CN116730710A - High-valence element doped indium tin oxide material and preparation method and application thereof - Google Patents
High-valence element doped indium tin oxide material and preparation method and application thereof Download PDFInfo
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- CN116730710A CN116730710A CN202310075225.2A CN202310075225A CN116730710A CN 116730710 A CN116730710 A CN 116730710A CN 202310075225 A CN202310075225 A CN 202310075225A CN 116730710 A CN116730710 A CN 116730710A
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 19
- 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 19
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 17
- 239000013077 target material Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 5
- 239000011651 chromium Substances 0.000 claims abstract description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims abstract description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 5
- 239000010937 tungsten Substances 0.000 claims abstract description 5
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 16
- 239000010408 film Substances 0.000 description 37
- 239000000843 powder Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 6
- 239000000969 carrier Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000004014 plasticizer Substances 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 235000015895 biscuits Nutrition 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 230000003071 parasitic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021424 microcrystalline silicon Inorganic materials 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229940079864 sodium stannate Drugs 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- 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
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- 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 photovoltaic cells, and provides a high-valence element doped indium tin oxide material, a preparation method and application thereof, wherein the high-valence element doped indium tin oxide target material comprises indium oxide, tin oxide and X oxide in a certain proportion, wherein X is one of molybdenum, tungsten, chromium, tantalum, niobium and vanadium, and the density of the indium tin oxide target material is 7.08-7.11g/m 3 Target resistivity (0.003-0.025). Times.10 ‑2 The high-valence element doped indium tin oxide target material provided by the invention can be used as a target material for a photovoltaic cell, a TCO film is deposited on a substrate, and the light transmittance and the mobility of the TCO film are improved under the condition of keeping lower free carrier concentration by lower doping amount.
Description
Technical Field
The invention relates to the technical field of photovoltaic cells, in particular to an indium tin oxide material doped with high-valence elements, and a preparation method and application thereof.
Background
Transparent conductive oxide (Transparent Conductive Oxide, abbreviated as TCO) films are widely used in the field of thin film batteries due to their excellent light transmittance and conductivity. TCO films are respectively deposited on the upper surface and the lower surface of the heterojunction solar cell (Heterojunction Solar Cell, HJT cell for short) and are used for transmitting light and transmitting current. The TCO film has the characteristics of low resistivity, high light transmittance and low-temperature deposition, and can meet the basic requirements of HJT batteries.
Currently HJT battery industry mainly uses indium tin oxide material (ITO target) to deposit TCO film, and the ITO target is based on In 2 O 3 A dopant of crystalline structure. In is generally considered as 2 O 3 The conduction band of (a) is mainly derived from 5s electrons of In, and the valence band is mainly formed by 2p electrons of O, so that the In can be improved by doping 2 O 3 Is a combination of the electrical properties of the substrate. In (In) 2 O 3 Intrinsic absences (oxygen absences) and Sn in crystal structure 4+ Substitution of In 3+ Both mechanisms together contribute a large number of free electrons. In (In) 2 O 3 In the lattice, in atoms are hexacoordinated, O atoms are tetracoordinated, and the six top corners of the cube are occupied by oxygen atoms, leaving two oxygen deficiency sites when In 2 O 3 After a certain proportion of tin is doped, sn 4+ Occupy In 3+ Bit to generate an electron, sn 4+ For In 3+ The substitution of the electrons generated becomes the main source of carriers. In the existing heterojunction battery structure, the front N electrode is a light receiving surface, and the N-type doped microcrystalline silicon film is matched with a TCO film with high mobility and low free carrier concentration, so that the light transmittance of a long wave band (between 400 and 1200 nm) can be greatly improved. However, since the conventional TCO film has low mobility and high free carrier concentration, it is necessary to develop an indium tin oxide material, which can be deposited as an ITO target to obtain a TCO film having high mobility, low free carrier concentration and high transmittance in a long wavelength band.
Disclosure of Invention
The present invention aims at solving at least the above problemsOne of the technical problems existing in the prior art. Therefore, the invention provides an indium tin oxide material doped with high valence elements, a preparation method and application thereof, and the invention provides an indium tin oxide material with high density (7.08-7.11 g/m) 3 ) Target resistivity (0.003-0.025). Times.10 -2 Omega cm, grain size 5.5-11.5 μm, high mobility, low free carrier concentration, high transmittance in long wavelength band, 30-60cm 2 The light transmittance between 400 and 1200nm can reach 88.00 to 91.00 percent, and the concentration of free carriers (1.80 to 2.15) is multiplied by 10 20 cm -3 。
A first aspect of the present invention provides an elemental high-valence doped indium tin oxide material.
