mpa, and the pressure is maintained for 120s; the pressure during cold isostatic pressing is 350Mpa and the pressure is maintained for 120s. And (3) placing the prepared target blank in a muffle furnace, heating to 550 ℃ at a heating rate of 0.5 ℃/min under normal pressure air condition for degreasing treatment for 10 hours, cooling to room temperature at a cooling rate of 1 ℃/min, introducing oxygen, heating to 1420 ℃ at a heating rate of 0.5 ℃/min, performing normal pressure heat preservation sintering treatment for 10 hours in an oxygen atmosphere, and cooling to room temperature at a cooling rate of 1 ℃/min to obtain the indium titanium cerium tantalum oxide target material of the embodiment.
The relative density of the target material obtained in this example was 98.75%, the resistivity was 0.87. Mu. Ω. Cm, and the mobility was 68cm 2 and/(V.s), the conductivity was 1120.68s/cm.
Example 2
(1) 9810g of indium oxide powder, 25g of titanium oxide powder, 57g of cerium oxide powder and 108g of tantalum oxide powder are weighed, and the average grain size of each oxide powder is 40-300 mu m and the purity is 4N for later use.
(2) Adding 4.90kg of pure water and 0.44kg of polyvinylpyrrolidone (PVP) dispersing agent into the slurry barrel to prepare a mixed solution; then adding the powder weighed in the step (1), and pre-dispersing for 40min at a stirring speed of 200 rpm. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 10h, wherein D50=0.328 μm and D90= 0.589 μm to obtain slurry I.
(3) Sequentially adding adhesive PVA and PEG into the slurry I obtained in the step (2), and pre-dispersing for 30min at a stirring speed of 100 rpm. Wherein, the mass of PVA and PEG is 4% of the total mass of slurry solid. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 5h, wherein D50=0.482 mu m and D90=0.523 mu m to obtain a second slurry.
(4) And (3) pumping the slurry II obtained in the step (3) into a parallel-flow spray drying tower for spray granulation, wherein in the spray granulation process, the air outlet temperature is 72 ℃, and the frequency of an atomizer is 120Hz. And then mixing and sieving the powder by adopting a mixer and a sieving machine. The mixed powder after sieving is the powder of the prepared indium titanium cerium tantalum oxide target material.
(5) Sequentially carrying out dry pressing and cold isostatic pressing on the prepared mixed powder to obtain a biscuit of the target, wherein the pressure of the target during dry pressing is 30Mpa, and the pressure is maintained for 120s; the pressure during cold isostatic pressing is 350Mpa and the pressure is maintained for 120s. And (3) placing the prepared target blank in a muffle furnace, heating to 550 ℃ at a heating rate of 0.5 ℃/min under normal pressure air condition for degreasing treatment for 10 hours, cooling to room temperature at a cooling rate of 1 ℃/min, introducing oxygen, heating to 1380 ℃ at the heating rate of 0.5 ℃/min, performing normal pressure heat preservation sintering treatment for 10 hours in an oxygen atmosphere, and cooling to room temperature at the cooling rate of 1 ℃/min to obtain the indium titanium cerium tantalum oxide target material of the embodiment.
The relative density of the target material obtained in this example was 98.88%, the resistivity was 0.93. Mu. Ω. Cm, and the mobility was 70.86cm 2 and/(V.s), the conductivity was 1085s/cm.
Example 3
(1) 9816g of indium oxide powder, 32g of titanium oxide powder, 62g of cerium oxide powder and 90g of tantalum oxide powder are weighed, and the average grain size of each oxide powder is 40-300 mu m and the purity is 4N for later use.
(2) Adding 4.82kg of pure water and 0.42kg of polyvinylpyrrolidone (PVP) dispersing agent into the slurry barrel to prepare a mixed solution; then adding the powder weighed in the step (1), and pre-dispersing for 30min at the stirring speed of 300 rpm. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1800r/min for 10h, wherein D50=0.323 μm and D90=0.615 μm to obtain slurry I.
(3) Sequentially adding adhesive PVA and PEG into the slurry I obtained in the step (2), and pre-dispersing for 30min at a stirring speed of 100 rpm. Wherein, the mass of PVA and PEG is 4% of the total mass of slurry solid. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 5h, wherein D50=0.484 μm and D90=0.546 μm to obtain a second slurry.
