CN114283961A - High-temperature resistance slurry and preparation method and application thereof - Google Patents
High-temperature resistance slurry and preparation method and application thereof Download PDFInfo
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- CN114283961A CN114283961A CN202111652454.3A CN202111652454A CN114283961A CN 114283961 A CN114283961 A CN 114283961A CN 202111652454 A CN202111652454 A CN 202111652454A CN 114283961 A CN114283961 A CN 114283961A
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- 238000002360 preparation method Methods 0.000 title claims description 15
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- 238000002156 mixing Methods 0.000 claims abstract description 22
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- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000000969 carrier Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 239000001856 Ethyl cellulose Substances 0.000 claims description 10
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 10
- 229920001249 ethyl cellulose Polymers 0.000 claims description 10
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 10
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 7
- PACGUUNWTMTWCF-UHFFFAOYSA-N [Sr].[La] Chemical compound [Sr].[La] PACGUUNWTMTWCF-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
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- 239000011812 mixed powder Substances 0.000 claims description 5
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- 239000011248 coating agent Substances 0.000 claims description 4
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- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- IGPAMRAHTMKVDN-UHFFFAOYSA-N strontium dioxido(dioxo)manganese lanthanum(3+) Chemical group [Sr+2].[La+3].[O-][Mn]([O-])(=O)=O IGPAMRAHTMKVDN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to the technical field of resistance paste, and particularly discloses high-temperature resistance paste which comprises the following components in percentage by mass: resistance control slurry A1-95%, resistance control slurry B1-90% and glass slurry 1-15%; the resistance regulation and control slurry A comprises the following components in percentage by massThe resistance regulation and control slurry B is composed of 60-85% of conductive ceramic powder and 15-40% of organic carriers, and the resistance regulation and control slurry B is composed of the following raw materials in parts by mass: 60-78.5% of noble metal conductive phase and Bi2O31.5-10% of ZnO glass binder phase and 15-30% of organic carrier, wherein the glass slurry consists of 70-85% of glass phase and 15-30% of organic carrier by mass fraction. The high-temperature resistance paste has a wide range of resistance value regulation and control, and the resistance value is directly regulated by mixing three kinds of pastes in different proportions, so that the operation is simple and convenient; the prepared high-temperature resistor has excellent high-temperature resistance, stable electrical property in a high-temperature environment, strong thermal shock resistance, no crack and no falling off in high-temperature thermal cycle, and can meet the requirements of high-temperature resistors with different resistance values.
Description
Technical Field
The invention belongs to the technical field of resistance paste, and particularly relates to high-temperature resistance paste as well as a preparation method and application thereof.
Background
The integrated circuit is an important crystal for the development of modern electronic technology in the 21 st century, and the thick film hybrid integrated circuit is an important component of the integrated circuit. Electronic paste is rapidly developed as a base material for manufacturing thick film hybrid integrated circuits, and is widely applied to the fields of electronics, aerospace and the like. Thick film resistor paste is an important kind of electronic paste, and is mainly divided into metal and nonmetal according to the functional phase components of the thick film resistor paste: the non-metal functional phase mainly comprises graphite and carbon black, the binding phase mainly comprises organic resin, and a film layer prepared by the sizing agent is easy to oxidize in a high-temperature environment, and the use temperature is generally not more than 200 ℃; the metal functional phase is mainly Ag, Pd, ruthenium, etc., Ag is the most conductive metal material, but Ag is the most conductive+The thick film element has mobility, and the resistance is unstable in the using process, so that the service life of the thick film element is greatly reduced; the Pd-Ag resistance paste prepared by doping Pd in the Ag resistance paste can effectively inhibit Ag+The Pd-Ag resistance paste has high process sensitivity, small sheet resistance coverage and poor process reproducibility; the ruthenium system mainly comprises ruthenium dioxide and ruthenate, and has the advantages of good process adaptability, high resistance stability and the like, but the ruthenium system thick film can generate complex reaction when used at the temperature of more than 900 ℃, and the high-temperature resistance stability is poor. The resistance paste is difficult to meet the application requirement in the aspect of high temperature due to the defects of the performance of the resistance paste. Therefore, it is highly desirable to develop a novel high temperature resistance paste with stable resistance.
