CN113793715B - Low-temperature coefficient resistance paste - Google Patents
Low-temperature coefficient resistance paste Download PDFInfo
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- CN113793715B CN113793715B CN202111354088.3A CN202111354088A CN113793715B CN 113793715 B CN113793715 B CN 113793715B CN 202111354088 A CN202111354088 A CN 202111354088A CN 113793715 B CN113793715 B CN 113793715B
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
- H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
- H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
- H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
- H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
- H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
- H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
- H01C17/06533—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of oxides
Abstract
The invention discloses a low-temperature coefficient resistance paste, which consists of 20-35% of conductive powder, 25-45% of glass bonding phase, 1-5% of additive and 30-45% of organic carrier by mass percent of 100%; the conductive powder is at least one of ruthenium dioxide and lead ruthenate, and the glass bonding phase is barium feldspar composite lead borosilicate glass, wherein the lead borosilicate glass powder and the barium feldspar are subjected to heat preservation in a muffle furnace at 450-500 ℃ for 24 hours and then are subjected to ball milling until the granularity is 0.7-1.3 mu m. According to the invention, the celsian is adopted to modify the lead-boron-silicon glass powder, and the temperature coefficient characteristic of the resistor is adjusted, so that the resistor slurry has the characteristic of small difference between positive and negative temperature coefficients, and can meet the use requirement of high-precision resistor products.
Description
Technical Field
The invention belongs to the technical field of resistance paste, and particularly relates to resistance paste which is applied to a high-precision resistor and has small temperature coefficient and small positive and negative temperature coefficient difference.
Background
The thick film resistor paste is a technology-intensive product integrating multiple subject fields of metallurgy, chemistry, materials, electronic technology, analysis and test technology and the like. In order to meet the requirements of printing and sintering processes and practical application requirements, the printing and sintering process has to have printability, functional characteristics and process compatibility. The common resistance paste is a paste formed by mixing a functional phase, a binding phase, an additive and an organic carrier according to a certain proportion.
The thick film resistor paste is used as a raw material for producing various resistors, and the paste is required to have a wider resistance range of 10-10M omega, so that the requirements of products in the resistors on resistance at different temperatures can be met.
The existing thick film resistor paste is applied to a resistor, the resistance value of the resistor changes along with the change of temperature, generally called as the temperature coefficient of the resistor, and the resistance value of a resistor product changes greatly due to the fact that the temperature coefficient of the resistor is too large or the difference of the resistance temperature coefficient is large in the process of high and low temperature change, and the thick film resistor paste cannot be applied to a high-precision resistor. Therefore, a resistance paste having a low temperature coefficient and a small difference between positive and negative temperature coefficients is required to satisfy the performance requirements of high-precision resistor products.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the resistor paste which is applied to a high-precision resistor and has small temperature coefficient and small positive and negative temperature coefficient difference.
In order to achieve the purpose, the low-temperature coefficient resistance paste provided by the invention comprises, by mass, 100% of conductive powder 20-35%, a glass binder phase 25-45%, an additive 1-5% and an organic carrier 30-45%.
The conductive powder is at least one of ruthenium dioxide and lead ruthenate, and the specific surface area of the ruthenium dioxide is 25-55 m2The specific surface area of the lead ruthenate is 3-10 m2/g。
The glass bonding phase is barium feldspar composite lead boron silicon glass, and the preparation method comprises the following steps: the barium feldspar composite lead-boron-silicon glass is prepared by uniformly mixing 50-70% of lead-boron-silicon glass powder and 30-50% of barium feldspar in a mass percent of 100%, preserving heat in a muffle furnace at 450-500 ℃ for 24 hours, and then performing ball milling on the mixture until the particle size is 0.7-1.3 mu m. Wherein the particle size of the celsian is 1.0-1.5 mu m; the lead-boron-silicon glass powder comprises the following components in percentage by mass of 100 percent: 50% -70% of PbO and SiO2 1%~5%、CaCO3 5%~10%、Al2O3 1%~10%、B2O31 to 20 percent of ZnO, 1 to 10 percent of lead-boron-silicon glass powder, wherein the softening temperature of the lead-boron-silicon glass powder is 350 to 400 ℃, and the granularity of the lead-boron-silicon glass powder is 1.0 to 1.5 mu m.
The additive is CuO or Nb2O5、Sb2O3At least two of them are mixed in an arbitrary ratio.
