CN115893988B - Evaporation target material for solar cell and preparation method thereof - Google Patents
Evaporation target material for solar cell and preparation method thereof Download PDFInfo
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- 230000008020 evaporation Effects 0.000 title claims abstract description 54
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 16
- 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 16
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 10
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 9
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims abstract description 8
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 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 6
- 229910001195 gallium oxide Inorganic materials 0.000 claims abstract description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract 2
- 239000002002 slurry Substances 0.000 claims description 61
- 239000002270 dispersing agent Substances 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 50
- 238000005245 sintering Methods 0.000 claims description 50
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- 238000002156 mixing Methods 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 21
- 238000007740 vapor deposition Methods 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 18
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 229920000058 polyacrylate Polymers 0.000 claims description 15
- 239000012798 spherical particle Substances 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 14
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- 230000008021 deposition Effects 0.000 claims description 9
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- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 7
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- 239000000203 mixture Substances 0.000 abstract description 8
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- 239000010408 film Substances 0.000 description 14
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- 239000004576 sand Substances 0.000 description 11
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- 238000005469 granulation Methods 0.000 description 10
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- 239000000463 material Substances 0.000 description 9
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- 238000003756 stirring Methods 0.000 description 4
- 229910006404 SnO 2 Inorganic materials 0.000 description 3
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- 238000010894 electron beam technology Methods 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- GEIAQOFPUVMAGM-UHFFFAOYSA-N Oxozirconium Chemical compound [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
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- 238000011056 performance test Methods 0.000 description 2
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- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
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- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 firstly Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Compositions Of Oxide Ceramics (AREA)
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Abstract
The invention discloses an evaporation target material for a solar cell and a preparation method thereof, wherein the evaporation target material comprises the following components in percentage by mass: indium oxide (In) 2 O 3 ) 98.5-99.5% and 0.5-1.5% of doped oxide, wherein the doped oxide is 2-4 of cerium oxide, tungsten oxide, molybdenum oxide, holmium oxide, yttrium oxide, zirconium oxide and gallium oxide. According to the evaporation target, unique chemical composition is adopted, doped oxide is introduced into an indium oxide matrix, and the current-carrying electron mobility can be obviously improved while higher current-carrying electron concentration is generated through binary or even multi-element co-doping, so that a film deposited by adopting the evaporation target has high near infrared transmittance and high electron mobility.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to an evaporation target material for a solar cell and a preparation method thereof.
Background
Amorphous silicon/crystalline silicon heterojunction solar cells have been widely studied and developed in recent years in industry due to their excellent photoelectric conversion efficiency. In order to improve the spectral response of the heterojunction solar cell in the infrared wavelength region and further fully utilize solar energy, so that the photoelectric conversion efficiency of the solar cell is further improved, and the development of a Transparent Conductive Oxide (TCO) film with high infrared transmittance is the sense of the problem. However, increasing the infrared transmittance of TCO films requires decreasing the electron concentration of the film, while also increasing the electron mobility of the film to ensure good conductivity.
To increase electron mobility of conventional Indium Tin Oxide (ITO) targets, it is desirable to reduce SnO 2 Content (e.g., 3%, 5%). At this time, electron mobility is slightly improved due to a certain reduction in carrier concentration, but conductivity of the thin film tends to be somewhat lowered. And SnO 2 When the content is low, the ITO target with ultra-high density is difficult to fire, which is extremely unfriendly to the actual magnetron sputtering coating process (the phenomenon of nodulation and poisoning on the surface of the target is extremely easy to occur), thereby influencing the coating quality and continuous production.
Disclosure of Invention
In order to achieve the above object and solve the above problems in the prior art, the present invention prepares a low density vapor deposition target by optimizing the chemical composition of the target, improving the grinding process and innovative sintering process, and the target can be used for preparing a TCO film with high electron mobility and high infrared transmittance, so as to meet the actual demands in the solar cell field.
The invention aims to provide an evaporation target material for a solar cell. The evaporation target material comprises the following components: indium oxide (In) 2 O 3 ) 98.5-99.5wt% of doped oxide 0.5-1.5wt%, the doped oxide being cerium oxide (CeO) 2 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoO) 3 ) Holmium oxide (H)o 2 O 3 ) Yttria (Y) 2 O 3 ) Zirconium oxide (ZrO) 2 ) Gallium oxide (Ga) 2 O 3 ) 2-4 of the above.