Specifically, the high-valence element doped indium tin oxide material comprises the following components in percentage by mass:
96-99% of indium oxide, 0.5-2% of tin oxide and 0.5-2% of X oxide, wherein X is one of molybdenum, tungsten, chromium, tantalum, niobium and vanadium.
In TCO films, mobility (μ) is mainly affected by scattering between electrons and dopant ions. According to the invention, by adding the oxide of X, wherein X is one of molybdenum, tungsten, chromium, tantalum, niobium and vanadium, doping is performed by using high-valence elements (+5 and +6), the valence difference between doped ions and replaced ions in the oxide is larger, each doped ion can provide more free carriers, enough free carriers can be obtained by using a smaller doping amount, ionized impurities and electrically neutral impurity scattering centers in the film can be effectively reduced, higher carrier mobility can be obtained, the absorption of the film to visible light can be reduced, and the light transmittance can be improved.
Preferably, the composition comprises the following components in percentage by mass:
97-99% of indium oxide, 0.5-1.5% of tin oxide and 0.5-1.5% of X oxide.
Further preferably, the composition comprises the following components in percentage by mass:
97-98% of indium oxide, 0.5-1% of tin oxide and 1-1.5% of X oxide.
More preferably, the composition comprises the following components in percentage by mass:
98% of indium oxide, 0.5% of tin oxide and 1.5% of X oxide.
Preferably, the oxide of X is MoO 3 、WO 3 、CrO 3 、Ta 2 O 5 、Nb 2 O 5 、V 2 O 5 One of them.
Further preferably, the oxide of X is MoO 3 、WO 3 、Nb 2 O 5 One of them.
Preferably, the indium oxide is indium oxide powder.
Preferably, the tin oxide is a tin oxide powder.
Preferably, the hafnium oxide is a hafnium oxide powder.
Preferably, the specific surface area of the indium oxide powder is 6-20m 2 /g。
Preferably, the specific surface area of the tin oxide powder is 10-25m 2 /g。
Preferably, the oxide of X is an oxide powder of X.
Preferably, the indium tin oxide material further comprises a binder and/or a plasticizer.
Preferably, the mass of the binder is 0.4 to 2.5% of the total mass of indium oxide, tin oxide and X oxide.
Preferably, the mass of the plasticizer is 0.1 to 2% of the total mass of indium oxide, tin oxide and X oxide.
Preferably, the binder is polyvinyl alcohol (PVA).
Preferably, the plasticizer is polyethylene glycol (PEG).
Preferably, the density of the high-valence element doped indium tin oxide material is 7.08-7.11g/m 3 . The density was measured using the archimedes drainage method.
The second aspect of the invention provides a preparation method of the high-valence element doped indium tin oxide material.
A preparation method of a high-valence element doped indium tin oxide material comprises the following steps:
mixing the components, forming, degreasing and sintering to obtain the high-valence element doped indium tin oxide material; the sintering temperature is 1550-1750 ℃.
Preferably, the mixing of the components is followed by ball milling.
Preferably, after ball milling, the ball mill further comprises adding a binder and/or a plasticizer, mixing, and then drying.
Preferably, the drying is spray drying.
Preferably, the powder obtained after spray drying has a specific surface area of 5-25m 2 /g。
Preferably, the powder obtained after spray drying has a bulk density of 1.2-1.8g/cm 3 。
Preferably, the shaping is a wet cold isostatic shaping technique (CIP shaping).
Preferably, the molding pressure is 100-200MPa.
Preferably, the sintering is a normal pressure high temperature atmosphere sintering process.
Preferably, the sintering temperature is 1600-1700 ℃, and the sintering time is 168-240h.
Further preferably, the sintering temperature is 1650-1700 ℃, and the sintering time is 200-240h.
More preferably, the sintering temperature is 1650 ℃ and the sintering time is 200h.
Preferably, the sintering atmosphere is an oxygen atmosphere and/or a nitrogen atmosphere.
Preferably, the preparation method of the indium oxide comprises the following steps:
dissolving metal indium with acid solution to generate indium trichloride solution, adding alkaline solution to generate precipitate, curing, filtering, drying to obtain indium hydroxide, and calcining at high temperature to obtain the indium oxide.
Preferably, the acid solution is hydrochloric acid.
Preferably, the alkaline solution is aqueous ammonia.
Preferably, the high-temperature calcination temperature is 600-1000 ℃, and the high-temperature calcination time is 8-12h.
Preferably, the tin oxide is prepared by a chemical precipitation method.
A third aspect of the invention provides the use of an indium tin oxide material.
An indium tin oxide material is applied to the field of photovoltaic cells.
A target for a photovoltaic cell, comprising the indium tin oxide material.
