CN110085347B - Lead-free stainless steel base heating resistor slurry and preparation method thereof - Google Patents
Lead-free stainless steel base heating resistor slurry and preparation method thereof Download PDFInfo
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- CN110085347B CN110085347B CN201910361943.XA CN201910361943A CN110085347B CN 110085347 B CN110085347 B CN 110085347B CN 201910361943 A CN201910361943 A CN 201910361943A CN 110085347 B CN110085347 B CN 110085347B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention relates to the technical field of resistance paste, in particular to lead-free stainless steel base heating resistance paste and a preparation method thereof. The thick film circuit resistance paste prepared by the invention has good conductivity, strong adhesive force, good weldability, good welding resistance, printing property, sintering property and environmental protection property, is matched with a stainless steel base material, and has good wettability and compatibility with a medium paste and an electrode paste.
Description
Technical Field
The invention relates to the technical field of resistance paste, in particular to lead-free stainless steel base heating resistance paste and a preparation method thereof.
Background
In the field of electric heating, the novel heating element requires small volume, large power, small thermal inertia, large surface heat load, low power consumption, high thermal efficiency, quick hot start, stable power, uniform temperature field, good manufacturability, self-temperature control of the body, safe and reliable operation, long service life and wide application range. The electrode slurry is a key material for packaging, electrode and interconnection of electronic components, and mainly comprises two major types of burn-through electrode slurry and curing conductive adhesive. The electrode paste may be classified into carbon paste (graphite conductor), metal paste (gold powder, silver powder, copper powder, silver-copper alloy), and modified ceramic paste according to the filler thereof. Classified according to curing conditions, there are thermal curing, ultraviolet curing, and the like. The traditional sintering-infiltrating electrode slurry contains a large amount of lead, is very unfavorable for environmental protection, and the conductive adhesive used at present also contains some harmful substances and has higher cost.
CN106205773 researches a thick film circuit rare earth electrode paste with good conductivity, strong adhesion, good weldability, good anti-welding solubility, printing property, sintering property and environmental protection property, which is matched with a stainless steel base material and has good wettability and compatibility with a medium paste and a resistance paste. The slurry can meet the index requirements to a certain extent, but the price of ruthenium as a noble metal is one kilogram and thirty-four thousand, so that the slurry has extremely high cost and lower economic benefit.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the lead-free stainless steel-based heating resistor paste with low cost and the preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
45 to 55 percent of composite functional phase
20 to 30 percent of inorganic bonding phase
20-30% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
75-95% of molybdenum disilicide powder
5-25% of nickel powder.
The lead-free stainless steel-based heating resistor paste preferably comprises the following components in percentage by mass:
50 percent of composite functional phase
25 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
85 percent of molybdenum disilicide powder
15% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 35-45%
CaO 25-30%
Ti2O 8-12%
Al2O3 13-18%
Na2O 5-10%
Bi2O3 2-6%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 5-7h at the temperature of 1400-1600 ℃, water quenching, ball milling and drying to obtain the lead-free glass micro powder.
Preferably, the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a certain proportion, smelting for 6h at 1500 ℃, quenching with water, ball-milling for 8h by taking distilled water as a medium, and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
75-85% of N-methylpyrrolidone
Polyvinyl formal acetal 13-21%
0.5 to 1.5 percent of polymethacrylic acid amine
Polyglycerol fatty acid ester 0.5-1.5%
Hydrogenated castor oil 0.5-1.5%.
