CN114121335B - Low-contact-resistance type resistance paste - Google Patents
Low-contact-resistance type resistance paste Download PDFInfo
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- CN114121335B CN114121335B CN202210078470.4A CN202210078470A CN114121335B CN 114121335 B CN114121335 B CN 114121335B CN 202210078470 A CN202210078470 A CN 202210078470A CN 114121335 B CN114121335 B CN 114121335B
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- 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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- 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
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C10/00—Adjustable resistors
- H01C10/30—Adjustable resistors the contact sliding along resistive element
- H01C10/305—Adjustable resistors the contact sliding along resistive element consisting of a thick film
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Abstract
The invention discloses a low-contact resistance type resistance paste, which comprises the following components in percentage by mass: 15-45% of conductive powder, 20-40% of glass bonding phase, 1-10% of additive and 30-45% of organic carrier; the conductive powder is graphite alkyne composite lead ruthenate prepared by a chemical deposition method, and the glass bonding phase is lead-boron-silicon glass powder with the softening temperature of 500-600 ℃. The resistance paste has the characteristics of good temperature coefficient and small contact resistance, and can meet the use requirements of resistance paste products for thick film sliding resistors and electric tools.
Description
Technical Field
The invention belongs to the technical field of resistance paste, and particularly relates to resistance paste with low contact resistance.
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 composite material must 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 resistance paste is used as a raw material for producing the thick film sliding resistor, and the paste is required to have good temperature coefficient and meet the requirement of low contact resistance of a thick film sliding resistor product. The existing resistance paste is applied to a thick film sliding resistor, and in the sliding process of the resistor, the contact point is heated and ignited due to high contact resistance, so that the resistor fails. Therefore, there is a need for a resistive paste having low contact resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the resistance paste which is suitable for the performance requirements of thick film sliding resistors and electric tools and has the characteristics of good temperature coefficient, low contact resistance and the like.
In order to achieve the aim, the low contact resistance type resistance paste provided by the invention comprises the following components in percentage by mass: 15-45% of conductive powder, 20-40% of glass bonding phase, 1-10% of additive and 30-45% of organic carrier.
The conductive powder is graphite alkyne composite lead ruthenate, wherein the mass ratio of the lead ruthenate to the graphite alkyne is 3: 1-5: 1, and the conductive powder is prepared by the following steps:
step 1: dissolving soluble salt of ruthenium in pure water to form Ru3+An ionic solution A; dissolving soluble salt of lead in pure water to form Pb2+An ionic solution B; adding the graphyne into pure water to form a turbid liquid C, wherein the concentration of the graphyne in the turbid liquid C is 5-10 g/L.
Step 2: solution A, B as Ru3+With Pb2+Dropwise adding the solution into the suspension C under the stirring condition with the molar ratio of 1:1, stopping stirring after the solution A, B is dropwise added, and standing for 20-24 hours.
And step 3: and (3) extracting the upper-layer liquid of the precipitate from the solution after standing, adding pure water into the extracted liquid again, stirring for 10-15 minutes, and standing for 20-24 hours.
And 4, step 4: and repeating the operation of the step 3 twice, and then carrying out suction filtration and freeze drying on the sediment at the bottom layer.
And 5: and (4) calcining the dried substance obtained in the step (4) at 550-600 ℃ for 30-40 minutes in vacuum, and performing breakage ball milling until the particle size is 0.7-1.3 mu m to obtain the graphite alkyne composite lead ruthenate.
In the step 1, the soluble salt of ruthenium is any one of ruthenium chloride, ruthenium iodide, ruthenium nitrate and ruthenium acetate; the soluble salt of lead is any one of lead nitrate and lead acetate.
The glass bonding phase is lead-boron-silicon glass powder, the softening temperature of the glass bonding phase is 500-600 ℃, the granularity of the glass bonding phase is 1.0-1.5 mu m, and the glass bonding phase is prepared from the following components in percentage by mass: 55 to 70 percent of PbO and SiO2 5%～25%、Al2O3 1%～10%、B2O31 to 20 percent and ZnO 5 to 10 percent.
The additive is ZnO or MnO2、ZrO2A mixture of any two or more of them.
The organic carrier comprises the following components in percentage by mass: 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 selected from one or more of terpineol, butyl carbitol and butyl carbitol acetate; the organic additive is selected from one or two of lecithin and oleic acid.