(4) And (3) pumping the slurry II obtained in the step (3) into a parallel-flow spray drying tower for spray granulation, wherein in the spray granulation process, the air outlet temperature is 72 ℃, and the frequency of an atomizer is 120Hz. And then mixing and sieving the powder by adopting a mixer and a sieving machine. The mixed powder after sieving is the powder of the prepared indium titanium cerium tantalum oxide target material.
(5) Sequentially carrying out dry pressing and cold isostatic pressing on the prepared mixed powder to obtain a biscuit of the target, wherein the pressure of the target during dry pressing is 30Mpa, and the pressure is maintained for 120s; the pressure during cold isostatic pressing is 350Mpa and the pressure is maintained for 120s. And (3) placing the prepared target blank in a muffle furnace, heating to 550 ℃ at a heating rate of 0.5 ℃/min under normal pressure air condition for degreasing treatment for 10 hours, cooling to room temperature at a cooling rate of 1 ℃/min, introducing oxygen, heating to 1450 ℃ at a heating rate of 0.5 ℃/min, performing normal pressure heat preservation sintering treatment for 10 hours in an oxygen atmosphere, and cooling to room temperature at a cooling rate of 1 ℃/min to obtain the indium titanium cerium tantalum oxide target material of the embodiment.
The relative density of the target material obtained in this example was 99.32%, the resistivity was 0.78. Mu. Ω. Cm, and the mobility was 73.53cm 2 and/(V.s), the conductivity was 1185.53s/cm.
Example 4
(1) 9824g of indium oxide powder and 33g of titanium oxide powder, 74g of cerium oxide powder and 85g of tantalum oxide powder were weighed, and each oxide powder had an average crystal grain size of 40 to 300 μm and a purity of 4N for use.
(2) Adding 4.5kg of pure water and 0.41kg of polyvinylpyrrolidone (PVP) dispersing agent into the slurry barrel to prepare a mixed solution; then adding the powder weighed in the step (1), and pre-dispersing for 60min at a stirring speed of 200 rpm. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 10h, wherein D50=0.323 μm and D90=0.532 μm to obtain slurry I.
(3) Sequentially adding adhesive PVA and PEG into the slurry I obtained in the step (2), and pre-dispersing for 40min at a stirring speed of 50 rpm. Wherein, the mass of PVA and PEG is 4% of the total mass of slurry solid. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1800r/min for 5h, wherein D50=0.492 μm and D90=0.514 μm to obtain a second slurry.
(4) And (3) pumping the slurry II obtained in the step (3) into a parallel-flow spray drying tower for spray granulation, wherein in the spray granulation process, the air outlet temperature is 72 ℃, and the frequency of an atomizer is 120Hz. And then mixing and sieving the powder by adopting a mixer and a sieving machine. The mixed powder after sieving is the powder of the prepared indium titanium cerium tantalum oxide target material.
(5) Sequentially carrying out dry pressing and cold isostatic pressing on the prepared mixed powder to obtain a biscuit of the target, wherein the pressure of the target during dry pressing is 30Mpa, and the pressure is maintained for 120s; the pressure during cold isostatic pressing is 350Mpa and the pressure is maintained for 120s. And (3) placing the prepared target blank in a muffle furnace, heating to 550 ℃ at a heating rate of 0.5 ℃/min under normal pressure air condition for degreasing treatment for 10 hours, cooling to room temperature at a cooling rate of 1 ℃/min, introducing oxygen, heating to 1420 ℃ at a heating rate of 0.5 ℃/min, performing normal pressure heat preservation sintering treatment for 10 hours in an oxygen atmosphere, and cooling to room temperature at a cooling rate of 1 ℃/min to obtain the indium titanium cerium tantalum oxide target material of the embodiment.
The relative density of the target material obtained in this example was 99.15%, the resistivity was 1.03. Mu. Ω. Cm, and the mobility was 67.34cm 2 and/(V.s), the conductivity was 1051.52s/cm.
Example 5
(1) 9795g of indium oxide powder and 30g of titanium oxide powder, 50g of cerium oxide powder and 101g of tantalum oxide powder are weighed, and the average grain size of each oxide powder is 40-300 mu m, and the purity is 4N for later use.
(2) Adding 4.88kg of pure water and 0.42kg of polyvinylpyrrolidone (PVP) dispersing agent into the slurry barrel to prepare a mixed solution; then adding the powder weighed in the step (1), and pre-dispersing for 60min at a stirring speed of 200 rpm. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1500r/min for 10h, wherein D50=0.323 μm and D90=0.548 μm to obtain slurry I.
