CN115376769A - Carbon composite ceramic resistance card and preparation method and application thereof - Google Patents
Carbon composite ceramic resistance card and preparation method and application thereof Download PDFInfo
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- CN115376769A CN115376769A CN202211058319.0A CN202211058319A CN115376769A CN 115376769 A CN115376769 A CN 115376769A CN 202211058319 A CN202211058319 A CN 202211058319A CN 115376769 A CN115376769 A CN 115376769A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 23
- 239000011230 binding agent Substances 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000003989 dielectric material Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 239000011812 mixed powder Substances 0.000 claims description 17
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 16
- 229930006000 Sucrose Natural products 0.000 claims description 16
- 239000005720 sucrose Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 229910052661 anorthite Inorganic materials 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 238000005488 sandblasting Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920001732 Lignosulfonate Polymers 0.000 claims description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000011065 in-situ storage Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 2
- 229930091371 Fructose Natural products 0.000 claims description 2
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 2
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002772 monosaccharides Chemical class 0.000 claims description 2
- 229920001542 oligosaccharide Polymers 0.000 claims description 2
- 150000002482 oligosaccharides Chemical class 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052596 spinel Inorganic materials 0.000 abstract description 7
- 239000011029 spinel Substances 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 47
- 230000000052 comparative effect Effects 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 229910052878 cordierite Inorganic materials 0.000 description 8
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 239000002734 clay mineral Substances 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 229910052634 enstatite Inorganic materials 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- BBCCCLINBSELLX-UHFFFAOYSA-N magnesium;dihydroxy(oxo)silane Chemical compound [Mg+2].O[Si](O)=O BBCCCLINBSELLX-UHFFFAOYSA-N 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 235000012222 talc Nutrition 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
-
- 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
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- 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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Electromagnetism (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a carbon composite ceramic resistance card and a preparation method and application thereof. According to the carbon composite ceramic resistance card provided by the invention, the dielectric phase and the conductive phase are distributed in a bicontinuous mode, the conductive phase is uniformly distributed in the carbon composite ceramic resistance card in the dielectric phase, the phase analysis shows that no spinel phase exists, and the electrical property and the mechanical property meet the use requirements.
Description
Technical Field
The invention belongs to the technical field of power electronics and power transmission and transformation, and relates to a carbon composite ceramic resistance card and a preparation method and application thereof.
Background
The carbon composite resistor has the characteristics of large open-capacitance flow, stable resistance value, good thermal stability and the like, can resist large current and impact, and meets the use requirements under the working conditions of high temperature, high frequency, high power and the like. And the electrodes are manufactured at two ends of the carbon composite ceramic resistor disc by adopting an aluminum spraying process, and when the carbon composite ceramic resistor disc is assembled with the insulating support, the insulating support presses the electrodes to form the carbon composite resistor. The performance of the carbon composite resistor depends on the performance of the carbon composite ceramic resistor sheet.
Carbon composite ceramic resistance cards are generally made by mixing, pressing and molding dielectric phase ceramic powder (such as alumina and its binder phase) and conductive phase carbon (such as carbon black, graphite, graphitized carbon, etc.) and then performing heat treatment. In the resistance card prepared by the formula and the method, the distribution state of carbon is often relatively isolated, the concentration and the mobility of current carriers in materials are seriously influenced, and finally the conductive capability of the resistance card is unstable. The unstable conductivity means that the resistivity of the resistance chip has large dispersity, and when the resistance chip is subjected to large pulse energy, the resistor cannot absorb the energy in time and uniformly disperse the energy to discharge the energy periodically, so that the rapid cooling is realized, and the resistance chip fails.
Disclosure of Invention
The invention aims to provide a carbon composite ceramic resistance card and a preparation method and application thereof.
The carbon composite ceramic resistance card provided by the invention is obtained by mixing and molding a conductive phase and a dielectric phase; wherein the conductive phase is uniformly distributed in the dielectric phase;
the conductive phase is generated in situ by an organic carbon source;
the dielectric phase is made of a dielectric material and a binder.