The invention has the following beneficial effects:
the method adopts the graphite alkyne composite lead ruthenate prepared by a chemical deposition method as a conductive phase to be applied to resistance slurry, and adopts freeze drying and vacuum calcination processes in the process of preparing the graphite alkyne composite lead ruthenate by a chemical deposition method to prevent the conductive phase from agglomeration in the drying and roasting processes, so that the obtained graphite alkyne composite lead ruthenate has small granularity and uniform distribution. After the resistor paste is sintered, the surface is smooth, the conductive phase materials are distributed more uniformly, the sliding electric brush is contacted with the conductive phase on the surface of the resistor body more uniformly, and the problem of large contact resistance of the traditional thick-film resistor paste is solved.
The preparation process of the resistor paste is simple, the process adaptability is strong, the electrostatic discharge and encapsulation change rate of the resistor is small, and the contact resistance of the surface of the resistor is small.
Drawings
FIG. 1 is a graph of resistance, temperature coefficient, electrostatic discharge, and encapsulation variation rate performance tests for resistor paste.
Fig. 2 is a resistance paste contact resistance test pattern.
Detailed Description
The invention is described in detail below with reference to specific figures 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. Preparation of conductive powder
Preparation of conductive phase 1:
step 1: dissolving ruthenium nitrate in pure water to form Ru3+Solution A with the ion concentration of 1 mol/L; dissolving lead nitrate in pure water to form Pb2+Solution B with the ion concentration of 1 mol/L; adding the graphyne into pure water to form turbid liquid C with the concentration of the graphyne being 5 g/L.
Step 2: according to Ru3+With Pb2+500mL of solution A and 500mL of solution B were added dropwise to 1000mL of suspension C with stirring at a molar ratio of 1:1, and after the addition of solution A, B was completed, stirring was stopped and the mixture was allowed to stand for 24 hours.
And step 3: and extracting the upper layer liquid of the precipitate from the solution after standing, adding pure water into the extracted liquid again, stirring for 10 minutes, and standing for 24 hours.
And 4, step 4: and repeating the operation of the step 3 twice, and then carrying out suction filtration and freeze drying on the sediment at the bottom layer.
And 5: and (4) calcining the dried substance in the step (4) for 30 minutes at 550-600 ℃ in vacuum, and performing breakage ball milling until the particle size is 0.7-1.3 mu m to obtain the graphite alkyne composite lead ruthenate.
Preparation of conductive phase 2: and replacing the graphite alkyne in the preparation of the conductive phase 1 with graphite with equal mass, and obtaining the graphite composite lead ruthenate by the same steps as the preparation of the conductive phase 1.
Preparation of conductive phase 3: replacing the graphite alkyne in the preparation of the conductive phase 1 with carbon black with equal mass, and obtaining the carbon black composite lead ruthenate by the same steps as the preparation of the conductive phase 1.
Preparation of conductive phase 4: the freeze drying in the step 4 of preparing the conductive phase 1 is changed into drying in an oven at 80 ℃, and other steps are the same as the preparation of the conductive phase 1.
Preparation of conductive phase 5: and (3) calcining the conductive phase 1 at 550-600 ℃ for 30 minutes in vacuum in the preparation step 5 instead of calcining the conductive phase at 550-600 ℃ for 30 minutes in air atmosphere, and other steps are the same as the preparation of the conductive phase 1.
Preparation of conductive phase 6: and (3) calcining the conductive phase 1 at 550-600 ℃ for 30 minutes in vacuum in the preparation step 5 instead of calcining the conductive phase at 550-600 ℃ for 30 minutes in a nitrogen atmosphere, and other steps are the same as the preparation of the conductive phase 1.
Preparation of conductive phase 7: and (3) calcining the conductive phase 1 at 550-600 ℃ for 30 minutes in vacuum in the preparation step 5 instead of calcining the conductive phase at 550-600 ℃ for 30 minutes in pure oxygen atmosphere, and other steps are the same as the preparation of the conductive phase 1.
Preparation of conductive phase 8: without preparing the solutions A and B, 6.65g of ruthenium dioxide and 11.15g of lead oxide were added to 1000mL of the suspension C under stirring, directly in a molar ratio of ruthenium dioxide to lead oxide of 1:1, the other steps being identical to those of the preparation of the conductive phase 1.
Conductive phase 9: directly adding 17.8g of solution A and solution B without preparing the solution A and the solution B, wherein the specific surface area is 3-10 m2Per g of lead ruthenate are added with stirring to 1000mL of suspension C, the other steps being identical to the preparation of the conductive phase 1.
Preparation of the conductive phase 10: uniformly mixing ruthenium dioxide, lead oxide and graphite alkyne according to the mass ratio of 6.65:11.15: 5.