Preferably, the photovoltaic cell is a photovoltaic heterojunction cell.
The raw materials for preparing the transparent conductive oxide film comprise the target material for the photovoltaic cell.
Preferably, the mobility of the transparent conductive oxide film is 30-60cm 2 /(V.s)。
Preferably, the transparent conductive oxide film has a light transmittance of 88.00 to 91.00%.
Preferably, the transparent conductive oxide film has a free carrier concentration of (1.50-2.15). Times.10 20 cm -3 。
A preparation method of a transparent conductive oxide film comprises the following steps:
depositing the target material for the photovoltaic cell on a substrate to obtain a transparent conductive oxide film (TCO film).
Preferably, the deposition is by sputter coating (PVD).
Preferably, the coating power of the sputtering coating is 1.0-10.0kW.
Preferably, the temperature of the sputter coating is 150-200 ℃.
Preferably, the substrate is a glass substrate.
Preferably, the deposited film has a thickness of 70-90mm.
Further preferably, the deposited film has a thickness of 80-85mm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The book is provided withThe high valence element doped indium tin oxide target material provided by the invention comprises oxides of indium oxide, tin oxide and X in a certain proportion, wherein X is one of molybdenum, tungsten, chromium, tantalum, niobium and vanadium, and the density of the indium tin oxide target material provided by the invention is 7.08-7.11g/m 3 Target resistivity (0.003-0.025). Times.10 -2 The omega cm, the grain size is 5.5-11.5 mu m, can be directly applied to the preparation of the TCO film on the front surface of the heterojunction battery;
(2) The method comprises the steps of firstly mixing the components, forming, degreasing, and sintering at 1550-1750 ℃ to obtain the high-valence element doped indium tin oxide material;
(3) The high-valence element doped indium tin oxide material provided by the invention can be used as a target material for a photovoltaic cell, and a TCO film is deposited on a substrate, so that the doping efficiency is greatly improved under the condition of less doping amount, enough free carrier concentration is obtained, the mobility is improved under the condition of keeping the free carrier concentration low, the parasitic absorption of long-band light can be reduced by the low doping amount, the light transmittance is improved, the utilization rate of a heterojunction cell to light is increased, and the mobility of the TCO film reaches 30-60cm 2 The light transmittance reaches 88.00-91.00 percent, and the concentration of free carriers is (1.80-2.15) multiplied by 10 20 cm -3 The target material can be applied to the preparation of a photovoltaic heterojunction battery, and the mobility is obviously improved compared with the conventional ITO target material (the mobility of the conventional ITO target material is generally 15-28 cm) 2 V.s), the lateral electron collecting capability of the TCO film is increased and the contact level of the TCO film with the metal electrode can be improved without decreasing the light transmittance.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Examples 1 to 8 and comparative examples 1 to 4
The components and amounts of the high valence element doped indium tin oxide materials of examples 1-8 are shown in table 1 below.
Comparative examples 1 to 3 differ from example 1 in the components and the amounts thereof, and the preparation method is the same.
Comparative example 4 differs from example 1 in that the sintering temperature was reduced to 1400 ℃ and the sintering time was unchanged.
The components and amounts of comparative examples 1 to 4 are different as shown in Table 1 below.
Table 1 the components of each of the examples and comparative examples and the amounts thereof (unit: mass%)
The preparation method of the high valence element doped indium tin oxide material of the above embodiments 1 to 8 comprises the following steps:
(1) Preparation of indium oxide powder:
dissolving an indium ingot (4N 5) by dilute hydrochloric acid to generate an indium trichloride solution; heating the solution, adding a little excessive ammonia water to form a precipitate, and heating and curing the precipitate together with the mother liquor for 6.5 hours; filtering, washing the precipitate until no chloride ions exist, and drying at room temperature to obtain indium hydroxide; calcining indium hydroxide in air at 1000deg.C for 8 hr to obtain indium oxide powder with specific surface area of 8.8m 2 /g。
(2) Preparing tin oxide powder:
adding sodium carbonate solution into sodium stannate solution, stirring by a stirrer, washing, and drying to obtain nano SnO 2 Powder, measured to a specific surface area value of 15m 2 /g。
(3) Preparation of indium tin oxide powder:
and mixing the prepared indium oxide powder with tin oxide powder, and performing ball milling. Ball milling is carried out by respectively using zirconium beads with the diameter of 0.65mm and zirconium beads with the diameter of 0.30mm, adding a binder (PVA) and a Plasticizer (PEG), wherein the mass of the binder is 1.8 percent of the total mass of the indium tin oxide powder, the mass of the plasticizer is 0.8 percent of the total mass of the indium tin oxide powder, and obtaining the ITO powder after spray drying.