The organic carrier comprises the following components in percentage by mass of 100 percent: 8-15% of resin, 1-5% of organic additive and 80-90% of organic solvent. Wherein the resin is selected from any one of rosin resin, ethyl cellulose, hydroxy cellulose and methyl cellulose; the organic solvent is at least one selected from terpineol, butyl carbitol and butyl carbitol acetate; the organic additive is at least one of soybean lecithin and oleic acid.
The invention has the following beneficial effects:
according to the invention, the celsian is adopted to modify the lead-boron-silicon glass and then is used as glass to be bonded and correspondingly used in the resistor paste, so that the resistor paste has the characteristics of wide resistance range and small difference between positive and negative temperature coefficients, the problems of large temperature coefficient and wide range of positive and negative temperature coefficients of the traditional thick film resistor paste are solved, and the product performance requirements of the high-precision thick film resistor are met.
Drawings
Fig. 1 is a resistance paste test pattern.
Detailed Description
The invention is described in detail below with reference to the drawings and examples, which do not limit the scope of the invention. The scope of the present invention is defined only by the appended claims, and any omissions, substitutions, and changes in the form of the embodiments disclosed herein that may be made by those skilled in the art are intended to be included within the scope of the present invention.
1. Selection of conductive powder: the specific surface area of the ruthenium dioxide is 25-55 m2The specific surface area of the lead ruthenate is 3-10 m2/g。
2. Preparing lead-boron-silicon glass powder: according to the mass percentage of PbO 65 percent and SiO2 3%、CaCO3 9%、Al2O3 3%、B2O3Weighing raw materials of 15% and ZnO 5%, uniformly mixing the raw materials, putting the obtained mixture into a smelting furnace at 1050 ℃ for smelting, keeping the temperature for 2 hours, performing water quenching on the obtained glass solution to obtain glass, crushing the glass into glass slag, grinding the glass slag into particles with the particle size of 1.0-1.5 mu m by using a ball mill, and drying to obtain the lead-boron-silicon glass powder.
3. Preparation of glass binder phase: and (2) wet-mixing the lead-boron-silicon glass powder and celsian with the granularity of 1.0-1.5 mu m according to the mass percentage in the table 1 by using deionized water in a ball mill for 2 hours, drying, then carrying out heat preservation sintering in a muffle furnace at 470 ℃ for 24 hours, carrying out breakage ball milling until the granularity ranges from 0.7 mu m to 1.3 mu m, and obtaining the celsian composite lead-boron-silicon glass BL-1 to BL-5 serving as glass bonding phases.
TABLE 1 mass% of glass binder phase
Meanwhile, the glass bonding phases BL-6 to BL-10 are used for comparison tests, and the preparation method of the glass bonding phases BL-6 to BL-10 is as follows:
according to the mass percentage, 40 percent of lead-boron-silicon glass powder and 16.3 percent of Al with the granularity of 0.5-1.5 mu m2O319.2% of SiO with a particle size of 0.5 to 1.5 μm2And carrying out heat preservation sintering on 24.5% BaO with the granularity of 0.5-1.5 mu m in a muffle furnace at 470 ℃ for 24 hours, and carrying out breakage ball milling until the granularity is 0.7-1.3 mu m to obtain the glass bonding phase BL-6.
According to the mass percentage of PbO 26 percent and SiO2 20.4%、CaCO3 3.6%、Al2O3 17.5%、B2O3Weighing raw materials of 6%, BaO 24.5% and ZnO 2%, uniformly mixing the raw materials, putting the mixture into a smelting furnace at 1050 ℃ for smelting, keeping the temperature for 1.5h, performing water quenching on the obtained mixture to obtain glass slag, grinding the glass slag into particles with the particle size of 0.7-1.3 mu m by using a ball mill, and drying to obtain the glass bonding phase BL-7.
And (2) insulating and sintering the celsian with the granularity of 0.5-1.5 mu m in a muffle furnace at 470 ℃ for 24h, mixing the celsian with lead-boron-silicon glass powder according to the mass ratio of 6:4, wet-mixing the mixture with deionized water in a ball mill for 2h, drying the mixture, and then performing breakage ball milling until the granularity is 0.7-1.3 mu m to obtain a glass bonding phase BL-8.
According to the mass percentage of PbO 65 percent and SiO2 3%、CaCO3 9%、Al2O3 3%、B2O3Weighing raw materials of 15% and ZnO 5%, uniformly mixing the raw materials, uniformly mixing the obtained mixture with celsian with the granularity of 1.0-1.5 mu m according to the mass ratio of 4:6, then putting the mixture into a 1050 ℃ smelting furnace for smelting, keeping the temperature for 1.5h, performing water quenching on the obtained glass solution to obtain glass, crushing the glass into glass slag, grinding the glass slag into the granularity of 0.7-1.3 mu m by using a ball mill, and drying to obtain the glass bonding phase BL-9.