The evaporation target material for the solar cell provided by the invention has unique chemical composition, the target material is free from deformation and cracking in the sintering process, the relative density is strictly controlled to be about 60%, and the actual requirement of an evaporation coating process is met. In addition, on the premise of keeping the content of the indium oxide of 98.5-99.5wt%, tungsten oxide, cerium oxide, holmium oxide, gallium oxide and other oxides are introduced into the indium oxide matrix, and the carrier electron mobility can be obviously improved while higher carrier electron concentration is generated through binary or even multi-element co-doping.
The invention also provides a preparation method of the evaporation target material for the solar cell, which comprises the following specific steps: firstly, mixing a main oxide, a doped oxide, a dispersing agent and deionized water according to a certain proportion, performing primary ball milling and mixing, and ending ball milling when D50 of primary ball milling and mixing slurry is less than 0.5 mu m; drying and crushing the primary ball-milling mixed slurry, sieving with a 60-80 mesh sieve, placing in a sintering furnace for primary calcination treatment, and introducing oxygen; then collecting calcined powder for standby;
mixing the calcined powder, the binder, the dispersing agent and the deionized water according to a certain proportion, performing secondary ball milling and mixing, adding the dispersing agent in batches for grinding for more than 4 hours, adding the binder in batches, and continuing to grind for more than 30 minutes to obtain slurry;
step three, preparing solid spherical particles from the slurry obtained in the step two in a granulating mode, and sieving and standing the obtained particles for later use;
filling the particles obtained in the step III into a die, and performing compression molding under the condition of molding pressure of 20-40 MPa to obtain an evaporation target biscuit;
and fifthly, placing the evaporation target biscuit obtained in the step four into a sintering furnace for sintering, and naturally cooling to room temperature after the sintering process is finished, so that the evaporation target can be obtained.
Preferably, in the third stepPreparing solid spherical particles from the slurry obtained in the step II through a granulating mode, and then sieving the solid spherical particles with a 80-mesh sieve to obtain particles for later use, wherein the specific surface area of the particles is controlled to be 5.0-6.0m in the granulating process 2 /g。
Preferably, in the fifth step, the specific sintering step is as follows:
a first temperature interval: the temperature is increased by 1 ℃/min at the room temperature of between 750 ℃ and 10 to 15L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 10-15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled to be 10-15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas to be 10-15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 10-15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃, the air flow is controlled at 10-15L/min, and the procedure is finished and naturally cooled to room temperature, so that the evaporation target material can be prepared.
Preferably, the mixture consists of nitrogen and hydrogen, wherein the hydrogen volume ratio is 3-5%.
Preferably, in the preparation method, the dispersing agent is ammonium polyacrylate in one ball milling process, and the ratio of the mass of the dispersing agent to the total mass of oxides is 0.3-0.9%.
Preferably, in the preparation method, the dispersing agent is ammonium polyacrylate in the secondary ball milling process of the calcined powder, and the ratio of the mass of the dispersing agent to the total mass of the oxides is 0.3-0.9%; the binder is polyvinyl alcohol, and the ratio of the mass of the binder to the total mass of the oxides is 1-3%.
Preferably, in the second step, the dispersant is firstly added in batches for grinding for more than 4 hours, and the binder is added in batches after D50 of the mixed slurry is less than 0.8 mu m.
The invention has the following beneficial effects:
firstly, the evaporation target material adopts unique chemistryThe chemical composition is that doped oxide is introduced into an indium oxide matrix, and binary or even multi-element co-doping can generate higher current-carrying electron concentration and simultaneously the current-carrying electron mobility is obviously improved, and a film deposited by adopting the evaporation target material has high near infrared transmittance and high electron mobility, and the electron mobility is compared with that of a conventional ITO target material (In 2 O 3 /SnO 2 =90/10) is 8 times higher, which is beneficial to improving the photoelectric conversion efficiency of the solar cell.