(3) Sequentially adding adhesive PVA and PEG into the slurry I obtained in the step (2), and pre-dispersing for 20min at a stirring speed of 150 rpm. Wherein, the mass of PVA and PEG is 4% of the total mass of slurry solid. Pumping the pre-dispersed slurry into a sand mill at a grinding speed of 1800r/min for 5h, D50=0.472 μm and D90=0.498 μm to obtain a second slurry.
(4) And (3) pumping the slurry II obtained in the step (3) into a parallel-flow spray drying tower for spray granulation, wherein in the spray granulation process, the air outlet temperature is 72 ℃, and the frequency of an atomizer is 120Hz. And then mixing and sieving the powder by adopting a mixer and a sieving machine. The mixed powder after sieving is the powder of the prepared indium titanium cerium tantalum oxide target material.
(5) Sequentially carrying out dry pressing and cold isostatic pressing on the prepared mixed powder to obtain a biscuit of the target, wherein the pressure of the target during dry pressing is 30Mpa, and the pressure is maintained for 120s; the pressure during cold isostatic pressing is 350Mpa and the pressure is maintained for 120s. And (3) placing the prepared target blank in a muffle furnace, heating to 550 ℃ at a heating rate of 0.5 ℃/min under normal pressure air condition for degreasing treatment for 10 hours, cooling to room temperature at a cooling rate of 1 ℃/min, introducing oxygen, heating to 1350 ℃ at a heating rate of 0.5 ℃/min, and performing normal pressure heat preservation sintering treatment for 10 hours in an oxygen atmosphere, and cooling to room temperature at a cooling rate of 1 ℃/min to obtain the indium titanium cerium tantalum oxide target material of the embodiment.
The relative density of the target material obtained in this example was 99.28%, the resistivity was 1.13. Mu. Ω. Cm, and the mobility was 67.89cm 2 and/(V.s), the conductivity was 1026.44s/cm.
Comparative example 1
This comparative example was identical to example 1 in that the content of each component was adjusted to 9832g of indium oxide powder and 37g of titanium oxide powder, 50g of cerium oxide powder and 81g of tantalum oxide powder.
The target material obtained in this comparative example was examined to have a relative density of 98.68%, a resistivity of 1.45. Mu. Ω. Cm, and a mobility of 52.51cm 2 and/(V.s), the conductivity was 1014.23s/cm.
As can be seen from the comparison of example 1 with comparative example 1, the content of titanium oxide powder exceeding the range of the present invention results in a significant decrease in the mobility and conductivity of the target.
Comparative example 2
In this comparative example, the content of each component was adjusted to 9781g of indium oxide powder, 34g of titanium oxide powder, 75g of cerium oxide powder, and 110g of tantalum oxide powder, and the remainder were the same as in example 1.
The target material obtained in this comparative example was examined to have a relative density of 98.77%, a resistivity of 1.67. Mu. Ω. Cm, and a mobility of 51.3cm 2 and/(V.s), the conductivity was 1007.57s/cm.
As can be seen from the comparison of example 1 and comparative example 2, an indium oxide powder content below the range of the present invention results in a significant decrease in the mobility and conductivity of the target.
Comparative example 3
In this comparative example, the content of each component was adjusted to 9810g of indium oxide powder, 33g of titanium oxide powder, 45g of cerium oxide powder, 112g of tantalum oxide powder, and the remainder were the same as in example 1.
The target material obtained in this comparative example was examined to have a relative density of 98.71%, a resistivity of 1.65. Mu. Ω. Cm, and a mobility of 52.83cm 2 and/(V.s), the conductivity was 1012.36s/cm.
As can be seen from the comparison of example 1 and comparative example 3, a cerium oxide powder content lower than the range of the present invention results in a significant decrease in the mobility and conductivity of the target.
Comparative example 4
In this comparative example, the content of each component was adjusted to 9805g of indium oxide powder, 24g of titanium oxide powder, 51g of cerium oxide powder, 120g of tantalum oxide powder, and the remainder were the same as in example 2.
The target material obtained in this comparative example was examined to have a relative density of 98.89%, a resistivity of 1.76. Mu. Ω. Cm, and a mobility of 54.38cm 2 and/(V.s), the conductivity was 1003.47s/cm.
As can be seen from the comparison of example 2 with comparative example 4, a higher content of tantalum oxide powder than the range of the present invention resulted in a significant decrease in the mobility and conductivity of the target.
Comparative example 5
In this comparative example, the content of each component was adjusted to 9800g of indium oxide powder, 38g of titanium oxide powder, 40g of cerium oxide powder, 112g of tantalum oxide powder, and the remainder were the same as in example 2.