Insulating and sintering the celsian with the granularity of 1.0-1.5 mu m in a muffle furnace at 470 ℃ for 24 hours to obtain heat-treated celsian; according to the mass percentage of PbO 65 percent and SiO2 3%、CaCO3 9%、Al2O3 3%、B2O3Weighing raw materials of 15% and ZnO 5%, uniformly mixing the raw materials, uniformly mixing the obtained mixture and the heat-treated celsian in a mass ratio of 4:6, then putting the mixture into a 1050 ℃ smelting furnace for smelting, keeping the temperature for 1.5h, performing water quenching on the obtained glass solution to obtain glass, crushing the glass into glass slag, grinding the glass slag into particles with a size of 0.7-1.3 mu m by using a ball mill, and drying to obtain the glass bonding phase BL-10.
4. Preparation of the additive: mixing CuO and Nb2O5、Sb2O3Mixing according to the mass ratio of 1:0.2:0.2 to obtain the additive.
5. Preparation of organic vehicle: weighing raw materials according to the mass percentage of 65% of terpineol, 3% of soybean lecithin, 8% of ethyl cellulose and 24% of butyl carbitol acetate, stirring and heating the terpineol and the soybean lecithin in a beaker to 70 ℃, adding the base cellulose, continuously stirring and completely dissolving, then adding the butyl carbitol acetate, preserving heat and stirring for 30min to obtain the organic carrier.
6. Preparing resistance paste: according to the mass percentage in the table 2, the specific surface area is 25-55 m2Ruthenium dioxide in g, having a specific surface area of3~10m2The lead ruthenate/g, the glass binder phase, the additive and the organic carrier are uniformly mixed, and then fully ground by a three-roll mill until the fineness is less than 5 mu m, so that the resistance paste of the embodiment 1-7 is prepared.
TABLE 2 weight percentages (%) -of resistance pastes in inventive examples 1 to 7
Meanwhile, according to the mass percentage in the table 3, after the components are uniformly mixed, the mixture is fully ground by a three-roll mill until the fineness is less than 5 μm, and the resistance slurry with the proportion of 1-8 in pairs is prepared.
TABLE 3 comparative examples 1 to 8% by mass of resistance paste (%)
Note: in the table, the barium feldspar (heat treatment) refers to that the barium feldspar with the granularity of 1.0-1.5 mu m is subjected to heat preservation sintering at 470 ℃ in a muffle furnace for 24 hours and then is subjected to ball milling until the particle size is 0.7-1.3 mu m.
The resistance pastes of the above examples 1 to 7 and comparative examples 1 to 8 were respectively printed on alumina ceramic substrates by a screen printing process according to the screen pattern of fig. 1, dried at 150 ℃ for 10min, sintered in a belt sintering furnace at 850 ± 5 ℃ for 60min with a sintering cycle and 10min peak heat preservation to prepare test samples, and the following performance tests were performed:
square resistance: the sheet resistance test was performed according to method 105 of the sheet resistance test method of electronic paste for SJ/T11512-2015 integrated circuits, and the resistance value at the a position in fig. 1 was measured.
Temperature Coefficient (TCR): according to the method 301 of temperature coefficient of resistance paste (TCR) test method in the test method of performance of electronic paste for SJ/T11512-2015 integrated circuit, the resistance values at the position a in figure 1 and at the temperature of 25 ℃, 125 ℃ and 55 ℃ of the resistor body are respectively tested. The resistance change rate of 1 ℃ per change at 25-125 ℃ is a positive temperature coefficient (HTCR), and the resistance change rate of 1 ℃ per change at 25-55 ℃ is a negative temperature coefficient (CTCR). The temperature coefficient range of the conventional resistance paste is-100- +100 ppm/DEG C. The temperature coefficient difference is referred to as HTCR-CTCR.
Electrostatic discharge (ESD): the resistance paste is characterized in that the change rate of the resistance value of the resistor body after the static discharge impact is used for determining the resistance of the resistor against the static discharge in use, and the change rate of the resistance value is close to zero, which indicates that the performance of the resistance paste is better. According to the performance test method of the electronic paste for the SJ/T11512-2015 integrated circuit, namely the method 302 resistance electrostatic discharge test method, the resistance value R1 of the resistance at the position a in the figure 1 is respectively tested, 5kV electrostatic discharge impact is carried out on the resistance at the position a, then the resistance value R2 of the resistance at the position a in the figure 1 is tested, and the resistance change rate before and after electrostatic discharge is calculated.