Secondly, the scheme optimizes the grinding process in the preparation process of the evaporation target, and in the secondary ball milling and dispersing process of the calcined powder, firstly, dispersing agents are added in batches to ensure that the slurry maintains proper viscosity so as to realize high-efficiency grinding of the slurry, and then binders are added in batches to continue ball milling, so that nano-scale particles uniformly dispersed in the slurry are orderly combined so as to improve the viscosity of the slurry. And then the slurry with the viscosity regulated is subjected to conventional granulation to obtain solid spherical particles with high compactness. The particles have good fluidity, in the forming process, the particles are easy to realize close packing, are extruded and crushed under the action of pressure and are completely combined into compact biscuit, and the bonding strength of the target material can be improved in the sintering process.
Thirdly, the scheme innovates the sintering process, adopts the mixed atmosphere of nitrogen and hydrogen in the evaporation target sintering process, and adopts a special variable-temperature sintering temperature system in the high-temperature stage. The nitrogen-hydrogen mixed atmosphere treatment can introduce rich oxygen vacancy defects so as to elongate the sintering dynamics process of the target material and reduce the sintering density, the variable-temperature sintering temperature system can improve the sintering activity of the powder surface so as to improve the sintering density, and the synergistic effect of the two achieves the purposes of controlling the sintering shrinkage of the target material and improving the bonding strength of the evaporation target material. The internal tissue uniformity of the prepared evaporation target is obviously improved by precisely controlling the sintering shrinkage of the target through the mixed atmosphere, the relative density is strictly controlled to be about 60%, and the preparation of the high-strength evaporation target with near net size is easy to realize. The thermal shock resistance of the evaporation target material obtained by the method is obviously improved, the target material cracking, powder falling and splashing caused by electron beam bombardment in the evaporation process are avoided, the uniformity and the compactness of a deposited film are ensured, the actual requirements of an evaporation coating process are met, and the preparation process is simple and is completely suitable for large-scale production.
Drawings
FIG. 1 shows the results of performance tests of examples and comparative examples;
Detailed Description
In order to make the technical means, the creation characteristics, the achievement of the purposes and the beneficial effects of the present invention easy to understand, the present invention is further described below in connection with the specific embodiments.
The embodiment provides an evaporation target material for a solar cell, wherein the evaporation target material comprises the following components in percentage by mass: 98.5 to 99.5% by weight of indium oxide (In 2 O 3 ) And 0.5-1.5wt% of a doped oxide; the doped oxide is cerium oxide (CeO) 2 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoO) 3 ) Holmium oxide (Ho) 2 O 3 ) Yttria (Y) 2 O 3 ) Zirconium oxide (ZrO) 2 ) Gallium oxide (Ga) 2 O 3 ) 2-4 of the above.
The embodiment provides a preparation method of the evaporation target, which comprises the following specific steps: step one, mixing a main oxide, a doped oxide, a dispersing agent and deionized water, and performing ball milling and mixing for one time, wherein the solid phase amount of the slurry is controlled to be 50wt%, and the solid phase amount refers to the mass ratio of solid mass to the total solid-liquid mass, and the solid mass comprises the total mass of calcined powder, a binder and the dispersing agent. Finishing ball milling when the granularity D50 of the mixed slurry is less than 0.5 mu m; drying and crushing the primary ball-milling slurry in a baking oven at 90 ℃, placing the primary ball-milling slurry in a sintering furnace at 1400 ℃ under a 60-80 mesh sieve for primary calcination for 4-6 hours, and introducing oxygen; and collecting the calcined powder for later use.
Mixing the calcined powder, the binder, the dispersing agent and deionized water, performing secondary ball milling mixing, controlling the solid phase amount of the slurry to be 50wt%, optimizing the feeding mode of the dispersing agent and the binder, firstly adding the dispersing agent in batches to enable the slurry to keep proper viscosity so as to achieve efficient grinding of the slurry for more than 4 hours, and continuously sanding for more than 30 minutes after D50 of the mixed slurry is less than 0.8 mu m and adding the binder in batches so as to enable the uniformly dispersed nano-scale particles in the slurry to be orderly combined so as to improve the viscosity of the slurry.
Step three, preparing solid spherical particles with high compactness from the grinding slurry by a conventional granulation method, and then taking particles under a 80-mesh sieve for standby, wherein the specific surface area is controlled to be 5.0-6.0m in the granulation process 2 /g。
And step four, filling the particles into a steel mould, and performing compression molding under the molding pressure of 20-40 MPa to obtain the evaporation target biscuit.