In the carbon composite ceramic resistance card, the organic carbon source is at least one of sucrose, fructose, glucose, lignosulfonate, naphthalenesulfonate-formaldehyde condensate salt, monosaccharide, oligosaccharide, water-soluble starch and water-soluble cellulose derivative;
the dielectric material is at least one of aluminum oxide, zinc oxide and magnesium oxide; the alumina is specifically gamma-alumina;
the average grain diameter of the alumina is 5-15 μm; in particular 8-12 μm; after the gamma-alumina is subjected to heat treatment, crystal grains are mostly flaky or platy, and are favorably connected with other components in the composite material to form a continuous structure;
the binder is at least one of metakaolin, talcum powder, anorthite, lignosulfonate, naphthalene sulfonate-formaldehyde condensate salt, water-soluble starch and water-soluble cellulose derivative;
the lignosulfonate is specifically calcium lignosulfonate or sodium lignosulfonate;
the particle size of the metakaolin is 4-8 μm; in particular 5 μm;
in the mixture of the metakaolin and the talcum powder, the molar ratio of magnesium to silicon is 1;
the proportion can ensure that magnesium and silicon form a high-temperature bonding phase cordierite phase in the sintered material, and the bonding and reinforcing effects are achieved on the composite material.
The mass ratio of the metakaolin to the anorthite is 4:1.
when the proportion is too small or too large, complex mesophase compounds are easily formed, and the mesophase compounds are basically brittle, so that the performance of the composite material is not improved.
The mass percentage of the organic carbon source in the mixture of the organic carbon source, the dielectric material and the binder is 12-15%; specifically 12.6 to 13 percent; the mass of the organic carbon source is calculated by a pure organic carbon source and is not calculated by the total mass of the aqueous solution in the preparation process;
the dielectric material accounts for 70-78% of the mass of the mixture consisting of the organic carbon source, the dielectric material and the binder; in particular 75-77%;
the mass percentage of the binder in the mixture of the organic carbon source, the dielectric material and the binder is 10-15%; in particular 10.5-12%.
The carbon composite ceramic resistance card is of a porous structure, and the aperture is 1-10 mu m;
the porosity is 20-30%; specifically 24.98%, 25.02 or 26.22%.
The invention adopts an organic carbon source to generate a conductive phase in situ (the grain diameter of the phase generated in situ is more uniform and the phase is more uniformly distributed in the composite material), and a bonding system is introduced in a clay mineral mode (the conventional method adopts the direct configuration of various substances, such as a ternary sintering aid MgO-CaO-SiO) 2 Respectively weighing pure oxides of MgO, caO and SiO 2 Mixed formulation of metakaolin Al 2 O 3 ·2SiO 2 Talc powder 3 MgO.4SiO 2 ·H 2 O and anorthite CaO & Al 2 O 3 ·2SiO 2 As the raw material is prepared into a bonding system, because a small amount of low-melting-point impurity components exist in the clay phase, the low-melting-point impurity components are easy to form a liquid phase at high temperature, and Al 3+ And Mg 2+ The diffusion speed is higher, the diffusion nucleation rate of cordierite is favorably improved, and compared with a common ternary sintering auxiliary agent, the composite material has multiple components and a clay phase which is formed by the multiple components and is dissolved in a segmented mode, namely the clay phase has higher capacity of forming a liquid phase, the generation of mesophase spinel can be effectively avoided, the decomposition of the generated mesophase spinel can be promoted, and the ceramic compactness is better promoted. ) The carbon composite ceramic resistance card with the dielectric phase and the conductive phase distributed in a bicontinuous mode and the conductive phase uniformly distributed in the dielectric phase is prepared.
Specifically, the method for preparing the carbon composite ceramic resistance card provided by the invention comprises the following steps:
1) Mixing the binder according to the proportion to obtain mixed powder A;
2) Mixing the mixed powder A, the dielectric material and the organic carbon source according to the proportion to obtain a mixed solution B;
or,
preparing an organic carbon source solution a by taking 2-5% of the total mass of the organic carbon source;
mixing the rest organic carbon source with the mixed powder A and the dielectric material according to a ratio to obtain a mixed solution B1;
mixing the organic carbon source solution a with the mixed solution B1 to obtain a mixed solution B2;
3) Drying, sieving and vacuum drying the mixed solution B or the mixed solution B2 to obtain mixed powder, and pressing to obtain a formed body green body;
4) And sequentially carrying out glue removal and sintering on the green molded body blank to obtain the carbon composite ceramic resistance card.