The target material obtained in this comparative example was examined to have a relative density of 98.93%, a resistivity of 1.82. Mu. Ω. Cm, and a mobility of 46.89cm 2 and/(V.s), the conductivity was 998.23s/cm.
As can be seen from the comparison of example 2 and comparative example 5, the content of titanium oxide powder being higher than the range of the present invention and the content of cerium oxide powder being lower than the range of the present invention resulted in a significant decrease in the mobility and conductivity of the target.
Comparative example 6
In this comparative example, the content of each component was adjusted to 9740g of indium oxide powder, 85g of titanium oxide powder, 70g of cerium oxide powder, 105g of tantalum oxide powder, and the remainder were the same as in example 3.
The target material obtained in this comparative example was examined to have a relative density of 98.28%, a resistivity of 1.56. Mu. Ω. Cm, and a mobility of 49.48cm 2 and/(V.s), the conductivity was 1002.62s/cm.
As can be seen from the comparison of example 3 with comparative example 6, the content of indium oxide powder being below the range of the present invention and the content of titanium oxide powder being above the range of the present invention resulted in a significant decrease in the mobility and conductivity of the target.
Comparative example 7
In this comparative example, the content of each component was adjusted to 9781g of indium oxide powder, 34g of titanium oxide powder, 75g of cerium oxide powder, and 110g of tantalum oxide powder, and the remainder were the same as in example 3.
The target material obtained in this comparative example was examined to have a relative density of 99.08%, a resistivity of 1.25. Mu. Ω. Cm, and a mobility of 49.32cm 2 and/(V.s), the conductivity was 1021.33s/cm.
As can be seen from the comparison of example 3 with comparative example 7, an indium oxide powder content below the range of the present invention resulted in a significant decrease in the mobility and conductivity of the target.
Comparative example 8
In this comparative example, the content of each component was adjusted to 9845g of indium oxide powder, 32g of titanium oxide powder, 82g of cerium oxide powder, 41g of tantalum oxide powder, and the remainder were the same as in example 4.
The target material obtained in this comparative example was examined to have a relative density of 98.84%, a resistivity of 1.28. Mu. Ω. Cm, and a mobility of 42.48cm 2 and/(V.s), the conductivity was 1017.66s/cm.
As can be seen from the comparison of example 4 and comparative example 8, the content of cerium oxide powder being higher than the range of the present invention and the content of tantalum oxide powder being lower than the range of the present invention resulted in a significant decrease in the mobility and conductivity of the target.
Comparative example 9
In this comparative example, the content of each component was adjusted to 9750g of indium oxide powder, 50g of titanium oxide powder, 84g of cerium oxide powder, 116g of tantalum oxide powder, and the remainder.
The target material obtained in this comparative example was examined to have a relative density of 98.68%, a resistivity of 1.83. Mu. Ω. Cm, and a mobility of 20.55cm 2 and/(V.s), the conductivity was 968.76s/cm.
As can be seen from the comparison of example 4 and comparative example 9, the content of indium oxide powder was lower than the range of the present invention, while the contents of titanium oxide powder, tantalum oxide powder and tantalum oxide powder were all higher than the range of the present invention, resulting in serious decrease in the mobility and conductivity of the target.
Comparative example 10
In this comparative example, the content of each component was adjusted to 9845g of indium oxide powder, 65g of cerium oxide powder, and 87g of tantalum oxide powder, and the remainder was the same, except that titanium oxide powder was not added, as compared with example 5.
The target material obtained in this comparative example was examined to have a relative density of 98.33%, a resistivity of 1.78. Mu. Ω. Cm, and a mobility of 21.59cm 2 and/(V.s), the conductivity was 926.69s/cm.
As can be seen from the comparison of example 5 and comparative example 10, the addition of no titanium oxide powder resulted in a serious decrease in the mobility and conductivity of the target.
Comparative example 11
In this comparative example, the content of each component was adjusted to 9847g of indium oxide powder, 34.8g of titanium oxide powder, 118.2g of tantalum oxide powder, and the remainder was the same as in example 5.
The target material obtained in this comparative example was examined to have a relative density of 99.24%, a resistivity of 1.84. Mu. Ω. Cm, and a mobility of 20.31cm 2 and/(V.s), the conductivity was 958.45s/cm.
As can be seen from the comparison of example 5 with comparative example 11, the absence of addition of cerium oxide powder and tantalum oxide powder at a content higher than the range of the present invention resulted in a serious decrease in the mobility and conductivity of the target.