Step five, placing the vapor deposition target biscuit after compression molding in a sintering furnace for sintering, wherein the sintering process is as follows:
a first temperature interval: the temperature is increased by 1 ℃/min at the room temperature of between 750 ℃ and 10 to 15L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 10-15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled to be 10-15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas to be 10-15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 10-15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃, the air flow is controlled at 10-15L/min, and the procedure is finished and naturally cooled to room temperature, so that the evaporation target material can be prepared.
In the fifth step, in the preparation method, the vapor deposition target biscuit after compression molding is placed in a sintering furnace, an air atmosphere is adopted in the low-temperature degreasing stage, a mixed atmosphere is adopted in the sintering stage, the mixed atmosphere consists of mixed gas of nitrogen and hydrogen, and the hydrogen volume ratio is 3-5%; after the temperature is raised to 750 ℃, mixed gas is introduced until the temperature is reduced to 800 ℃.
In the first step, the dispersing agent is ammonium polyacrylate in one ball milling process, but the dispersing agent is not limited to the ammonium polyacrylate, and the adding amount is 0.3-0.9 wt%, and the adding amount refers to the mass ratio of the dispersing agent to the total oxide, and the total oxide comprises the total mass of indium oxide and doped oxide. The dispersant is ammonium polyacrylate in the secondary ball milling process of the calcined powder, but the dispersant is not limited to the dispersant, and the addition amount of the dispersant is 0.3 to 0.9 weight percent, wherein the addition amount refers to the mass ratio of the dispersant to the total oxide, and the total oxide comprises the total mass of indium oxide and doped oxide; the binder is polyvinyl alcohol, but is not limited to such a binder, and the addition amount thereof is 1 to 3wt%, and the addition amount refers to the mass ratio of the binder to the total oxide, which includes the total mass of indium oxide and doped oxide.
Examples 1 to 3
Mixing 9.9Kg of indium oxide powder, 0.05Kg of tungsten oxide powder, 0.05Kg of cerium oxide powder, a dispersing agent (ammonium polyacrylate) and deionized water, performing ball milling and mixing for one time, controlling the solid phase amount of the slurry to be 50wt%, adding the dispersing agent to be 0.6wt% of the mass of the total oxide, and ending ball milling when D50 of the mixed slurry is less than 0.5 mu m (namely, the particle ratio of the particles with the particle size less than 0.5 mu m in the slurry reaches 50 percent); and (3) placing the primary ball-milling slurry in a 90 ℃ oven for drying and crushing, sieving the dried and crushed material with a 80-mesh sieve, placing the material in a sintering furnace for primary calcination at 1400 ℃ for 6 hours, and introducing oxygen. Mixing calcined powder, a binder (polyvinyl alcohol), a dispersing agent (ammonium polyacrylate) and deionized water, performing secondary ball milling and mixing, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.8wt% of the mass of the total oxide, controlling the adding amount of the binding agent to be 2.5% of the mass of the total oxide, optimizing the adding mode of the dispersing agent and the binding agent, firstly adding the dispersing agent in three times at 15min intervals in the process of adding and stirring so as to keep the slurry to be proper in viscosity, then transferring the slurry to a sand mill for 4h efficient grinding, and when D50 of the mixed slurry is less than 0.8 mu m (namely, the proportion of particles with the particle size smaller than 0.8 mu m in the slurry is 50%), then adding the binding agent in five times at 5min intervals, and continuing to sand for 30min (the starting time of sand grinding is the first time of adding the binding agent and starting), so that the uniformly dispersed nano-sized particles in the slurry are orderly combined, thereby improving the slurry viscosity. The grinding slurry is prepared into solid spheres with high compactness by a conventional granulation methodGranulating, sieving with 80 mesh sieve, and granulating with specific surface area of 5.0-6.0m 2 And/g. Filling the particles into a steel die, and performing compression molding under the molding pressure of 20MPa, 30MPa and 40MPa to obtain vapor deposition target blanks (marked as A01, A02 and A03). Placing the vapor deposition target biscuit after compression molding in a sintering furnace for sintering, wherein the sintering atmosphere consists of mixed gas of nitrogen and hydrogen, and the hydrogen accounts for 5 percent by volume, and the sintering process comprises the following steps:
a first temperature interval: the temperature is between room temperature and 750 ℃, the heating rate is 1 ℃/min, and the air flow is controlled at 10L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled at 15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas at 15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃ and the air flow is controlled at 10L/min.
