CN113683408A - Ceramic target material applied to solar cell and preparation method thereof - Google Patents
Ceramic target material applied to solar cell and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic target material applied to a solar cell and a preparation method thereof, wherein the ceramic target material comprises the following steps: s1, adding tin oxide and antimony oxide into a ball mill, adding a dispersing agent and a solvent for primary ball milling, adding a sintering aid, and carrying out secondary ball milling and mixing to obtain slurry; s2, performing spray granulation on the slurry, and sieving to obtain powder; s3, placing the powder in a mould for compression molding to obtain a biscuit; and S4, sintering the biscuit to obtain the ceramic target material applied to the solar cell. The ceramic target material has good density and resistivity, and a film prepared from the ceramic target material has excellent photoelectric property and humidity-resistant and corrosion-resistant properties, and can improve the stability and durability of a solar cell.
Description
Technical Field
The invention relates to the technical field of sputtering targets, in particular to a ceramic target applied to a solar cell and a preparation method thereof.
Background
In recent years, with the rapid development of the photovoltaic industry and the optoelectronic information industry, the development and production scale of conductive films are gradually expanding.
CN103739282A discloses a preparation method of a trace element composite doping modified tin antimony oxide ceramic target material, and specifically discloses that ATO powder with antimony oxide mass percentage of 0.1-1.0% is weighed firstly, and then manganese oxide powder and copper oxide powder are respectively weighed according to 0.5-1.0% of the total mass of the ATO powder as composite doping modifiers; and then ball-milling the powder, the organic solvent and the mixing balls together, wherein the mass ratio of the powder to the organic solvent to the mixing balls is = 1: 1: 1-1: 2: 1, placing the obtained slurry into an oven for low-temperature baking until the organic solvent is completely volatilized, and then grinding and sieving the slurry by using an open sieve to obtain mixed powder; after the mixed powder is subjected to cold isostatic pressing forming in a die, a blank body is sintered in an air atmosphere by adopting a pressureless sintering mode, the heating rate is 0.5-5 ℃/min, the sintering temperature is 1200-1450 ℃, and the heat preservation time is 1-10 hours, so that the modified ATO ceramic target is obtained, manganese oxide and copper oxide are adopted as sintering aids, and the density and the resistivity of the modified ATO ceramic target are still to be improved.
Disclosure of Invention
The invention provides a ceramic target material applied to a solar cell and a preparation method thereof.
The invention adopts the following technical scheme for solving the technical problems:
a preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding tin oxide and antimony oxide into a ball mill, adding a dispersing agent and a solvent for primary ball milling, adding a sintering aid, and carrying out secondary ball milling and mixing to obtain slurry;
s2, performing spray granulation on the slurry, and sieving to obtain powder;
s3, placing the powder in a mould for compression molding to obtain a biscuit;
and S4, sintering the biscuit to obtain the ceramic target material applied to the solar cell.
Preferably, the weight ratio of the tin oxide to the antimony oxide to the dispersant to the solvent to the sintering aid is 10: 0.8-2: 0.05-0.5: 2-5: 0.08 to 2.
Preferably, the weight ratio of the tin oxide to the antimony oxide to the dispersant to the solvent to the sintering aid is 10: 1.8: 0.3: 4: 0.12.
as a preferable scheme, the sintering aid is prepared from titanium dioxide and barium nitrate according to a weight ratio of 1: 0.5 to 2.
As a preferable scheme, the sintering aid is prepared from titanium dioxide and barium nitrate according to a weight ratio of 1: 0.6.
The inventors of the present invention have found that volatilization of tin dioxide can be effectively reduced and generation of pores can be prevented by using a sintering aid comprising titanium dioxide and barium nitrate.
As a preferable scheme, the titanium dioxide is modified titanium dioxide, and the preparation method of the modified titanium dioxide comprises the following steps:
s11, adding 1-4 parts by weight of oxalic acid and 1-4 parts by weight of citric acid into 40-48 parts by weight of deionized water to prepare a mixed acid solution;
s12, adding 10 parts by weight of titanium dioxide into 40-100 parts by weight of mixed acid solution, uniformly dispersing, adding 0.8-2 parts by weight of calcium phosphate and 0.5-1 part by weight of boric acid, stirring at 200-500 rpm for 40-100 min, filtering, and drying to obtain the modified titanium dioxide.