Preferably, the organic carrier comprises the following components in percentage by mass:
80 percent of N-methylpyrrolidone
Polyvinyl formal acetal 17%
1 percent of polymethacrylic acid amine
Polyglycerin fatty acid ester 1%
Hydrogenated castor oil 1%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 75-85 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPa.s.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
The invention has the beneficial effects that:
1. the thick film circuit resistance paste prepared by the invention has good conductivity, strong adhesive force, good weldability, good welding resistance, printing property, sintering property and environmental protection property, is matched with a stainless steel base material, and has good wettability and compatibility with a medium paste and an electrode paste;
2. the nickel and the molybdenum disilicide are only hundreds of yuan per kilogram, the cost of the resistance paste is low, the economic efficiency is higher, and the lead-free performance in the paste is realized.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
50 percent of composite functional phase
25 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
85 percent of molybdenum disilicide powder
15% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 38%
CaO 26%
Ti2O 10%
Al2O3 15%
Na2O 7%
Bi2O3 4%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a certain proportion, smelting for 6h at 1500 ℃, quenching with water, ball-milling for 8h by taking distilled water as a medium, and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
80 percent of N-methylpyrrolidone
Polyvinyl formal acetal 17%
1 percent of polymethacrylic acid amine
Polyglycerin fatty acid ester 1%
Hydrogenated castor oil 1%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 80 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPas.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
Example 2
The lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
45 percent of composite functional phase
30 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
75 percent of molybdenum disilicide powder
25% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 35%
CaO 30%
Ti2O 10%
Al2O3 14%
Na2O 9%
Bi2O3 2%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 7 hours at the temperature of 1400 ℃, water quenching, ball milling and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
n-methylpyrrolidone 75%
Polyvinyl formal acetal 21%
1 percent of polymethacrylic acid amine
Polyglycerol fatty acid ester 1.5%
Hydrogenated castor oil 1.5%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 75 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPas.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
Example 3
The lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
55 percent of composite functional phase
20 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
95 percent of molybdenum disilicide powder
25% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 45%
CaO 25%
Ti2O 10%
Al2O3 13%
Na2O 5%
Bi2O3 2%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 5 hours at 1600 ℃, water quenching, ball milling and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
n-methylpyrrolidone 85%
Polyvinyl formal acetal 13%
0.5 percent of polymethacrylic acid amine
Polyglycerol fatty acid ester 0.5%
Hydrogenated castor oil 1%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at 85 ℃, and controlling the viscosity of the organic carrier to be 200-300mPa & s.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
Example 4
The lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
55 percent of composite functional phase
20 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
90 percent of molybdenum disilicide powder
10% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 35%
CaO 28%
Ti2O 8%
Al2O3 15%
Na2O 10%
Bi2O3 4%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 7 hours at the temperature of 1400 ℃, water quenching, ball milling and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
80 percent of N-methylpyrrolidone
Polyvinyl formal acetal 15.5%
Polymethacrylic acid amine 1.5%
Polyglycerol fatty acid ester 1.5%
Hydrogenated castor oil 1.5%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 80 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPas.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
Example 5
The lead-free stainless steel-based heating resistor paste comprises the following components in percentage by mass:
50 percent of composite functional phase
20 percent of inorganic bonding phase
30% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
molybdenum disilicide powder 80%
20% of nickel powder.
The inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO2 40%
CaO 25%
Ti2O 12%
Al2O3 14%
Na2O 6%
Bi2O3 3%。
the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 6 hours at 1500 ℃, quenching with water, ball-milling, and drying to obtain the lead-free glass micro powder.
Wherein the particle size of the lead-free glass micro powder is 1-3 mu m.
The organic carrier comprises the following components in percentage by mass:
n-methyl pyrrolidone 82%
Polyvinyl formal acetaldehyde 15%
1 percent of polymethacrylic acid amine
Polyglycerin fatty acid ester 1%
Hydrogenated castor oil 1%.
The preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 80 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPas.
The preparation method of the lead-free stainless steel-based heating resistor paste comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
The resistance paste of the embodiments 1-5 of the invention is coated on a stainless steel substrate for sintering, the sintering temperature is controlled at 900 ℃, the temperature is controlled at 15min, the obtained resistance film has the thickness of 10-15um, the sheet resistance is 2-100 ohm, the adhesive force is more than 10N, and the aging strength is more than 10N.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (8)
1. A lead-free stainless steel base heating resistor sizing agent is characterized in that: the composite material comprises the following components in percentage by mass:
45 to 55 percent of composite functional phase
20 to 30 percent of inorganic bonding phase
20-30% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
75-95% of molybdenum disilicide powder
5-25% of nickel powder;
the inorganic bonding phase is lead-free glass micro powder and comprises the following components in percentage by mass:
SiO235-45%
CaO25-30%
Ti2O8-12%
Al2O313-18%
Na2O5-10%
Bi2O32-6%；
the organic carrier comprises the following components in percentage by mass:
75-85% of N-methylpyrrolidone
Polyvinyl formal acetal 13-21%
0.5 to 1.5 percent of polymethacrylic acid amine
Polyglycerol fatty acid ester 0.5-1.5%
Hydrogenated castor oil 0.5-1.5%.