Naturally cooling to room temperature after the procedure is finished, and preparing the vapor deposition target materials (the reference numbers are A11, A12 and A13). Putting the evaporation target with the diameter of 32mm and the height of 40mm into a crucible of an activated plasma deposition (RPD) device, wherein the substrate is corning glass with the thickness of 0.7mm, and argon and oxygen are used as working gases (Ar: O) under vacuum condition 2 =100:30, flow ratio), the working pressure of the evaporation cavity was controlled to 0.353Pa (deposition pressure), the electron gun power supply was started to perform evaporation plating to obtain a thin film, and the electron mobility and near infrared transmittance of the thin film were tested, respectively, and the test results are shown in table 1.
Examples 4 to 6
Mixing 9.9Kg indium oxide powder, 0.05Kg tungsten oxide powder, 0.05Kg holmium oxide powder, dispersant (ammonium polyacrylate) and deionized water, performing ball milling and mixing once, controlling the solid phase amount of the slurry to be 50wt%, adding 0.6wt% of dispersant, and when D50 of the mixed slurry is less than 0.5 mu m (namely slurry)Finishing ball milling when the proportion of particles with the particle diameter smaller than 0.5 mu m in the material reaches 50 percent; and (3) placing the primary ball-milling slurry in a 90 ℃ oven for drying and crushing, sieving the dried and crushed material with a 80-mesh sieve, placing the material in a sintering furnace for primary calcination at 1400 ℃ for 6 hours, and introducing oxygen. Mixing calcined powder, a binder (polyvinyl alcohol), a dispersing agent (ammonium polyacrylate) and deionized water, performing secondary ball milling and mixing, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.8% of the mass of the total oxide, controlling the adding amount of the binding agent to be 2.5% of the mass of the total oxide, optimizing the adding mode of the dispersing agent and the binding agent, firstly adding the dispersing agent in three times at 15min intervals in the process of adding and stirring so that the slurry maintains proper viscosity, then transferring the slurry into a sand mill for 4h efficient grinding, and continuously sanding for 30min (the sanding starting time is the first time) when the uniformly dispersed nano-scale particles in the slurry are combined in order so as to improve the viscosity of the slurry when the D50 of the mixed slurry is less than 0.8 mu m (i.e. the particle ratio of the particle size of less than 0.8 mu m is 50%). Preparing solid spherical particles with high compactness from the grinding slurry by a conventional granulation method, sieving the solid spherical particles with a sieve of 80 meshes for standby, and controlling the specific surface area in the granulation process to be 5.0-6.0m 2 And/g. Filling the particles into a steel die, and performing compression molding under the molding pressure of 20MPa, 30MPa and 40MPa to obtain vapor deposition target blanks (marked as B01, B02 and B03). Placing the vapor deposition target biscuit after compression molding in a sintering furnace for sintering, wherein the sintering atmosphere consists of mixed gas of nitrogen and hydrogen, and the hydrogen accounts for 5 percent by volume, and the sintering process comprises the following steps:
a first temperature interval: the temperature is between room temperature and 750 ℃, the heating rate is 1 ℃/min, and the air flow is controlled at 10L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled at 15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas at 15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃ and the air flow is controlled at 10L/min.
Naturally cooling to room temperature after the procedure is finished, and preparing the vapor deposition target materials (the reference numbers are B11, B12 and B13). Putting the evaporation target with the diameter of 32mm and the height of 40mm into a crucible of an activated plasma deposition (RPD) device, wherein the substrate is corning glass with the thickness of 0.7mm, and argon and oxygen are used as working gases (Ar: O) under vacuum condition 2 =100:30, flow ratio), the working pressure of the evaporation cavity was controlled to 0.353Pa (deposition pressure), the electron gun power supply was started to perform evaporation plating to obtain a thin film, and the electron mobility and near infrared transmittance of the thin film were tested, respectively, and the test results are shown in table 1.