The results of the tests of the above examples and comparative examples are shown in Table 4, and are compared with that of 2031 (a product of DuPont, USA) which is commercially available.
TABLE 4 comparison of resistance paste Properties
As can be seen from table 4, in the embodiments 1 to 7 of the present invention, when the resistor paste is compared with a commercial thick film resistor paste, and barium feldspar composite lead-boron-silicon glass is used as glass for bonding and is correspondingly used in the resistor paste, the resistor paste with a small temperature coefficient value, a small positive and negative temperature coefficient difference value, and excellent resistance ESD performance can be obtained. Example 3 is compared with comparative examples 1, 2 and 3, which shows that the temperature coefficient characteristics of the resistance paste can be adjusted only by using the glass binder phase compounded by celsian and lead-boron-silicon glass powder, so that the resistance paste with small temperature coefficient value, small difference between positive and negative temperature coefficients and excellent resistance ESD performance is obtained. Example 3 is compared with comparative examples 4, 5, 6, 7 and 8, which shows that the temperature coefficient characteristics of the resistance paste can be adjusted only after the celsian and the lead-boron-silicon glass powder are treated and compounded according to the process of the invention, and the resistance paste with small temperature coefficient value, small difference value between positive and negative temperature coefficients and excellent resistance ESD performance is obtained.
Claims (7)
1. A low temperature coefficient resistor paste, characterized by: the resistance paste consists of 20-35% of conductive powder, 25-45% of glass bonding phase, 1-5% of additive and 30-45% of organic carrier by mass percent of 100%;
the conductive powder is at least one of ruthenium dioxide and lead ruthenate;
the glass bonding phase is barium feldspar composite lead boron silicon glass, and the preparation method comprises the following steps: the barium feldspar composite lead-boron-silicon glass is prepared by uniformly mixing 50-70% of lead-boron-silicon glass powder and 30-50% of barium feldspar in a mass percent of 100%, preserving heat in a muffle furnace at 450-500 ℃ for 24 hours, and then performing ball milling on the mixture until the particle size is 0.7-1.3 mu m.
2. The low temperature coefficient of resistance paste of claim 1, wherein: the specific surface area of the ruthenium dioxide is 25-55 m2The specific surface area of the lead ruthenate is 3-10 m2/g。
3. The low temperature coefficient of resistance paste of claim 1, wherein: the lead-boron-silicon glass powder comprises the following components in percentage by mass of 100 percent: 50% -70% of PbO and SiO2 1%~5%、CaCO3 5%~10%、Al2O3 1%~10%、B2O31 to 20 percent of ZnO, 1 to 10 percent of lead-boron-silicon glass powder, wherein the softening temperature of the lead-boron-silicon glass powder is 350 to 400 ℃, and the granularity of the lead-boron-silicon glass powder is 1.0 to 1.5 mu m.
4. The low temperature coefficient of resistance paste of claim 1, wherein: the particle size of the celsian is 1.0-1.5 mu m.
5. The low temperature coefficient of resistance paste of claim 1, wherein: the additive is CuO or Nb2O5、Sb2O3At least two of them are mixed in an arbitrary ratio.
6. The low temperature coefficient of resistance paste of claim 1, wherein: the organic carrier comprises the following components in percentage by mass of 100 percent: 8-15% of resin, 1-5% of organic additive and 80-90% of organic solvent.
7. The low temperature coefficient of resistance paste of claim 6, wherein: the resin is selected from any one of rosin resin, ethyl cellulose, hydroxy cellulose and methyl cellulose; the organic solvent is at least one selected from terpineol, butyl carbitol and butyl carbitol acetate; the organic additive is at least one of soybean lecithin and oleic acid.
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CN114121335B (en) * | 2022-01-24 | 2022-04-19 | 西安宏星电子浆料科技股份有限公司 | Low-contact-resistance type resistance paste |
CN114121336B (en) * | 2022-01-27 | 2022-04-19 | 西安宏星电子浆料科技股份有限公司 | High-wear-resistance paste |
CN114267473B (en) * | 2022-02-28 | 2022-05-27 | 西安宏星电子浆料科技股份有限公司 | Easily-printed chip resistor paste with stable viscosity and thixotropic value |
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