In step 1) of the above method, a clay mineral (metakaolin Al) 2 O 3 ·2SiO 2 (the clay mineral used as a binder is more active than general calcined kaolin, having a particle size of 5 μm); talc powder 3MgO 4SiO 2 ·H 2 O and anorthite CaO. Al 2 O 3 ·2SiO 2 Compared with the main component of alumina (about 2000 ℃), the anorthite has lower melting temperature (1250-1550 ℃), can promote the mutual permeation among the components during sintering so as to accelerate the formation of mullite, and can effectively avoid SiO when the anorthite is melted, so that the viscosity of reactants is increased (from the thermodynamic point of view) 2 The carbon black can react with partial conductive carbon black at high temperature to generate partial SiC to form a spinel phase (which deteriorates the performance of the composite material), so that the product is a cordierite phase; after the anorthite is melted, the anorthite is filled among crystal grains of mullite and/or cordierite, so that the mechanical property and the electrical property of the composite material can be improved.
In the mixing step, the mixing method is ball milling; specifically, the rotating speed is 350r/min in the ball milling process; the time is 30-60min;
in the step 2), in the mixing step, the mixing method is ball milling; specifically, in the ball milling, the rotating speed is 250r/min; the time is 30-60min;
in the mixed solution B, the organic carbon source exists in the form of aqueous solution;
in the organic carbon source solution a, the mass percentage concentration of the organic carbon source is 10-15%;
the mode of mixing the organic carbon source twice is adopted, so that the raw materials can be uniformly mixed. Since the density of sucrose is greatly different from the densities of alumina powder and clay mineral, uniform mixing is difficult when the materials are completely dry-mixed. In the invention, the sucrose solution can also replace PVA as a binder, wherein the binder is a low-temperature binder for powder and is burnt out in the heat treatment process; the bonding system referred to above is one in which a liquid phase high temperature bonding agent is formed under heat treatment to form part of the final product.
In the drying step in the step 3), drying is carried out until the water content is 2-5wt%; the temperature is 160 ℃; the time is 10h;
in the sieving step, the mesh number of the sieve pores is 80-120; in particular to 100 meshes;
in the vacuum drying step, the temperature is 140-180 ℃; in particular to 160 ℃; the time is 1-3h; in particular for 2h;
in the pressing step, the pressure is 3MPa; the time is 60-180s; specifically 120s;
the step 4) of glue discharging comprises the following steps: firstly, putting the green compact into a vacuum furnace, sealing a furnace door, vacuumizing until the vacuum degree of the furnace is less than or equal to 9Pa, filling 60Pa nitrogen or argon for atmosphere replacement, repeating for 2-4 times, starting to heat according to a glue discharging curve, and filling enough argon while vacuumizing to keep 15KPa argon continuously flowing in the furnace;
the rubber discharge curve is as follows: raising the temperature of room temperature to 160 ℃ at a heating rate of 1 ℃/min, preserving heat at 160 ℃ for 2h, raising the temperature of 160 ℃ to 800 ℃ at 20 ℃/min, raising the temperature of 800 ℃ to 1200 ℃ at 10 ℃/min, raising the temperature of 1200 ℃ to 1450 ℃ at 5 ℃/min, preserving heat at 1450 ℃ for 2h, reducing the temperature of 1450 ℃ to 800 ℃ at 10 ℃/min, and reducing the temperature below 800 ℃ along with the furnace;
in the sintering step, the sintering atmosphere is inert atmosphere; the sintering temperature is 1400-1480 ℃; specifically 1450 ℃; the time is 1-3h; in particular 2h; the pressure of the inert atmosphere is 12-18KPa; specifically 15KPa.
The method further comprises the following steps: after the step 4), naturally cooling the ceramic wafer obtained by sintering at the temperature of less than 800 ℃, spraying sand, and spraying an electrode layer;
in the sand blasting step, the sand blasting thickness is 1-1.5mm.
In addition, the resistor containing the carbon composite ceramic resistor disc and the application of the carbon composite ceramic resistor disc in the preparation of the resistor also belong to the protection scope of the invention. Specifically, the resistor is a carbon composite resistor.
According to the carbon composite ceramic resistance card provided by the invention, the dielectric phase and the conductive phase are distributed in a bicontinuous mode, the conductive phase is uniformly distributed in the carbon composite ceramic resistance card in the dielectric phase, the phase analysis shows that no spinel phase exists, and the electrical property and the mechanical property meet the use requirements.
Drawings
FIG. 1 is a graph of the binder removal curve of example 1.
Fig. 2 is an SEM result of the carbon composite ceramic resistor sheet obtained in example 1.
Fig. 3 is a polarized light microstructure of the carbon composite ceramic resistor sheet obtained in example 1.
Fig. 4 shows the sheet resistance of the carbon composite ceramic resistor sheet obtained in example 1.
Fig. 5 shows the sheet resistivity of the carbon composite ceramic resistor sheet obtained in example 1.