Preparation of conductive phase 11: the specific surface area is 3 to 10m2Lead ruthenate/g and graphite alkyne are uniformly mixed according to the mass ratio of 17.8: 5.
Preparation of the conductive phase 12: uniformly mixing ruthenium dioxide, lead oxide and carbon black according to the mass ratio of 6.65:11.15: 5.
Preparation of conductive phase 13: the specific surface area is 3 to 10m2Lead ruthenate/g and carbon black are uniformly mixed according to the mass ratio of 17.8: 5.
Preparation of conductive phase 14: uniformly mixing ruthenium dioxide, lead oxide and graphite according to the mass ratio of 6.65:11.15: 5.
Preparation of conductive phase 15: the specific surface area is 3 to 10m2Lead ruthenate/g, graphite in a mass ratio of 17.8:5, mixing uniformly.
2. Preparation of glass binder phase: according to mass percentage of PbO 55 percent and SiO2 22%、Al2O3 4%、B2O310 percent and ZnO 9 percent, uniformly mixing various oxides, putting the obtained mixture into a 1350 ℃ smelting furnace 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 1-1.5 mu m by using a ball mill, and drying to obtain the lead-boron-silicon glass powder with the softening temperature of 530 ℃.
3. Preparation of the additive: adding ZnO and MnO2、ZrO2Mixing according to the weight ratio of 1:0.2:0.2 to obtain the additive.
4. Preparation of organic vehicle: stirring 65g of terpineol and 3g of soybean lecithin in a beaker, heating to 70 ℃, adding 8g of ethyl cellulose, continuously stirring until the ethyl cellulose is completely dissolved, adding 24g of butyl carbitol acetate, and stirring for 30 minutes under the condition of heat preservation to obtain the organic carrier.
5. Preparing resistance paste: the components were uniformly mixed in mass percentage in table 1, and then sufficiently ground by a three-roll mill until the fineness was less than 5 μm, to prepare the resistance pastes of examples 1 to 5 and comparative examples 1 to 14.
Table 1 resistance paste formulation (mass%,%)
Respectively printing the resistance paste on an alumina ceramic substrate by a screen printing process according to the screen printing plate patterns shown in the figures 1 and 2, drying at 150 ℃ for 10min, sintering in a belt sintering furnace at 850 +/-5 ℃, keeping the sintering period for 60min and the peak value for 10min to prepare a test sample, and carrying out the following performance tests:
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 position a in fig. 1 was tested.
Temperature Coefficient (TCR): the resistance values at the A position of the resistor body in the graph 1 at 25 ℃, 125 ℃ and 55 ℃ are respectively tested according to a resistance paste Temperature Coefficient (TCR) test method 301 in an electronic paste performance test method for SJ/T11512-2015 integrated circuits. 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.
Electrostatic discharge: the resistance paste is characterized by comprising a resistance paste, wherein the resistance paste is prepared by mixing a resistance slurry and a resistance paste, wherein the resistance paste is prepared by mixing a resistance paste and a resistance paste, and the resistance paste is prepared by mixing a resistance paste and a resistance paste. According to the performance test method of the electronic paste for the SJ/T11512-2015 integrated circuit, namely the resistance electrostatic discharge test method 302, the resistance value R1 of the resistor at the position A in the figure 1 is respectively tested, 5kV electrostatic pulse impact is carried out on the resistance value R2, and the resistance value change rate before and after pulse voltage is calculated.
Encapsulation change rate: the surface of the resistor body is covered with glass slurry, the smaller the resistance change rate before and after sintering, the smaller the encapsulation change rate, the more stable the resistor is, and the encapsulation change rate is generally required to be small +/-0.5%. In the test chart 1, the resistance value R1 of the resistor body is arranged at the position A, the surface of the resistor body is printed with encapsulation glass slurry, the resistor body is dried at 150 ℃ and sintered at 500-600 ℃, then the resistance value R2 of the resistor body is measured, and the resistance change rate before and after encapsulation is calculated.
Contact resistance: according to the structure of fig. 2, the c-position resistor is contacted with a metal brush with a pressure of 20 g. Separately test Rab、Rac、RbcResistance value of (1), contact resistance DeltaRContact with=（Rac+Rbc-Rab）/2RabThe smaller the contact resistance, the more and more uniform the distribution of the conductive phase on the surface of the resistor, and the better the contact effect with the brush. Contact resistance of less than 0.3% is generally required.
The results of the tests of the above examples and comparative examples are shown in Table 2, and are compared with those of 4351 (DuPont, U.S.) and R-315-P (ESL, U.S.).