2. The lead-free stainless steel-based heat-generating resistor paste according to claim 1, characterized in that: the composite material comprises the following components in percentage by mass:
50 percent of composite functional phase
25 percent of inorganic bonding phase
25% of organic carrier;
the composite functional phase comprises the following components in percentage by mass:
85 percent of molybdenum disilicide powder
15% of nickel powder.
3. The lead-free stainless steel-based heat-generating resistor paste according to claim 1, characterized in that: the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a ratio, smelting for 5-7h at the temperature of 1400-1600 ℃, water quenching, ball milling and drying to obtain the lead-free glass micro powder.
4. The lead-free stainless steel-based heat-generating resistor paste according to claim 3, characterized in that: the preparation method of the inorganic bonding phase comprises the following steps: mixing the oxides according to a certain proportion, smelting for 6h at 1500 ℃, quenching with water, ball-milling for 8h by taking distilled water as a medium, and drying to obtain the lead-free glass micro powder.
5. The lead-free stainless steel-based heat-generating resistor paste according to claim 3, characterized in that: the particle size of the lead-free glass micro powder is 1-3 mu m.
6. The lead-free stainless steel-based heat-generating resistor paste according to claim 1, characterized in that:
the organic carrier comprises the following components in percentage by mass:
80 percent of N-methylpyrrolidone
Polyvinyl formal acetal 17%
1 percent of polymethacrylic acid amine
Polyglycerin fatty acid ester 1%
Hydrogenated castor oil 1%.
7. The lead-free stainless steel-based heat-generating resistor paste according to claim 1, characterized in that: the preparation method of the organic carrier comprises the following steps: weighing the raw materials according to the mass ratio, dissolving the raw materials in a water bath at the temperature of 75-85 ℃, and controlling the viscosity of the organic carrier to be 200-300 mPa.s.
8. The production method of a lead-free stainless steel-based heat-generating resistor paste according to any one of claims 1 to 7, characterized in that: the method comprises the following steps: and stirring and dispersing the composite functional phase, the inorganic bonding phase and the organic carrier in a container, and then performing three-roll rolling to obtain the resistance paste with the viscosity range of 100 pas +/-20 pas.
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| CN201910361943.XA CN110085347B (en) | 2019-04-30 | 2019-04-30 | Lead-free stainless steel base heating resistor slurry and preparation method thereof |
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| CN201910361943.XA CN110085347B (en) | 2019-04-30 | 2019-04-30 | Lead-free stainless steel base heating resistor slurry and preparation method thereof |
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| CN110085347B true CN110085347B (en) | 2020-11-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4289297A4 (en) * | 2021-02-02 | 2024-04-03 | Shenzhen Smoore Technology Ltd | Heating component and electronic atomizing device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5470506A (en) * | 1988-12-31 | 1995-11-28 | Yamamura Glass Co., Ltd. | Heat-generating composition |
| CN105828465A (en) * | 2016-03-31 | 2016-08-03 | 东莞珂洛赫慕电子材料科技有限公司 | Thick-film resistor slurry based on stainless steel base material and preparation method thereof |
| CN106211378A (en) * | 2016-06-30 | 2016-12-07 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of silicon carbide-containing silver palladium combined resistance slurry and preparation method thereof |
| CN106205773B (en) * | 2016-07-06 | 2018-04-24 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of rare earth thick film circuit electrode slurry based on stainless steel substrate and preparation method thereof |
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