Fig. 6 is a practical diagram of the resistor sheet of the embodiment 1.
Fig. 7 shows the polarizing microstructure of the carbon composite ceramic resistor sheet obtained in example 2.
Fig. 8 is an XRD of the carbon composite ceramic resistance card obtained in example 2.
Fig. 9 is an SEM result of the carbon composite ceramic resistor sheet obtained in example 2.
Fig. 10 is a practical diagram of the resistor disc of example 2.
Fig. 11 is a micro-topography of the resistor disc obtained in example 3, the left image is a polarization microstructure, and the right image is an SEM result.
Fig. 12 is an XRD of the resistive sheet obtained in comparative example 1.
Fig. 13 is a practical use picture of the resistance card of the comparative example 1.
FIG. 14 is an electron micrograph of a comparative example.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
1) Accurate scaleMetakaolin in an amount of 3.75mol (i.e. 923.175 g), 1mol of talc, the mole ratio of magnesium to silicon in the mixture of metakaolin and talc being 1:3.8 cordierite phase 2 MgO.2Al 2 O 3 5Si (Mg: si molar ratio of 1: 2.5), wherein Si is excessive, the formation of an enstatite crystal phase is avoided, if the content of magnesium is excessive, more enstatite crystal phases can be doped in the generated cordierite phase, the thermal expansion coefficient of cordierite is increased, and the performance of carbon resistance is deteriorated, 230g of anorthite is put into a high-energy planetary ball mill, the rotating speed is 350r/min, and the ball milling is carried out for 60min, so that mixed powder A is obtained;
2) Weighing 866g of a 15% sucrose solution, 129.9g of sucrose as an organic carbon source, 120g of the mixed powder A and 750g of gamma-alumina, and performing secondary ball milling by planetary ball milling at a rotating speed of 250r/min for 60min to obtain a mixed solution B.
In the mixed solution B, the mass percentage of sucrose in a mixture consisting of organic carbon source sucrose, adhesive mixed powder A and dielectric material gamma-alumina is 13%;
the dielectric material gamma-alumina accounts for 75 percent of the mass of the mixture consisting of the organic carbon source sucrose, the adhesive mixed powder A and the dielectric material gamma-alumina;
the mass percentage of the binder mixed powder A in the mixture composed of the organic carbon source sucrose, the binder mixed powder A and the dielectric material gamma-alumina is 12%.
3) Keeping the temperature of the mixed solution B in an oven at 160 ℃ for 10h, drying, sieving by a 100-mesh sieve to obtain mixed powder, and pressing for 1-2min under the pressure of 3MPa to obtain a green body of a formed body;
4) Putting the green compact obtained in the step 3) into a vacuum furnace, closing a furnace door, vacuumizing until the vacuum degree of the furnace is less than or equal to 9Pa, filling 60Pa nitrogen or argon for atmosphere replacement, and repeating for 2-4 times to avoid air residue; heating according to a glue discharging curve, and filling sufficient argon while vacuumizing to keep the continuous circulation of 15KPa argon in the furnace;
the step can remove the moisture in the green body, is beneficial to subsequent vacuumizing, and also prevents the organic carbon sucrose from being directly burned out by water gas.
The rubber discharge curve is as follows: heating the room temperature to 160 ℃ at a heating rate of 1 ℃/min, keeping the temperature at 160 ℃ for 2h, heating the temperature at 160 ℃ to 800 ℃ at 20 ℃/min, heating the temperature at 800 ℃ to 1200 ℃ at 10 ℃/min, heating the temperature at 1200 ℃ to 1450 ℃ at 5 ℃/min, keeping the temperature at 1450 ℃ for 2h, cooling the temperature at 1450 ℃ to 800 ℃ at 10 ℃/min, and cooling the temperature below 800 ℃ with a furnace to obtain a ceramic wafer; the temperature profile is shown in figure 1.
And sintering the green body for 2h at 1450 ℃ under the protection of inert (such as argon) gas, wherein the pressure of argon atmosphere is 15KPa, and obtaining the resistance card.
5) Performing sand blasting treatment on two end surfaces of the ceramic chip, wherein the sand blasting thickness is 1-1.5mm; and spraying an electrode layer (Cu) on the end surface subjected to sand blasting, welding an extraction electrode from the electrode layer, and assembling the extraction electrode and the insulating support together to obtain the carbon composite ceramic resistance card.