The inventor finds that compared with titanium dioxide, the modified titanium dioxide prepared by the method can improve the performance of the target material, effectively reduce the resistivity, and improve the compactness and the corrosion resistance.
As a preferable scheme, the first ball milling rotating speed is 200-500 rpm, the ball milling time is 4-10 h, the second ball milling rotating speed is 100-400 rpm, and the second ball milling time is 2-6 h.
As a preferable scheme, the spray granulation specifically comprises: adding the slurry into a centrifugal spray dryer for spray granulation; the spray granulation conditions are as follows: the inlet temperature of the hot air is 65-80 ℃, the outlet temperature is 50-65 ℃, and the inlet temperature isThe air volume is 150-250 m3The outlet air volume is 250-350 m3The rotation speed of the centrifugal atomizer is 6000-14000 r/min, and the pumping speed of the slurry is 25-35 ml/min.
Preferably, the compression molding adopts cold isostatic pressing, the pressure of the cold isostatic pressing is 200-400 MPa, and the pressure maintaining time is 4-8 min.
As a preferable scheme, the sintering specifically comprises:
putting the biscuit into a sintering furnace for sintering;
firstly, heating to 250-400 ℃ at a speed of 1-2 ℃/min, and preserving heat for 3-8 h;
heating to 600-800 ℃ at a speed of 0.5-2 ℃/min, and preserving heat for 2-6 h;
then heating to 950-1100 ℃ at a speed of 0.5-2 ℃/min, and preserving heat for 1-4 h;
and finally, raising the temperature to 1250-1350 ℃ at a speed of 0.3-0.9 ℃/min, and preserving the heat for 1-4 h.
As a preferable scheme, the sintering specifically comprises:
putting the biscuit into a sintering furnace for sintering;
firstly, heating to 350 ℃ at the speed of 1.5 ℃/min, and preserving heat for 6 hours;
then heating to 720 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h;
then heating to 1080 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2 h;
finally, the temperature is raised to 1340 ℃ at the speed of 0.5 ℃/min, and the temperature is kept for 2 h.
The inventor of the invention finds that the performance of the target material can be more effectively improved by adopting the sectional sintering compared with one-step sintering, some impurities can be effectively removed, and the density, the resistivity and the corrosion resistance of the film prepared by the target material are improved.
The invention has the beneficial effects that: the ceramic target material has good density and resistivity, and a film prepared from the ceramic target material has excellent photoelectric property and humidity-resistant and corrosion-resistant properties, and can improve the stability and durability of a solar cell.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, the parts are all parts by weight unless otherwise specified.
Example 1
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 1.8 parts by weight of antimony oxide into a ball mill, adding 0.3 part by weight of polyacrylic acid and 4 parts by weight of deionized water, carrying out first ball milling at the rotating speed of 400rpm for 6 hours, adding 0.12 part by weight of sintering aid, carrying out second ball milling and mixing at the rotating speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 75 ℃, the outlet temperature is 58 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the pumping speed of the slurry is 30ml/min, and the slurry is sieved by a 200-mesh sieve to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 300MPa, and the pressure maintaining time is 5min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; firstly, heating to 350 ℃ at the speed of 1.5 ℃/min, and preserving heat for 6 hours; then heating to 720 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h; then heating to 1080 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2 h; and finally, heating to 1340 ℃ at the speed of 0.5 ℃/min, and preserving heat for 2 hours to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from titanium dioxide and barium nitrate according to the weight ratio of 1: 0.6.
In this example, the ceramic target has a relative density of 96.5% and a resistivity of 1.39 × 10-3Ω·cm。
Example 2
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 0.8 part by weight of antimony oxide into a ball mill, adding 0.05 part by weight of polyacrylic acid and 2 parts by weight of deionized water, carrying out first ball milling at the rotating speed of 400rpm for 6 hours, adding 0.08 part by weight of sintering aid, carrying out second ball milling and mixing at the rotating speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 70 ℃, the outlet temperature is 55 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the pumping speed of the slurry is 30ml/min, and the slurry is sieved by a 200-mesh sieve to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 280MPa, and the pressure maintaining time is 6min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; firstly, heating to 380 ℃ at the speed of 1.2 ℃/min, and preserving heat for 5 hours; then heating to 750 ℃ at the speed of 1.2 ℃/min, and preserving heat for 2.5 h; then heating to 1050 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h; and finally, heating to 1300 ℃ at the speed of 0.6 ℃/min, and preserving the heat for 2 hours to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from titanium dioxide and barium nitrate according to the weight ratio of 1: 0.5.