(4) Shaping a blank:
and (3) injecting powder into a die by using a rotary target die, forming under the pressure of 150MPa by using a wet hydraulic press, and performing cold isostatic pressing reinforcement to obtain a target biscuit.
(5) Degreasing and sintering:
degreasing the target biscuit prepared in the step (4), and then sintering at a high temperature in an oxygen atmosphere at a sintering temperature of 1650 ℃ for 200 hours to obtain the compact ITO target. And testing the density of the target material by an Archimedes drainage method, sampling, preparing samples, and measuring the grain size by a metallographic microscope.
Application example 1
Preparing an ITO target: the indium tin oxide materials prepared in the above examples and comparative examples are ITO targets.
Application example 2
Preparation of TCO film: the ITO targets prepared in the above examples and comparative examples were used on the cleaned glass substrate, respectively, and TCO films were prepared by sputter coating deposition at a coating power of 7.5kW and a temperature of 180℃and a deposition film thickness of 80mm, and then the mobility, free carrier concentration, and light transmittance of the films were tested.
Product effect test
1. Binding flaw detection
The ITO targets (rotary targets) prepared in the above examples and comparative examples were respectively indium-coated and bound to titanium tubes, and subjected to ultrasonic flaw detection without dark cracks. And then carrying out subsequent sputtering coating deposition to prepare the TCO film.
2. Indium tin oxide material and performance test result of TCO conductive glass
TABLE 2 results of Performance test of indium tin oxide materials and TCO films prepared in examples and comparative examples
As is clear from Table 2, the ITO targets prepared in examples 1 to 8 of the present invention have densities of 7.08 to 7.11g/m 3 Target resistivity (0.003-0.025). Times.10 -2 Omega cm, grain size 5.5-11.5 μm. The ITO targets prepared in examples 1-8 of the present invention were used to deposit TCO films on glass by sputtering, respectively, to obtain conductive glass (TCO conductive glass) containing TCO films with mobility up to 30-60cm 2 (V.s), the light transmittance between 400 and 1200nm reaches 88.00 to 91.00 percent, and the concentration of free carriers (1.80 to 2.15) is multiplied by 10 20 cm -3 The TCO film prepared by the invention has lower doping amount, and the light transmittance and mobility of the TCO film are improved under the condition of keeping lower free carrier concentration.
Whereas the oxide of comparative example 1, which is not doped with X, results in a decrease in mobility of the TCO film. In comparative example 2, two oxides of X are doped at the same time, pores among grains are more under the same sintering process, and the prepared target material has lower density. Comparative example 3 increased the content of doping element, and the film severely absorbed parasitic long-wave light due to higher doping concentration, resulting in reduced mobility and transmittance, and increased free carrier concentration. Comparative example 4 reduced the sintering temperature, the sintering time was unchanged, and the grain growth was insufficient due to the incomplete penetration of the molded body, resulting in a serious decrease in the density of the target, too low the target density, blurring of the grain boundary, and no PVD coating test was performed.
Claims (10)
1. The indium tin oxide material is characterized by comprising the following components in percentage by mass:
96-99% of indium oxide, 0.5-2% of tin oxide and 0.5-2% of X oxide, wherein X is one of molybdenum, tungsten, chromium, tantalum, niobium and vanadium.
2. The indium tin oxide material of claim 1, comprising the following components in mass percent:
97-99% of indium oxide, 0.5-1.5% of tin oxide and 0.5-1.5% of X oxide.
3. The indium tin oxide material of claim 1, comprising the following components in mass percent:
97-98% of indium oxide, 0.5-1% of tin oxide and 1-1.5% of X oxide.
4. The indium tin oxide material of claim 1, wherein the indium tin oxide material has a density of 7.08-7.11g/m 3 。
5. The method for preparing an indium tin oxide material according to any one of claims 1 to 4, comprising the steps of:
and mixing the components, molding, degreasing and sintering to obtain the indium tin oxide material.
The sintering temperature is 1550-1750 ℃.
6. The method according to claim 5, wherein the sintering temperature is 1600-1700 ℃, and the sintering time is 168-240h.
7. Use of the indium tin oxide material of any one of claims 1 to 4 in the field of photovoltaic cells.
8. A target for a photovoltaic cell, characterized by comprising the indium tin oxide material according to any one of claims 1 to 4.
9. A transparent conductive oxide film, characterized in that a raw material for preparing the transparent conductive oxide film comprises the target for a photovoltaic cell according to claim 8.
10. The method for producing a transparent conductive oxide film according to claim 9, comprising the steps of:
and depositing the target material for the photovoltaic cell on a substrate to obtain the transparent conductive oxide film.
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