Examples 7 to 9
Mixing 9.85Kg of indium oxide powder, 0.05Kg of tungsten oxide powder, 0.05Kg of cerium oxide powder, 0.05Kg of holmium oxide powder, a dispersing agent (ammonium polyacrylate) and deionized water, performing ball milling and mixing for one time, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.6% of the mass of the total oxide, and finishing ball milling when D50 of the mixed slurry is less than 0.5 mu m (namely, the particle ratio of particles with the particle size smaller than 0.5 mu m in the slurry reaches 50 percent); and (3) placing the primary ball-milling slurry in a 90 ℃ oven for drying and crushing, sieving the dried and crushed material with a 80-mesh sieve, placing the material in a sintering furnace for primary calcination at 1400 ℃ for 6 hours, and introducing oxygen. Mixing calcined powder, a binder (polyvinyl alcohol), a dispersing agent (ammonium polyacrylate) and deionized water, performing secondary ball milling and mixing, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.8% of the mass of the total oxide, and the adding amount of the binding agent to be 2.5% of the mass of the total oxide, optimizing the adding mode of the dispersing agent and the binding agent, firstly adding the dispersing agent in the adding and stirring process for three times at 15min intervals to ensure that the slurry keeps proper viscosity, transferring the slurry to a sand mill for 4h of efficient grinding, and adding the binding agent in five times at 5min intervals when the D50 of the mixed slurry is less than 0.8 mu m (namely, the particle ratio of the particles with the particle size smaller than 0.8 mu m in the slurry is 50 percent)And (3) continuing to sand for 30min (the sand grinding takes place after the binder is added for the first time and the sand grinding is started), so that the uniformly dispersed nano-scale particles in the slurry are orderly combined, and the viscosity of the slurry is improved. Preparing solid spherical particles with high compactness from the grinding slurry by a conventional granulation method, sieving the solid spherical particles with a sieve of 80 meshes for standby, and controlling the specific surface area in the granulation process to be 5.0-6.0m 2 And/g. Filling the particles into a steel die, and performing compression molding under the molding pressure of 20MPa, 30MPa and 40MPa to obtain vapor deposition target blanks (marked as C01, C02 and C03). Placing the vapor deposition target biscuit after compression molding in a sintering furnace for sintering, wherein the sintering atmosphere consists of mixed gas of nitrogen and hydrogen, and the hydrogen accounts for 5 percent by volume, and the sintering process comprises the following steps:
a first temperature interval: the temperature is between room temperature and 750 ℃, the heating rate is 1 ℃/min, and the air flow is controlled at 10L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled at 15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas at 15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃ and the air flow is controlled at 10L/min.
Naturally cooling to room temperature after the procedure is finished, and preparing the vapor deposition target materials (marked as C11, C12 and C13). Putting the evaporation target with the diameter of 32mm and the height of 40mm into a crucible of an activated plasma deposition (RPD) device, wherein the substrate is corning glass with the thickness of 0.7mm, and argon and oxygen are used as working gases (Ar: O) under vacuum condition 2 =100:30, flow ratio), the working pressure of the evaporation cavity was controlled to 0.353Pa (deposition pressure), the electron gun power supply was started to perform evaporation plating to obtain a thin film, and the electron mobility and near infrared transmittance of the thin film were tested, respectively, and the test results are shown in table 1.