The ceramic target material of this example has a relative density of 94.9% and a resistivity of 1.62 × 10-3Ω·cm。
Example 3
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 2 parts by weight of antimony oxide into a ball mill, adding 0.5 part by weight of polyacrylic acid and 5 parts by weight of deionized water, carrying out first ball milling at the rotating speed of 400rpm for 6 hours, adding 0.2 part by weight of sintering aid, carrying out second ball milling and mixing at the rotating speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 70 ℃, the outlet temperature is 55 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the pumping speed of the slurry is 30ml/min, and the slurry is sieved by a 200-mesh sieve to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 280MPa, and the pressure maintaining time is 6min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; firstly, heating to 300 ℃ at a speed of 1.5 ℃/min, and preserving heat for 5 hours; then heating to 700 ℃ at the speed of 0.8 ℃/min, and preserving heat for 3 h; then heating to 1020 ℃ at the speed of 1.2 ℃/min, and preserving heat for 2 h; and finally, heating to 1280 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2.5 hours to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from titanium dioxide and barium nitrate according to the weight ratio of 1: 2.
In this example, the ceramic target has a relative density of 95.2% and a resistivity of 1.59 × 10-3Ω·cm。
Example 4
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 1.2 parts by weight of antimony oxide into a ball mill, adding 0.2 part by weight of polyacrylic acid and 3.5 parts by weight of deionized water, carrying out first ball milling at the first ball milling rotation speed of 400rpm for 6 hours, adding 0.14 part by weight of sintering aid, carrying out second ball milling and mixing at the second ball milling rotation speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 75 ℃, the outlet temperature is 58 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the slurry pumping speed is 30ml/min and 200 ml/minSieving to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 300MPa, and the pressure maintaining time is 5min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; firstly, heating to 350 ℃ at the speed of 1.5 ℃/min, and preserving heat for 6 hours; then heating to 720 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h; then heating to 1080 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2 h; and finally, heating to 1340 ℃ at the speed of 0.5 ℃/min, and preserving heat for 2 hours to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from titanium dioxide and barium nitrate according to the weight ratio of 1: 1.
The ceramic target material described in this example has a relative density of 95.8% and a resistivity of 1.53 × 10-3Ω·cm。
Example 5
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 1.8 parts by weight of antimony oxide into a ball mill, adding 0.3 part by weight of polyacrylic acid and 4 parts by weight of deionized water, carrying out first ball milling at the rotating speed of 400rpm for 6 hours, adding 0.12 part by weight of sintering aid, carrying out second ball milling and mixing at the rotating speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 75 ℃, the outlet temperature is 58 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the pumping speed of the slurry is 30ml/min, and the slurry is sieved by a 200-mesh sieve to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 300MPa, and the pressure maintaining time is 5min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; firstly, heating to 350 ℃ at the speed of 1.5 ℃/min, and preserving heat for 6 hours; then heating to 720 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h; then heating to 1080 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2 h; and finally, heating to 1340 ℃ at the speed of 0.5 ℃/min, and preserving heat for 2 hours to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from modified titanium dioxide and barium nitrate according to a weight ratio of 1: 0.6.
The preparation method of the modified titanium dioxide comprises the following steps:
s11, adding 2 parts by weight of oxalic acid and 3 parts by weight of citric acid into 45 parts by weight of deionized water to prepare a mixed acid solution;
s12, adding 10 parts by weight of titanium dioxide into 60 parts by weight of mixed acid solution, uniformly dispersing, adding 1.2 parts by weight of calcium phosphate and 0.8 part by weight of boric acid, stirring at the rotating speed of 400rpm for 60min, filtering, and drying to obtain the modified titanium dioxide.
In this example, the ceramic target has a relative density of 99.2% and a resistivity of 0.98 × 10-3Ω·cm。
Comparative example 1
Comparative example 1 differs from example 1 in that the sintering aid described in comparative example 1 was titanium dioxide alone, and the rest was the same.
