CN110415859B - Wear-resistant long-life conductive carbon paste - Google Patents
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- CN110415859B CN110415859B CN201910599844.5A CN201910599844A CN110415859B CN 110415859 B CN110415859 B CN 110415859B CN 201910599844 A CN201910599844 A CN 201910599844A CN 110415859 B CN110415859 B CN 110415859B
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- 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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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Abstract
The invention provides wear-resistant long-life conductive carbon paste which comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 18-25% of phenolic resin; 8-12% of epoxy resin; 8-12% of thermosetting acrylic resin; 0.5-1.5% of titanium dioxide; 0.5-1.5% of nano zinc oxide; 8-12% of fumed silica; 0.5-1.5% of defoaming agent; 8-12% of graphene; 8-12% of carbon black; 20-30% of high-boiling-point solvent. The conductive carbon paste provided by the invention has the advantages of long service life, high hardness, excellent wear resistance, small total resistance change rate, small contact noise and excellent electrical stability.
Description
Technical Field
The invention relates to the technical field of conductive carbon paste, in particular to wear-resistant conductive carbon paste with a long service life.
Background
The conductive carbon paste is a viscous substance formed by uniformly distributing particles of a conductive material in a thermoplastic or thermosetting resin. The counter electrode made of the conductive slurry has practical application in the fields of rocker potentiometers, solar batteries, supercapacitors, energy catalysis and the like, and the conductive carbon slurry is generally printed and dried to form a carbon film and is applied. The existing carbon film contains high-content resin, common resin comprises epoxy resin, phenolic resin, thermosetting acrylic resin and the like, the high-content resin causes poor conductivity of the carbon film, and the adhesion among layers in the carbon film is poor, so that the stability of the carbon film is poor.
Disclosure of Invention
In order to solve the problems, the invention provides the wear-resistant long-life conductive carbon paste which is long in service life, high in hardness, excellent in wear resistance, small in total resistance change rate, small in contact noise and excellent in electrical stability.
In order to achieve the purpose, the invention is solved by the following technical scheme:
the wear-resistant long-life conductive carbon paste comprises conductive carbon paste, and the conductive carbon paste is prepared from the following raw materials in percentage by mass: 18-25% of phenolic resin; 8-12% of epoxy resin; 8-12% of thermosetting acrylic resin; 0.5-1.5% of titanium dioxide; 0.5-1.5% of nano zinc oxide; 8-12% of fumed silica; 0.5-1.5% of defoaming agent; 8-12% of graphene; 8-12% of carbon black; 20-30% of high-boiling-point solvent.
Specifically, the conductive carbon paste is prepared from the following raw materials in percentage by mass: 20% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 10% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; 27% of high-boiling point solvent.
Specifically, the particle fineness of the fumed silica is 1000 meshes.
Specifically, the high boiling point solvent is ethylene glycol.
Specifically, the preparation process of the conductive carbon paste comprises the following steps:
s1, weighing the raw materials according to the proportion for later use;
s2, preparing a mixing container, adding phenolic resin, epoxy resin and thermosetting acrylic resin into the mixing container, then adding titanium dioxide and nano zinc oxide, and uniformly mixing in the mixing container;
s3, preparing a stirring device, transferring the uniformly mixed mixture obtained in the step S2 into the stirring device, starting the stirring device, stirring for 10 hours, gradually increasing the temperature of the mixture in the stirring process, and adding a small amount of high-boiling-point solvent when the temperature reaches 38-40 ℃;
s4, adding fumed silica and a defoaming agent, and continuing stirring for 5 hours;
s5, adding graphene and carbon black, and continuously stirring for 2h to obtain a semi-finished slurry;
s6 transferring the semi-finished slurry to a three-roll grinder for grinding for 1 h;
and S7, continuously adding the balance of high-boiling-point solvent, and adjusting the viscosity to 500-800 dpa & S to obtain the conductive carbon paste.
Specifically, the stirring device is a planetary stirrer.
The invention has the beneficial effects that:
the wear-resistant long-life conductive carbon paste disclosed by the invention is suitable for a rocker potentiometer, and has the advantages of long service life, high hardness, excellent wear resistance, small total resistance change rate, small contact noise and excellent electrical stability.
Drawings
Fig. 1 is a schematic view of a preparation process of the wear-resistant long-life conductive carbon paste.