In addition, the thick film resistor paste is used as a raw material of a thick film resistor, and is required to have a wider resistance range so as to meet the requirements of thick film resistors with different resistances. At present, the resistance value of a thick film resistor is mainly regulated and controlled by regulating and controlling the proportion of a conductive phase and a glass phase in resistor paste, the resistance value is fixed after the formula of the method is fixed, if a thick film resistor with a wide resistance value range is to be prepared, the formula of the paste needs to be readjusted, and the seriated resistor paste is prepared through complicated processes of raw material preparation, material mixing, grinding, detection and the like, so that the method is long in time consumption, high in cost and inconvenient to store and use.
Disclosure of Invention
The invention aims to provide high-temperature resistance paste with adjustable resistance and a preparation method thereof, which overcome the defects in the background art.
In order to achieve the purpose, the invention provides high-temperature resistance paste which comprises the following components in percentage by mass: resistance control slurry A1-95%, resistance control slurry B1-90% and glass slurry 1-15%; the resistance regulation and control slurry A is composed of 60-85% of conductive ceramic powder and 15-40% of organic carriers in mass fraction, and the resistance regulation and control slurry B is composed of the following raw materials in mass fraction: 60-78.5% of noble metal conductive phase and Bi2O31.5-10% of ZnO glass binder phase and 15-30% of organic carrier, wherein the glass slurry consists of 70-85% of glass phase and 15-30% of organic carrier by mass fraction.
Preferably, in the high-temperature resistance paste, the conductive ceramic powder is lanthanum strontium manganate, lanthanum strontium cobaltate or lanthanum strontium ferrite, and the particle size of the conductive ceramic powder is 0.3-2 μm.
Preferably, in the high-temperature resistance paste, the noble metal is Pt or Pd.
Preferably, in the high-temperature resistance paste, Bi is contained2O3Bi in the-ZnO glass binder phase2O3The mass fraction of (A) is 90-95%.
Preferably, in the high-temperature resistance paste, the glass phase in the glass paste comprises the following raw materials in percentage by mass: al (Al)2O35~10%、SiO240-50% of CaO, 1-10% of CaO, 30-40% of BaO and TiO2 1~5%。
Preferably, in the high-temperature resistance paste, the organic vehicle comprises the following components in percentage by mass: 75-85% of butyl carbitol, 5-15% of tributyl citrate, 1-5% of ethyl cellulose, 851-5% of Span-and 1-10% of 1, 4-butyrolactone.
The preparation method of the high-temperature resistance paste comprises the following steps:
(1) preparing an organic carrier;
(2) preparing resistance regulation slurry A: mixing and grinding conductive ceramic powder and an organic carrier according to a proportion to obtain resistance regulation and control slurry A;
(3) preparing resistance regulation slurry B: firstly Bi is added2O3And ZnO powder are subjected to high-temperature smelting, quenching and ball milling to obtain Bi2O3-ZnO glass frit of Bi2O3-ZnO glass powder and noble metal powder are mixed to prepare mixed powder, the mixed powder and an organic carrier are uniformly mixed and ground, and resistance regulation and control slurry B is obtained;
(4) preparing glass slurry: firstly, carrying out high-temperature smelting, quenching and ball milling on glass-phase raw material powder to obtain glass-phase powder, and mixing and grinding the glass-phase powder and an organic carrier to obtain glass slurry;
(5) and mixing the resistance regulation slurry A, the resistance regulation slurry B and the glass slurry to obtain the high-temperature resistance slurry.
Preferably, in the preparation method of the high-temperature resistance paste, in the step (1), butyl carbitol and tributyl citrate are weighed according to a proportion, stirred and mixed, then ethyl cellulose is added, and the mixture is heated to 90-100 ℃ and stirred for 1-2 hours under a heat preservation condition to completely dissolve the ethyl cellulose; adding Span-85 and 1, 4-butyrolactone, and continuously stirring for 2-3 h at 90-100 ℃ to obtain a clear and transparent uniform solution, namely the organic carrier.
Preferentially, in the preparation method of the high-temperature resistance paste, in the step (3), the high-temperature smelting is carried out at the temperature of 1300-1400 ℃ for 2-4 h; bi2O3The ZnO glass powder and the noble metal powder are mixed in a planetary gravity mixer in the mixing process, the revolution speed of the planetary gravity mixer is 1200-1500 rpm, the rotation speed is 30-60% of the revolution speed, and the mixing time is 30-60 min; the mixing process of the mixed powder of the glass powder and the conductive phase and the organic carrier is carried out in a three-roller grinding machine, the rotating speed of the three-roller grinding machine is 250-450 r/min, and the grinding and mixing time is 1-2 h.