TABLE 2 comparison of resistance paste Properties
As can be seen from table 2, when the resistance paste prepared in embodiments 1 to 5 of the present invention is compared with a commercial thick film resistance paste, and the resistance paste with good temperature coefficient, electrostatic discharge, encapsulation change rate, and small contact resistance can be obtained by applying the composite graphyne to the resistance paste in the process of preparing lead ruthenate by the chemical deposition method.
In example 2, compared with comparative examples 1 and 2, the characteristics of excellent temperature coefficient, electrostatic discharge, encapsulation change rate and small contact resistance can be obtained only by using the graphite alkyne composite lead ruthenate as the conductive phase.
The comparison between the example 2 and the comparative examples 3, 4, 5 and 6 shows that the characteristics of excellent temperature coefficient and small contact resistance can be obtained only by applying the graphite alkyne composite lead ruthenate prepared by the chemical deposition method to resistance paste through freeze drying and vacuum calcination processes.
Example 2 compares with comparative examples 7-14, and shows that, no matter ruthenium dioxide and lead oxide are directly compounded with graphyne, carbon black or graphite, or lead ruthenate is directly compounded with graphyne, carbon black or graphite, the obtained conductive phase can not meet the requirement that the contact resistance is less than 0.3% although good temperature coefficient or electrostatic discharge and encapsulation change rate can be obtained when the obtained conductive phase is used for the resistance paste, and the graphite alkyne composite ruthenate lead material prepared by the chemical deposition method can simultaneously obtain the performance requirements of excellent temperature coefficient, electrostatic discharge, encapsulation change rate and small contact resistance when the obtained conductive phase is applied to the resistance paste.
Claims (7)
1. The low-contact-resistance resistor paste is characterized by comprising the following components in percentage by mass: 15-45% of conductive powder, 20-40% of glass bonding phase, 1-10% of additive and 30-45% of organic carrier;
the conductive powder is graphite alkyne composite lead ruthenate, wherein the mass ratio of the lead ruthenate to the graphite alkyne is 3: 1-5: 1, and the conductive powder is prepared by the following steps:
step 1: dissolving soluble salt of ruthenium in pure water to form Ru3+An ionic solution A; dissolving soluble salt of lead in pure water to form Pb2+An ionic solution B; adding the graphdine into pure water to form a turbid liquid C, wherein the concentration of the graphdine in the turbid liquid C is 5-10 g/L;
step 2: solution A, B as Ru3+With Pb2+Dropwise adding the solution into the suspension C under the stirring condition with the molar ratio of 1:1, stopping stirring after the solution A, B is dropwise added, and standing for 20-24 hours;
and step 3: extracting the upper-layer liquid of the precipitate from the standing solution, adding pure water into the extracted liquid again, stirring for 10-15 minutes, and standing for 20-24 hours;
and 4, step 4: repeating the operation of the step 3 twice, and then carrying out suction filtration and freeze drying on the sediment at the bottom layer;
and 5: calcining the dried substance obtained in the step (4) at 550-600 ℃ for 30-40 minutes in vacuum, and performing breakage ball milling until the particle size is 0.7-1.3 mu m to obtain the graphite alkyne composite lead ruthenate;
the glass bonding phase is lead-boron-silicon glass powder, the softening temperature of the glass bonding phase is 500-600 ℃, and the granularity of the glass bonding phase is 1.0-1.5 mu m.
2. The low contact resistance resistor paste according to claim 1, wherein the soluble salt of ruthenium is any one of ruthenium chloride, ruthenium iodide, ruthenium nitrate and ruthenium acetate.
3. The low contact resistance resistor paste according to claim 1, wherein the soluble salt of lead is any one of lead nitrate and lead acetate.
4. The low contact resistance type resistance paste according to claim 1, wherein the lead-boron-silicon glass powder is prepared from the following components in percentage by mass: 55 to 70 percent of PbO and SiO2 5%～25%、Al2O3 1%～10%、B2O31 to 20 percent and ZnO 5 to 10 percent.
5. The low contact resistance resistor paste according to claim 1, wherein said additive is ZnO, MnO or MnO2、ZrO2A mixture of any two or more of them.
6. The low contact resistance resistor paste according to claim 1, wherein the organic vehicle comprises, in mass percent: 8-15% of resin, 1-5% of organic additive and 80-90% of organic solvent.
7. The low contact resistance type resistor paste according to claim 6, wherein the resin is selected from any one of rosin resin, ethyl cellulose, hydroxy cellulose, and methyl cellulose; the organic solvent is selected from one or more of terpineol, butyl carbitol and butyl carbitol acetate; the organic additive is selected from one or two of lecithin and oleic acid.
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