FIG. 2 is a graph showing the results of the pencil hardness test of the conductive carbon pastes obtained in examples 1 to 6 of the present invention.
FIG. 3 is a graph showing the results of testing the product life of the conductive carbon paste obtained in examples 1 to 6 of the present invention.
Fig. 4 is a graph showing the total resistance change rate and the contact noise performance of the conductive carbon paste obtained in example 5 of the present invention.
FIG. 5 is a graph showing the test results of the total resistance change rate and contact noise performance of Japanese rattan-bin FC-403T.
FIG. 6 is a graph showing the test results of the total resistance change rate and contact noise performance of Eschen ED581 SS.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 24% of phenolic resin; 12% of epoxy resin; 12% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 2% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Example 2
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 24% of phenolic resin; 12% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; fumed silica 4%; 1% of defoaming agent; 10% of graphene; 10% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Example 3
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 24% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 6% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Example 4
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 22% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 8% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Example 5
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 20% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 10% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Example 6
The wear-resistant long-life conductive carbon paste comprises conductive carbon paste, wherein the conductive carbon paste is prepared from the following raw materials in percentage by mass: 18% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 12% of fumed silica; 1% of defoaming agent; 10% of graphene; 12% of carbon black; and 27% of ethylene glycol.
Preferably, the particle fineness of the fumed silica is 1000 meshes, the fineness of the fumed silica is small, and after the product is prepared, the fumed silica is dispersively filled in the resin, so that the wear resistance of the product can be further improved.
Preferably, the defoaming agent is silicone emulsion, so as to eliminate bubbles generated in the stirring process and avoid influence on the electrical properties of the conductive carbon paste caused by excessive small bubbles in the conductive carbon paste.
Preparing conductive carbon paste:
as shown in fig. 1, the raw materials of the above examples 1 to 6 were prepared separately, and the preparation process thereof included the following steps:
s1, weighing the raw materials according to the proportion for later use;
s2, preparing a mixing container, adding phenolic resin, epoxy resin and thermosetting acrylic resin into the mixing container, then adding titanium dioxide and nano zinc oxide, and uniformly mixing in the mixing container;
s3, preparing a planetary stirrer, transferring the uniformly mixed mixture obtained in the step S2 into the planetary stirrer, starting the planetary stirrer, stirring for 10 hours, gradually increasing the temperature of the mixture in the stirring process, and adding a small amount of high-boiling-point solvent when the temperature reaches 38 ℃;
s4, adding fumed silica and a defoaming agent, and continuing stirring for 5 hours;
s5, adding graphene and carbon black, and continuously stirring for 2h to obtain a semi-finished slurry;
s6 transferring the semi-finished slurry to a three-roll grinder for grinding for 1 h;
and S7, continuously adding the balance of high-boiling-point solvent, and adjusting the viscosity to 600dpa & S to obtain the conductive carbon paste.
Testing one:
the conductive carbon paste prepared in the above examples 1 to 6 was printed to form a carbon film resistor disc, and then the carbon film resistor disc and other parts were assembled to form a rocker potentiometer, the type of which was referred to FJ06K rocker potentiometer provided by yokko gmbh, and the rocker potentiometer was subjected to a pencil hardness test and a rotational life test (wear resistance times), wherein a rotational life tester was used for the rotational life test, and the test results were shown in fig. 2 to 3.
As can be seen from the data in the graph of fig. 2, as the percentage of fumed silica increases, the hardness of the carbon film resistor disc gradually increases, and when the percentage of fumed silica exceeds 10%, the hardness of the carbon film resistor disc does not increase any more, so that, in consideration of the comprehensive cost, 10% of fumed silica is the optimal value of the index;
from the data of the graph in fig. 3, it is found that the service life of the carbon film resistor disc gradually increases with the increase of the percentage of the fumed silica, the peak value is reached when the percentage of the fumed silica reaches 10%, and the service life of the carbon film resistor disc begins to decrease after the percentage of the fumed silica exceeds 10%, so that the percentage of the fumed silica of 10% is the optimal value of the index.
It can be concluded from fig. 2 and 3 that, when the percentage of fumed silica in the conductive carbon paste is 10%, the hardness is the highest, and the service life is the longest, so that example 5 is the most preferable example.