Preferentially, in the preparation method of the high-temperature resistance paste, in the step (5), the three components of the resistance regulation and control paste A, the resistance regulation and control paste B and the glass paste are ground in a three-roll grinder, and the rotating speed of the three-roll grinder is 250-450 r/min; and grinding and mixing time is 10-20 min.
The application of the high-temperature resistance paste in preparing the resistance film layer is to print the high-temperature resistance paste on the surface of a base material by a screen printing process, dry the high-temperature resistance paste in air and sinter the high-temperature resistance paste to obtain the resistance film layer.
Preferably, in the application of the high-temperature resistance paste in preparing the resistance film layer, the substrate is an alumina ceramic plate, a zirconia ceramic plate, an alumina coating or a zirconia coating; the drying process comprises the following steps: drying at 150-200 ℃ for 15-30 min, wherein the sintering process comprises the following steps: keeping the temperature of 1100-1200 ℃ for 1-2 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the high-temperature resistance paste can be directly mixed according to different proportions of three pastes to adjust the resistance value, the operation is simple and convenient, and the resistance value adjusting range is wide; the prepared resistor has excellent high temperature resistance, can resist over 1100 ℃, and has stable electrical property in a high-temperature environment; the high-temperature resistor has strong thermal shock resistance, does not have cracks and does not fall off in high-temperature thermal cycle, and can meet the requirements of high-temperature resistors with different resistance values.
2. The high-temperature resistance slurry can be applied to various base materials of aluminum oxide and zirconium oxide, and the prepared resistor has good adhesive force with the base materials, is not easy to fall off, and has a wide application range.
Drawings
Fig. 1 is a photograph of the resistor paste prepared in example 1 of the present invention.
Fig. 2 is a photograph of the resistive film layer prepared in example 1 of the present invention.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Example 1
The high-temperature resistance paste comprises the following components in percentage by mass: resistance control paste A67.57%, resistance control paste B28.57% and glass paste 3.86%.
The resistance regulation and control slurry A consists of 75% of strontium lanthanum cobaltate powder and 25% of organic carrier by mass, and the grain size of the strontium lanthanum cobaltate powder is 1-2 mu m.
The resistance regulation and control slurry B consists of the following raw materials in percentage by mass: 78.4% of Pd conductive phase and Bi2O35% of ZnO glass binder phase and 16.6% of organic carrier, Bi2O3Bi in-ZnO glass bonding phase raw material2O3The mass fraction of (A) is 92% and the mass fraction of ZnO is 8%.
The glass slurry consists of a glass phase with the mass fraction of 80% and an organic carrier with the mass fraction of 20%, wherein the glass phase consists of the following raw materials in mass fraction: al (Al)2O3 7.65%、SiO246.6 percent, CaO 5.25 percent, BaO38.32 percent and TiO2 2.18%。
The organic carrier consists of the following components in percentage by mass: 79.2 percent of butyl carbitol, 10 percent of tributyl citrate, 2.8 percent of ethyl cellulose, Span-853 percent and 5 percent of 1, 4-butyrolactone.
A preparation method of high-temperature resistance paste comprises the following steps:
(1) preparing an organic carrier: weighing butyl carbitol and tributyl citrate according to the proportion, putting the butyl carbitol and the tributyl citrate into a beaker, slowly adding ethyl cellulose, heating and stirring in a water bath at 90 ℃ for 2 hours to completely dissolve the ethyl cellulose; adding Span-85 and 1, 4-butyrolactone after the solution is transparent, and continuously heating and stirring in a water bath at 90 ℃ for 2 hours to obtain a clear and transparent uniform solution, namely the organic carrier;
(2) preparing resistance regulation slurry A: mixing and grinding strontium lanthanum cobaltite powder and an organic carrier according to a proportion to obtain resistance regulation slurry A;
(3) preparing resistance regulation slurry B: glass raw material Bi2O3Uniformly mixing with ZnO powder, smelting at 1400 ℃ for 2h to obtain glass melt, then pouring the obtained glass melt into deionized water for quenching to obtain glass slag, ball-milling the glass slag into glass powder, uniformly mixing with Pd powder in a planetary gravity mixer at the revolution speed of 1300rpm and the rotation speed of the planetary gravity mixerThe rotating speed is 40 percent of the revolution speed, and the stirring time is 30 min; finally, uniformly mixing the mixture with an organic carrier and grinding the mixture in a three-roller grinding machine, wherein the rotating speed of the three-roller grinding machine is 450r/min, and the grinding and mixing time is 1h, so that resistance regulation and control slurry B is obtained;
(4) preparing glass slurry: uniformly mixing glass phase raw material powder, smelting at 1400 ℃ for 3h to obtain a glass melt, then pouring the obtained glass melt into deionized water for quenching to obtain glass slag, ball-milling the glass slag into glass phase powder, and mixing and grinding the glass phase powder and an organic carrier to obtain glass slurry;
(5) mixing the resistance regulation slurry A, the resistance regulation slurry B and the glass slurry according to the proportion, grinding in a three-roll grinder at the rotating speed of 450r/min for 10min to obtain the high-temperature resistance slurry, wherein the rotating speed is 450r/min, and the mixing time is 10min, and the high-temperature resistance slurry is shown in figure 1.