The ceramic target material of the comparative example has a relative density of 90.8% and a resistivity of 2.46X 10-3Ω·cm。
Comparative example 2
Comparative example 2 differs from example 1 in that the sintering aid of comparative example 2 is barium nitrate alone, and the rest is the same.
The ceramic target material of the comparative example has a relative density of 89.3% and a resistivity of 2.73 × 10-3Ω·cm。
Comparative example 3
Comparative example 3 is different from example 5 in that the modified titania described in comparative example 3 is prepared by a method different from that of example 5, and the other steps are the same.
The preparation method of the modified titanium dioxide comprises the following steps:
s11, adding 2 parts by weight of oxalic acid and 3 parts by weight of citric acid into 45 parts by weight of deionized water to prepare a mixed acid solution;
s12, adding 10 parts by weight of titanium dioxide into 60 parts by weight of mixed acid solution, stirring at the rotating speed of 400rpm for 60min, filtering and drying to obtain the modified titanium dioxide.
The ceramic target material of the comparative example has a relative density of 96.7% and a resistivity of 1.36 × 10-3Ω·cm。
Comparative example 4
Comparative example 4 differs from example 1 in that the sintering method described in comparative example 4 differs from example 1, and the rest is the same.
A preparation method of a ceramic target material applied to a solar cell comprises the following steps:
s1, adding 10 parts by weight of tin oxide and 1.8 parts by weight of antimony oxide into a ball mill, adding 0.3 part by weight of polyacrylic acid and 4 parts by weight of deionized water, carrying out first ball milling at the rotating speed of 400rpm for 6 hours, adding 0.12 part by weight of sintering aid, carrying out second ball milling and mixing at the rotating speed of 200rpm for 5 hours, and thus obtaining slurry;
s2, adding the slurry into a centrifugal spray dryer for spray granulation, wherein the spray granulation conditions are as follows: the inlet temperature of hot air is 75 ℃, the outlet temperature is 58 ℃, and the inlet air quantity is 200m3H, outlet air volume 300m3The rotation speed of the centrifugal atomizer is 8000r/min, the pumping speed of the slurry is 30ml/min, and the slurry is sieved by a 200-mesh sieve to obtain powder;
s3, placing the powder in a mould for cold isostatic pressing, wherein the cold isostatic pressing pressure is 300MPa, and the pressure maintaining time is 5min, so as to obtain a biscuit;
s4, placing the biscuit into a sintering furnace for sintering; sintering at 1340 ℃ and preserving heat for 6h to obtain the ceramic target material applied to the solar cell.
The sintering aid is prepared from titanium dioxide and barium nitrate according to the weight ratio of 1: 0.6.
The ceramic target material of the comparative example has a relative density of 93.2% and a resistivity of 1.71X 10-3Ω·cm。
1. Corrosion resistance test
Placing the ceramic target material in a magnetron sputtering cavity, coating a film on the surface of the PET subjected to corona treatment, wherein the sputtering gas is argon, the sputtering pressure is 0.2Pa, the sputtering power is 1kW, the thickness of the obtained aluminum alloy film is 200nm, and the test results are shown in Table 1.
TABLE 1 test results
As can be seen from Table 1, the film prepared by the ceramic target material of the present invention has good corrosion resistance.
Compared with examples 1 to 4, different preparation parameters can influence the density and the resistivity of the prepared ceramic target material, wherein example 1 is the best preparation parameter, and the corrosion resistance of the film prepared by the method is also the best.
Comparing example 1 with example 5, it is known that the compactness can be remarkably improved and the resistivity can be reduced by modifying titanium dioxide, and the corrosion resistance of the film prepared by the titanium dioxide is further improved.
Compared with the comparative examples 1 and 1-2, the sintering aid composed of titanium dioxide and barium nitrate is selected, so that the compactness can be improved and the resistivity can be reduced compared with a single sintering aid, and the corrosion resistance of the prepared film is better compared with the single sintering aid.
Compared with the comparative example 3, the modified titanium dioxide prepared by different modification methods has different influences on the density and the resistivity of the ceramic target, wherein the modified titanium dioxide prepared by the modification method provided by the invention can obviously improve the density and reduce the resistivity.
Comparing example 1 with comparative example 4, it can be seen that the ceramic target material prepared by the sintering method of the present invention has better compactness and lower resistivity compared with the one-step sintering method.