For further comparison, the conductive carbon paste of the present invention has longer service life and higher hardness, and two comparative examples are added, wherein comparative example 1 is a carbon film resistor printed by using the conductive carbon paste of Japan rattan house FC-403T, and comparative example 2 is a carbon film resistor printed by using the conductive carbon paste of American Eschen ED581SS, and the conductive carbon paste is also made into a rocker potentiometer in the same manner as described above, and the rocker hardness test and the rotation life test are performed, and the test results are shown in the following table 1.
TABLE 1 results of the Pencil hardness test and the spin life test of comparative examples 1 to 2 and examples 1 to 6
Table 1 above, wherein C represents fumed silica and "+ 2% C" represents example 1 containing 2% fumed silica.
As can be seen from the data in the table 1, the service life of the carbon film resistor sheet printed by using the conductive carbon paste of the Japan rattan storehouse FC-403T is 40 ten thousand times, and the service life of the carbon film resistor sheet printed by using the conductive carbon paste of the American Equisson ED581SS is 80 ten thousand times, but the conductive carbon paste of the application can reach 150 ten thousand times when the addition amount of the fumed silica reaches 6 percent, has the service life performance far superior to that of the conductive carbon paste of the Japan rattan storehouse FC-403T and that of the American Equisson ED581SS, can reach 290 ten thousand times at most, and is longer.
Similarly, the carbon film resistor sheet is printed by using the conductive carbon paste of Japan rattan storehouse FC-403T and the conductive carbon paste of America Eichsen ED581SS, and the hardness tests are all 7H, while in the application, in example 5, when the addition amount of the fumed silica is 10%, the hardness standard of 8H can be reached, and the hardness is obviously improved.
And (2) testing:
in order to investigate the electrical properties of the conductive carbon paste of example 5, the following tests were performed.
The conductive carbon paste prepared in the above example 5 was printed to form a carbon film resistor sheet, and then the carbon film resistor sheet and other parts were assembled to form a rocker potentiometer, the type of which was referred to FJ06K rocker potentiometer provided by yokko gmbh, and the rocker potentiometer was subjected to the full resistance change rate [ (post-test product resistance-original product resistance)/original product resistance ] and the contact noise test, wherein the contact noise test used a contact noise tester, the test results obtained are shown in fig. 4, the full resistance change rate and the contact noise in fig. 4 were respectively subjected to 2 parallel tests, and the difference between the 2 parallel tests was not large, indicating that the electrical properties thereof were stable.
Referring to fig. 4, firstly, the total resistance change rate is evaluated, the abscissa is the service life of the product, the ordinate is the total resistance change rate, the total resistance change rate is in an increasing trend along with the increase of the service life of the conductive carbon paste, and when the service life of the conductive carbon paste reaches 290 ten thousand times, the total resistance change rate is still lower than 15%;
for the contact noise test, the abscissa is the service life of the product, the ordinate is the contact noise, the total resistance change rate is in an increasing trend along with the increase of the service life of the conductive carbon paste, and when the service life of the conductive carbon paste reaches 290 ten thousand times, the total resistance change rate is still lower than 20%.
For further comparison, the conductive carbon paste of the present invention has a smaller total resistance change rate and a smaller contact noise, and two comparative examples are added, wherein comparative example 1 is a carbon film resistor printed by using the conductive carbon paste of japan rattan house FC-403T, comparative example 2 is a carbon film resistor printed by using the conductive carbon paste of american egkson ED581SS, a rocker potentiometer is also fabricated in the same manner as described above, and the test results of the total resistance change rate [ (product resistance after test-original product resistance)/original product resistance ] and the contact noise are tested, and are shown in fig. 5 to 6.
FIG. 5 is a test result chart of Japanese rattan storehouse FC-403T, the total resistance change rate and the contact noise are respectively tested for 2 times in parallel, in the 2 times of parallel tests, the total resistance change rate test is successful once and fails once, the success rate is 50%, the electrical property is unstable, and the successful test curve is an increasing curve; the contact noise was successfully tested twice.
For the full-resistance change rate test, taking a successful test curve as an example, when the service life of the full-resistance change rate test reaches 40 ten thousand times, the full-resistance change rate reaches 14.04 percent, along with the increment of the service life, and when the service life reaches 80 ten thousand times, the full-resistance change rate reaches 23.12 percent, which indicates that the electrical property of the full-resistance change rate test is unstable;
for the contact noise test, at the stage of 0-80 ten thousand service lives, the contact noise is lower than 15%, and the performance is relatively stable.