The high-temperature resistance paste prepared in the embodiment is printed on an alumina ceramic chip by adopting a screen printing process, a 250-mesh screen is adopted for printing, drying is carried out for 30min at 150 ℃ in the air, and heat preservation is carried out for 2h at 1200 ℃ to complete sintering, so as to obtain the resistance film layer.
The prepared resistance film layer is shown in figure 2, the sheet resistance of the resistance film layer is 83.3 omega/□, the sheet resistance of the resistance film layer after being processed at 900 ℃ for 100h is 95 omega/□, and the resistance film layer is complete and does not crack or fall off. After being treated at 1100 ℃ for 10h, the sheet resistance is 103 omega/□, and the resistance film layer has no cracking and falling-off phenomenon.
Example 2
The high-temperature resistance paste comprises the following components in percentage by mass: 93.2 percent of resistance regulating and controlling slurry A, 1.5 percent of resistance regulating and controlling slurry B and 5.3 percent of glass slurry.
The resistance regulation and control slurry A consists of 70% of lanthanum strontium manganate powder and 30% of organic carriers by mass fraction, wherein the particle size of the lanthanum strontium manganate powder is 1-2 mu m.
The resistance regulation and control slurry B consists of the following raw materials in percentage by mass: 70% of Pt conductive phase and Bi2O39% of ZnO glass binder phase and 21% of organic carrier, Bi2O3Bi in-ZnO glass bonding phase raw material2O3Is 95% by mass, ZnOThe content was 5%.
The glass slurry consists of a glass phase with the mass fraction of 80% and an organic carrier with the mass fraction of 20%, wherein the glass phase consists of the following raw materials in mass fraction: al (Al)2O38%、SiO245 percent of CaO, 4.8 percent of BaO and 40 percent of TiO2 2.2%。
The organic carrier consists of the following components in percentage by mass: 79.2 percent of butyl carbitol, 10 percent of tributyl citrate, 2.8 percent of ethyl cellulose, Span-853 percent and 5 percent of 1, 4-butyrolactone.
The high temperature resistance paste was prepared in the same manner as in example 1.
The high-temperature resistance paste prepared in the embodiment is printed on a zirconia ceramic chip by adopting a screen printing process, a 250-mesh screen is adopted for printing, drying is carried out at 150 ℃ for 30min in the air, and heat preservation is carried out at 1200 ℃ for 2h to complete sintering, so as to obtain a resistance film layer. The resistance value of the resistance film layer is 3500 omega/□, and the square resistance is 4100 omega/□ after the resistance film layer is processed at 1100 ℃ for 10 hours.
Example 3
The high-temperature resistance paste comprises the following components in percentage by mass: resistance control paste A85%, resistance control paste B6.7% and glass paste 8.3%. The resistance adjusting paste a, the resistance adjusting paste B, and the glass paste were the same as in example 2. The preparation method is the same as example 2.
Example 4
The high-temperature resistance paste comprises the following components in percentage by mass: 65.7% of resistance regulating and controlling slurry A, 29.5% of resistance regulating and controlling slurry B and 4.8% of glass slurry. The resistance adjusting paste a, the resistance adjusting paste B, and the glass paste were the same as in example 2. The preparation method is the same as example 2.
Example 5
The high-temperature resistance paste comprises the following components in percentage by mass: 65.7% of resistance regulating and controlling slurry A, 31.5% of resistance regulating and controlling slurry B and 2.8% of glass slurry. The resistance adjusting paste a, the resistance adjusting paste B, and the glass paste were the same as in example 2. The preparation method is the same as example 2.
Example 6
The high-temperature resistance paste comprises the following components in percentage by mass: 46.8% of resistance regulating slurry A, 50.12% of resistance regulating slurry B and 3.08% of glass slurry. The resistance adjusting paste a, the resistance adjusting paste B, and the glass paste were the same as in example 2. The preparation method is the same as example 2.