Examples 10 to 12
Mixing 9.85Kg of indium oxide powder, 0.05Kg of tungsten oxide powder, 0.05Kg of cerium oxide powder, 0.025Kg of holmium oxide powder, 0.025Kg of gallium oxide powder, a dispersing agent (ammonium polyacrylate) and deionized water, performing ball milling and mixing for one time, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.6% of the mass of the total oxide, and finishing ball milling when D50 of the mixed slurry is less than 0.5 mu m (namely, the particle ratio of the particles with the particle size smaller than 0.5 mu m in the slurry reaches 50 percent); and (3) placing the primary ball-milling slurry in a 90 ℃ oven for drying and crushing, sieving the dried and crushed material with a 80-mesh sieve, placing the material in a sintering furnace for primary calcination at 1400 ℃ for 6 hours, and introducing oxygen. Mixing calcined powder, a binder (polyvinyl alcohol), a dispersing agent (ammonium polyacrylate) and deionized water, performing secondary ball milling and mixing, controlling the solid phase amount of the slurry to be 50wt%, controlling the adding amount of the dispersing agent to be 0.8% of the mass of the total oxide, controlling the adding amount of the binding agent to be 2.5% of the mass of the total oxide, optimizing the adding mode of the dispersing agent and the binding agent, firstly adding the dispersing agent in three times at 15min intervals in the process of adding and stirring so that the slurry maintains proper viscosity, then transferring the slurry into a sand mill for 4h efficient grinding, and when D50 of the mixed slurry is less than 0.8 mu m (namely, the proportion of particles with the particle size smaller than 0.8 mu m in the slurry reaches 50%), then adding the binding agent in five times at 5min intervals, and continuing to sand for 30min (the starting time of adding the binding agent for the first time and starting sand grinding), so that the uniformly dispersed nano-sized particles in the slurry are combined orderly, thereby improving the slurry viscosity. Preparing solid spherical particles with high compactness from the grinding slurry by a conventional granulation method, sieving the solid spherical particles with a sieve of 80 meshes for standby, and controlling the specific surface area in the granulation process to be 5.0-6.0m 2 And/g. Filling the particles into a steel die, and performing compression molding under the molding pressure of 20MPa, 30MPa and 40MPa to obtain vapor deposition target blanks (marked as D01, D02 and D03). Placing the vapor deposition target biscuit after compression molding in a sintering furnace for sintering, wherein the sintering atmosphere consists of mixed gas of nitrogen and hydrogen, and the hydrogen accounts for 5 percent by volume, and the sintering process comprises the following steps:
a first temperature interval: the temperature is between room temperature and 750 ℃, the heating rate is 1 ℃/min, and the air flow is controlled at 10L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled at 15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas at 15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 15L/min;
sixth temperature interval: the temperature reduction rate is 1 ℃/min at 800-100 ℃ and the air flow is controlled at 10L/min.
Naturally cooling to room temperature after the procedure is finished, and preparing the vapor deposition target materials (the reference numerals are D11, D12 and D13). Putting the evaporation target with the diameter of 32mm and the height of 40mm into a crucible of an activated plasma deposition (RPD) device, wherein the substrate is corning glass with the thickness of 0.7mm, and argon and oxygen are used as working gases (Ar: O) under vacuum condition 2 =100:30, flow ratio), the working pressure of the evaporation cavity was controlled to 0.353Pa (deposition pressure), the electron gun power supply was started to perform evaporation plating to obtain a thin film, and the electron mobility and near infrared transmittance of the thin film were tested, respectively, and the test results are shown in table 1.
In the embodiment, the mass percentage of indium oxide in the evaporation target is 98.5-99%, and the prepared film has higher electron mobility and higher near infrared transmittance, thereby being beneficial to improving the photoelectric conversion efficiency of the solar cell.
The invention adopts a Cary5000UV-VIS-NIR spectrophotometer to test the optical characteristics of the sample film in the near infrared region (wavelength is in the range of 700-1100 nm); the electron mobility of the films was tested using a Keithley-4200SCS semiconductor characterization test system.
Comparative example 1
ITO target with outsourcing composition ratio of 90/10 and diameter of 6 inches. Coating in a DC magnetron sputtering system, wherein the substrate is corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (no water vapor or hydrogen is introduced), and the electron mobility of the prepared film is 18.24cm 2 The near infrared transmittance was 80.3%.
Comparative example 2
ITO target with outsourcing composition ratio of 97/3 and diameter of 6 inches. Coating in a DC magnetron sputtering system, wherein the substrate is corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (no water vapor or hydrogen is introduced), and the electron mobility of the prepared film is 26.32cm 2 The near infrared transmittance was 86.5%.
The results of the performance tests for each example and comparative example are shown in Table 1 below:
as can be seen from the above table, the photoelectric properties of the films in each example were significantly improved compared to comparative examples 1 and 2. As can be seen from comparison of the examples, the photoelectric performance of the film and the target composition are closely related; the forming pressure can seriously affect the relative density of the evaporation target after sintering, and further can adversely affect the evaporation process. On the one hand, when the relative density of the vapor deposition target is low, the strength of the target itself is also poor. When the electron beam bombards the target, the target is liable to crack or break due to minute local thermal expansion, and the powder falling phenomenon (A11, B11, C11 and D11 belong to the category). On the other hand, when the relative density is too high, the target material cannot buffer the stress and strain applied by the electron beam bombardment, and further cracks and splash phenomena are generated (A13, B13, C13 and D13 belong to the category). Both of these cause interruption of the coating process, thereby reducing production efficiency. The invention aims to meet the actual requirement of the evaporation coating process, and the relative density of the target material is controlled to be about 60 percent.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalent changes and variations in the above-mentioned embodiments can be made by those skilled in the art without departing from the scope of the present invention.