Comparative example 12
This comparative example is different from example 5 in that the sintering is performed in conventional air without introducing oxygen. The remainder being identical.
The target material obtained in this comparative example was examined for a relative density of 97.24%, a resistivity of 2.35. Mu. Ω. Cm, a mobility of 31.34cm 2/(V.s), and a conductivity of 918.58s/cm.
As can be seen from the comparison between example 5 and comparative example 12, conventional sintering was employed during sintering, which resulted in a decrease in the relative density of the target, an increase in the resistivity, and a decrease in the mobility without the introduction of oxygen.
The properties of the targets obtained in the above examples and comparative examples are shown in Table 1 below.
TABLE 1
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-mobility indium titanium cerium tantalum oxide target material is characterized by comprising the following preparation steps:
(1) Weighing indium oxide powder, titanium oxide powder, cerium oxide powder and tantalum oxide powder according to the mass ratio of 97.95-98.47:0.23-0.35:0.50-0.75:0.80-1.12;
(2) Adding a dispersing agent into water, stirring and dissolving uniformly, adding the oxide powder weighed in the step (1), stirring for pre-dispersing, pumping the pre-dispersed slurry into a sand mill for grinding by a pump to obtain slurry I;
(3) Adding a binder into the slurry I obtained in the step (2) for pre-dispersing, and grinding by a sand mill to obtain slurry II;
(4) Granulating the slurry obtained in the step (3) through spraying, and then mixing and sieving to obtain indium titanium cerium tantalum oxide mixed powder;
(5) Carrying out heat treatment on the indium titanium cerium tantalum oxide mixed powder obtained in the step (4) after dry pressing and cold isostatic pressing to obtain an indium titanium cerium tantalum oxide target material with high mobility;
the heat treatment process in the step (5) is as follows: degreasing treatment is carried out in air atmosphere at 400-600 ℃, then cooling is carried out to room temperature, oxygen is introduced, and normal pressure sintering treatment is carried out by heating to 1300-1550 ℃ in oxygen atmosphere.
2. The method for producing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the average grain size of the indium oxide powder, the titanium oxide powder, the cerium oxide powder and the tantalum oxide powder in step (1) is 40 to 300 μm and the purity is not lower than 4N.
3. The method for preparing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the dispersant in the step (2) is one of PVP, SDBS, a polycarboxylic acid compound, a polyvinyl acid salt or sodium hexadecyl benzenesulfonate; the addition amount of the dispersing agent accounts for 1-5% of the total mass of the oxide powder; the rotational speed of the pre-dispersion is 100-300 rpm, and the time is 20-60 min; the grinding rotating speed is 800-1800 r/min, and the grinding time is 6-10 h.
4. The method for preparing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the solid content of the slurry I in the step (2) is 30% -75%; the grain diameter D50 of the slurry I is 0.2-0.6 mu m, and the D90 is 0.2-1.2 mu m.
5. The method for preparing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the binder in the step (3) is a mixture of PVA and PEG, PVA or PVB; the addition amount of the adhesive is 5-10% of the total mass of the solids in the second slurry; the rotation speed of the pre-dispersion is 50-150 rpm, and the time is 20-40 min; the grinding rotating speed is 800-1600 r/min, and the grinding time is 2-5 h.
6. The method for preparing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the solid content of the second slurry in the step (3) is 45-75%; the grain diameter D50 of the slurry II is 0.2-0.5 mu m, and the D90 is 0.2-1.2 mu m.
7. The method for preparing the high-mobility indium titanium cerium tantalum oxide target material according to claim 1, wherein in the step (4), spray granulation is carried out by a flow type spray drying tower, the air outlet temperature is 68-75 ℃ in the spray granulation process, and the frequency of an atomizer is 120Hz.
8. The method for preparing a high mobility indium titanium cerium tantalum oxide target according to claim 1, wherein the dry pressing pressure in the step (5) is 20-95 Mpa, and the molding time is 60-180 s; the pressure during cold isostatic pressing is 200-500 Mpa, and the molding time is 60-180 s.
9. The method for preparing the high-mobility indium titanium cerium tantalum oxide target material according to claim 1, wherein the temperature rise rate of the degreasing treatment in the step (5) is 0.1-0.5/min, and the heat preservation time is 1-10 h; the temperature rising rate of the sintering treatment is 0.1-1 ℃/min, and the heat preservation time is 8-12 h.
10. A high mobility indium titanium cerium tantalum oxide target prepared by the method of any one of claims 1 to 9.
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