In light of the foregoing description of preferred embodiments according to the invention, it is clear that many changes and modifications can be made by the person skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A preparation method of a ceramic target material applied to a solar cell is characterized by comprising the following steps:
s1, adding tin oxide and antimony oxide into a ball mill, adding a dispersing agent and a solvent for primary ball milling, adding a sintering aid, and carrying out secondary ball milling and mixing to obtain slurry;
s2, performing spray granulation on the slurry, and sieving to obtain powder;
s3, placing the powder in a mould for compression molding to obtain a biscuit;
and S4, sintering the biscuit to obtain the ceramic target material applied to the solar cell.
2. The method for preparing a ceramic target material for a solar cell according to claim 1, wherein the weight ratio of the tin oxide to the antimony oxide to the dispersant to the solvent to the sintering aid is 10: 0.8-2: 0.05-0.5: 2-5: 0.08 to 2.
3. The method for preparing a ceramic target material for a solar cell according to claim 1, wherein the weight ratio of the tin oxide to the antimony oxide to the dispersant to the solvent to the sintering aid is 10: 1.8: 0.3: 4: 0.12.
4. the method for preparing the ceramic target material for the solar cell according to claim 1, wherein the sintering aid is prepared from titanium dioxide and barium nitrate according to a weight ratio of 1: 0.5 to 2.
5. The method for preparing the ceramic target material for the solar cell according to claim 1, wherein the sintering aid is prepared from titanium dioxide and barium nitrate according to a weight ratio of 1: 0.6.
6. The method for preparing a ceramic target material for a solar cell according to claim 1, wherein the first ball milling rotation speed is 200-500 rpm, the ball milling time is 4-10 hours, the second ball milling rotation speed is 100-400 rpm, and the second ball milling time is 2-6 hours.
7. The method for preparing a ceramic target material for a solar cell according to claim 1, wherein the spray granulation is specifically as follows: adding the slurry into a centrifugal spray dryer for spray granulation; the spray granulation conditions are as follows: the inlet temperature of hot air is 65-80 ℃, the outlet temperature is 50-65 ℃, and the inlet air volume is 150-250 m3The outlet air volume is 250-350 m3The rotation speed of the centrifugal atomizer is 6000-14000 r/min, and the pumping speed of the slurry is 25-35 ml/min.
8. The method for preparing a ceramic target material for a battery according to claim 1, wherein the press forming is performed by cold isostatic pressing, the pressure of the cold isostatic pressing is 200-400 MPa, and the pressure holding time is 4-8 min.
9. The method for preparing a ceramic target material for a battery according to claim 1, wherein the sintering is specifically:
putting the biscuit into a sintering furnace for sintering;
firstly, heating to 250-400 ℃ at a speed of 1-2 ℃/min, and preserving heat for 3-8 h;
heating to 600-800 ℃ at a speed of 0.5-2 ℃/min, and preserving heat for 2-6 h;
then heating to 950-1100 ℃ at a speed of 0.5-2 ℃/min, and preserving heat for 1-4 h;
and finally, raising the temperature to 1250-1350 ℃ at a speed of 0.3-0.9 ℃/min, and preserving the heat for 1-4 h.
10. The method for preparing a ceramic target material for a battery according to claim 1, wherein the sintering is specifically:
putting the biscuit into a sintering furnace for sintering;
firstly, heating to 350 ℃ at the speed of 1.5 ℃/min, and preserving heat for 6 hours;
then heating to 720 ℃ at the speed of 1 ℃/min, and preserving heat for 3 h;
then heating to 1080 ℃ at the speed of 0.8 ℃/min, and preserving heat for 2 h;
finally, the temperature is raised to 1340 ℃ at the speed of 0.5 ℃/min, and the temperature is kept for 2 h.
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CN114524664A (en) * | 2022-02-25 | 2022-05-24 | 洛阳晶联光电材料有限责任公司 | Ceramic target material for solar cell and preparation method thereof |
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CN114188601A (en) * | 2021-12-10 | 2022-03-15 | 云南大学 | Preparation method and application of solid electrolyte |
CN114188601B (en) * | 2021-12-10 | 2023-09-05 | 云南大学 | Preparation method and application of solid electrolyte |
CN114524664A (en) * | 2022-02-25 | 2022-05-24 | 洛阳晶联光电材料有限责任公司 | Ceramic target material for solar cell and preparation method thereof |
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