Claims (5)
1. The preparation method of the evaporation target material for the solar cell is characterized by comprising the following steps of: the evaporation target comprises the following components in percentage by mass: 98.5-99.5% of indium oxide and 0.5-1.5% of doped oxide, wherein the doped oxide is 2-4 of cerium oxide, tungsten oxide, molybdenum oxide, holmium oxide, yttrium oxide, zirconium oxide and gallium oxide;
the preparation method of the evaporation target material comprises the following specific steps:
firstly, mixing a main oxide, a doped oxide, a dispersing agent and deionized water according to a certain proportion, performing primary ball milling and mixing, and ending ball milling when D50 of primary ball milling and mixing slurry is less than 0.5 mu m; drying and crushing the primary ball-milling mixed slurry, sieving with a 60-80 mesh sieve, placing in a sintering furnace for primary calcination treatment, and introducing oxygen; then collecting calcined powder for standby;
mixing the calcined powder, the binder, the dispersing agent and the deionized water according to a certain proportion, performing secondary ball milling and mixing, adding the dispersing agent in batches for grinding for more than 4 hours, adding the binder in batches, and continuing to grind for more than 30 minutes to obtain slurry;
step three, preparing solid spherical particles from the slurry obtained in the step two in a granulating mode, and sieving and standing the obtained particles for later use;
filling the particles obtained in the step III into a die, and performing compression molding under the condition of molding pressure of 30MPa to obtain an evaporation target biscuit;
step five, placing the vapor deposition target biscuit obtained in the step four into a sintering furnace for sintering, and naturally cooling to room temperature after the sintering process is finished, so that a vapor deposition target can be obtained;
in the fifth step, the specific sintering steps are as follows:
a first temperature interval: the temperature is increased by 1 ℃/min at the room temperature of between 750 ℃ and 10 to 15L/min;
a second temperature interval: the temperature is increased at 750-1450 ℃ at a speed of 2 ℃/min, and the flow rate of the mixed gas is controlled at 10-15L/min;
third temperature interval: 1450-1400 ℃, the cooling rate is 2 ℃/min, and the mixed gas flow is controlled to be 10-15L/min;
fourth temperature interval: preserving heat for 6h at 1400 ℃, and controlling the flow rate of the mixed gas to be 10-15L/min;
fifth temperature interval: the temperature reduction rate is 3 ℃/min at 1400-800 ℃, and the mixed gas flow is controlled at 10-15L/min;
sixth temperature interval: cooling at 800-100deg.C at a rate of 1deg.C/min, controlling air flow at 10-15L/min, and naturally cooling to room temperature to obtain vapor deposition target;
the mixed gas consists of nitrogen and hydrogen, wherein the volume ratio of the hydrogen is 3-5%.
2. The method for preparing an evaporation target for a solar cell according to claim 1, wherein the method comprises the steps of: in the third step, the slurry obtained in the second step is prepared into solid spherical particles in a granulating mode, and then the solid spherical particles are sieved by a 80-mesh sieve to be used, wherein the specific surface area of the solid spherical particles is controlled to be 5.0-6.0m in the granulating process 2 /g。
3. The method for preparing the evaporation target for the solar cell according to claim 1, wherein in the preparation method, the dispersing agent is ammonium polyacrylate in one ball milling process, and the ratio of the mass of the dispersing agent to the total mass of oxides is 0.3-0.9%.
4. The preparation method of the evaporation target material for the solar cell according to claim 1, wherein in the preparation method, the dispersing agent is ammonium polyacrylate in the secondary ball milling process of calcined powder, and the ratio of the mass of the dispersing agent to the total mass of oxides is 0.3-0.9%; the binder is polyvinyl alcohol, and the ratio of the mass of the binder to the total mass of oxides is 1-3%.
5. The method for preparing a deposition target for a solar cell according to claim 1, wherein in the second step, the dispersant is added in batches for grinding for more than 4 hours, and the binder is added in batches after the D50 of the mixed slurry is less than 0.8 μm.
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