And printing the high-temperature resistance paste obtained in the step 3-6 on a zirconia ceramic sheet by adopting the same method as in the step 2, and drying and sintering to obtain the resistance film layer. The resistance of the resistance film layer and the resistance after 10h treatment at 1100 ℃ are shown in Table 2.
TABLE 2 sheet resistance of the resistance films obtained in examples 3-6 and resistance after 10h treatment at 1100 deg.C
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. The high-temperature resistance paste is characterized by comprising the following components in percentage by mass: resistance control slurry A1-95%, resistance control slurry B1-90% and glass slurry 1-15%; the resistance regulation and control slurry A is composed of 60-85% of conductive ceramic powder and 15-40% of organic carriers in mass fraction, and the resistance regulation and control slurry B is composed of the following raw materials in mass fraction: 60-78.5% of noble metal conductive phase and Bi2O31.5-10% of ZnO glass binder phase and 15-30% of organic carrier, wherein the glass slurry consists of 70-85% of glass phase and 15-30% of organic carrier by mass fraction.
2. The high-temperature resistor paste as recited in claim 1, wherein the conductive ceramic powder is lanthanum strontium manganate, lanthanum strontium cobaltate or lanthanum strontium ferrite, and the particle size of the conductive ceramic powder is 0.3-2 μm.
3. The high temperature resistive paste of claim 1, wherein the noble metal is Pt or Pd.
4. A high-temperature resistive paste according to claim 1, wherein said Bi is2O3Bi in the-ZnO glass binder phase2O3The mass fraction of (A) is 90-95%.
5. A high-temperature resistor paste according to claim 1, wherein the glass phase in the glass paste comprises the following raw materials in mass fraction: al (Al)2O35~10%、SiO240-50% of CaO 1-10%, BaO 30-40% and TiO21~5%。
6. A high-temperature resistor paste according to claim 1, wherein the organic vehicle comprises the following components in percentage by mass: 75-85% of butyl carbitol, 5-15% of tributyl citrate, 1-5% of ethyl cellulose, 851-5% of Span-and 1-10% of 1, 4-butyrolactone.
7. A method for preparing a high-temperature resistor paste according to any one of claims 1 to 6, comprising the steps of:
(1) preparing an organic carrier;
(2) preparing resistance regulation slurry A: mixing and grinding conductive ceramic powder and an organic carrier according to a proportion to obtain resistance regulation and control slurry A;
(3) preparing resistance regulation slurry B: firstly Bi is added2O3And ZnO powder are subjected to high-temperature smelting, quenching and ball milling to obtain Bi2O3-ZnO glass frit of Bi2O3-ZnO glass powder and noble metal powder are mixed to prepare mixed powder, the mixed powder and an organic carrier are uniformly mixed and ground, and resistance regulation and control slurry B is obtained;
(4) preparing glass slurry: firstly, carrying out high-temperature smelting, quenching and ball milling on glass-phase raw material powder to obtain glass-phase powder, and mixing and grinding the glass-phase powder and an organic carrier to obtain glass slurry;
(5) and mixing the resistance regulation slurry A, the resistance regulation slurry B and the glass slurry to obtain the high-temperature resistance slurry.
8. The preparation method of the high-temperature resistance paste according to claim 7, wherein in the step (1), butyl carbitol and tributyl citrate are weighed according to a proportion, stirred and mixed, then ethyl cellulose is added, and the mixture is heated to 90-100 ℃ and stirred for 1-2 hours under a heat preservation condition to completely dissolve the ethyl cellulose; adding Span-85 and 1, 4-butyrolactone, and continuously stirring for 2-3 h at 90-100 ℃ to obtain a clear and transparent uniform solution, namely the organic carrier.
9. The application of the high-temperature resistance paste according to claims 1-6 in preparing a resistance film layer, wherein the high-temperature resistance paste is printed on the surface of a substrate by a screen printing process, and is dried and sintered in air to obtain the resistance film layer.
10. The use of the high-temperature resistor paste according to claim 9 for preparing a resistor film, wherein the substrate is an alumina ceramic plate, a zirconia ceramic plate, an alumina coating or a zirconia coating; the drying process comprises the following steps: drying at 150-200 ℃ for 15-30 min, wherein the sintering process comprises the following steps: keeping the temperature of 1100-1200 ℃ for 1-2 h.
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