Fig. 6 is a test result graph of the ericsson ED581SS in the united states, in which the total resistance change rate and the contact noise are respectively tested in parallel for 2 times, and in the 2 parallel tests, the total resistance change rate test is successful once and failed once, the success rate is 50%, which indicates that the electrical performance is unstable, and the successful test curve is an increasing curve; the contact noise was successfully tested twice.
For the full-resistance change rate test, taking a successful test curve as an example, when the service life of the full-resistance change rate test reaches 80 ten thousand times, the full-resistance change rate of the full-resistance change rate test reaches 14.65 percent, along with the increment of the service life, and when the service life of the full-resistance change rate test reaches 110 ten thousand times, the full-resistance change rate of the full-resistance change rate test reaches 19.44 percent, which indicates that the electrical property of the full-resistance change rate test;
for the contact noise test, when the service life is 0-100 ten thousand times, the contact noise is lower than 20%, before the service life is 100 ten thousand times, the contact noise is relatively stable, but when the service life exceeds 100 ten thousand times, the contact noise is 27%, and the normal work of the rocker positioner is seriously influenced.
The above examples only show 6 embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. The wear-resistant long-life conductive carbon paste comprises conductive carbon paste and is characterized in that the conductive carbon paste is prepared from the following raw materials in percentage by mass: 20% of phenolic resin; 10% of epoxy resin; 10% of thermosetting acrylic resin; 1% of titanium dioxide; 1% of nano zinc oxide; 10% of fumed silica; 1% of defoaming agent; 10% of graphene; 10% of carbon black; 27% of high-boiling point solvent.
2. The wear-resistant long-life conductive carbon paste as claimed in claim 1, wherein the fumed silica has a particle fineness of 1000 mesh.
3. The wear-resistant long-life conductive carbon paste as claimed in claim 1, wherein the high-boiling point solvent is ethylene glycol.
4. The wear-resistant long-life conductive carbon paste as claimed in claim 1, wherein the conductive carbon paste is prepared by the following steps:
s1, weighing the raw materials according to the proportion for later use;
s2, preparing a mixing container, adding phenolic resin, epoxy resin and thermosetting acrylic resin into the mixing container, then adding titanium dioxide and nano zinc oxide, and uniformly mixing in the mixing container;
s3, preparing a stirring device, transferring the uniformly mixed mixture obtained in the step S2 into the stirring device, starting the stirring device, stirring for 10 hours, gradually increasing the temperature of the mixture in the stirring process, and adding a small amount of high-boiling-point solvent when the temperature reaches 38-40 ℃;
s4, adding fumed silica and a defoaming agent, and continuing stirring for 5 hours;
s5, adding graphene and carbon black, and continuously stirring for 2h to obtain a semi-finished slurry;
s6 transferring the semi-finished slurry to a three-roll grinder for grinding for 1 h;
and S7, continuously adding the balance of high-boiling-point solvent, and adjusting the viscosity to 500-800 dpa & S to obtain the conductive carbon paste.
5. The wear-resistant long-life conductive carbon paste as claimed in claim 4, wherein the stirring device is a planetary stirrer.
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| US7105200B2 (en) * | 2001-09-10 | 2006-09-12 | Noritake Co., Limited | Method of producing thick-film sheet member |
| CN101974266B (en) * | 2010-09-30 | 2012-09-19 | 彩虹集团公司 | Low-temperature conductive carbon slurry and preparation method thereof |
| CN104231919B (en) * | 2014-10-15 | 2017-01-18 | 大连海事大学 | Nanometer reinforced, non-transition-layer, organosilicone and low-surface-energy type antifouling paint and preparation method thereof |
| CN104464883B (en) * | 2014-12-26 | 2017-02-22 | 苏州格瑞丰纳米科技有限公司 | Graphene electrocondution slurry with dispersants adsorbed on surface and manufacturing method and application thereof |
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| CN107682943B (en) * | 2017-09-20 | 2020-09-22 | 中国科学院山西煤炭化学研究所 | Multifunctional graphene electric heating slurry, multifunctional electric heating film prepared from multifunctional graphene electric heating slurry, preparation method and application |
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