The resulting SEM of this example shows the microstructure shown in FIG. 2. As can be seen from the figure, the carbon composite ceramic resistance chip obtained in example 1 has a porous structure and a pore diameter in the range of 1 to 10 μm. The alumina phase is a continuous phase, the sintering condition is good, the grain boundary is obvious, the porosity of the continuous phase is low, and the densification degree is high. The conductive phase is uniformly distributed in the alumina matrix in the form of nano particles, is basically in a continuous state and has good dispersibility.
As is clear from the polarizing microstructure shown in FIG. 3, the alumina phase is a lamellar self-shape crystal with a good crystal morphology, and the crystal grain size is distributed between 1 to 20 μm. The alumina grains are mostly connected together in the form of a plate or a plate, which is related to the gamma-alumina used.
The Vickers hardness of the carbon composite ceramic resistance card is tested by adopting a digital display microhardness machine HV-1000, and the results are shown in Table 1. As can be seen from Table 1, the difference between the maximum value 116.2 and the minimum values 100.9, 110.5, 112.2 and 107.7 is small, and the uniformity is very excellent for the composite resistive sheet.
TABLE 1 Vickers hardness of carbon composite ceramic resistance card
| 1 | 2 | 3 | 4 | 5 | Average | |
| HV | 110.5 | 112.2 | 107.7 | 100.9 | 116.2 | 109.5 |
The sheet resistivity and sheet resistance of the carbon composite ceramic resistive sheet were analyzed using a four-probe micro-resistance meter digital display bridge QJ84A (portable) test (as shown in fig. 4 and 5 and table 2). From the analysis of the results, the resistivity of the material is 12 omega cm, the square resistance is 25.3 omega/□, and the material shows good resistance uniformity.
TABLE 2 sheet resistance change of the carbon composite ceramic resistor chip
| Maximum of | Minimum size | Average | Maximum percentage change | Radial non-uniformity | Mean percent change |
| 0.27 | 0.24 | 0.253 | 12.50％ | 11.76％ | 2.00％ |
From the above results, it is understood that the carbon composite ceramic resistor sheet provided in example 1 of the present invention has excellent resistance uniformity, and pulse energy can be uniformly dispersed in the resistor body. From the data of this embodiment, the resistance is uniform, the pulse energy can be diffused in the resistor sheet, the heat dissipation is uniform, the "bulge" phenomenon due to the heat accumulation does not occur during the actual use, and the surface of the product is smooth, as shown in fig. 6.
Example 2
The difference compared to example 1 is in step 2).
Taking 6.5g of sucrose solution with the total mass of 130g, adding the rest 123.5g of sucrose solution with the total mass of 10% into the mixed powder A in the form of sucrose particles, mixing in a dry mixing mode to obtain a mixed solution B1, and then pouring the 10% sucrose solution into the mixed solution B1 to obtain a mixed solution B2.
The mixed solution B used in the step 3) of the embodiment 1 is replaced by the mixed solution B2 obtained in the embodiment, and the step 3) and the subsequent steps are carried out to obtain the carbon composite ceramic resistance card provided by the invention.
As is clear from the results of the polarization microscope shown in FIG. 7, the material is heterogeneous and exhibits significant anisotropy and polychromism. The alumina phase is a flaky self-shape crystal with good crystal morphology, and the grain size distribution is between 1 and 10 mu m, which is similar to that of the embodiment 1.
From XRD shown in FIG. 8, no silicon carbide was formed, and the conductive phase was a graphite phase, and had a distinct characteristic peak at 26 ° (PDF # 65-6212).
Fig. 9 is an SEM result of the carbon composite ceramic resistor sheet obtained in example 2. As can be seen, the product obtained in this example is a bicontinuous composite of graphitized carbon (containing graphite) and alumina ceramic.
The Vickers hardness of the resistive sheet obtained in this example is shown in Table 2.
TABLE 2 Vickers hardness of carbon composite ceramic resistance card
| 1 | 2 | 3 | 4 | 5 | Average | |
| HV | 113.6 | 109.39 | 116.1 | 102.05 | 108.38 | 109.904 |
As can be seen from table 2, the uniformity of the composite resistive sheet was very excellent.
The resistivity of the carbon composite ceramic resistance chip is the result of three times of measurement by using a four-probe micro-resistance measuring instrument to digitally display a bridge QJ84A, and is respectively 36.1, 32.9 and 34.2 omega cm, and the average value is 34.4 omega cm. The amplitude of the variation is small.
After the resistance card obtained in the embodiment is in service, the surface of the product has no trace of arc flash, and the smoothness is kept. As shown in fig. 10.
Example 3
The difference compared to example 1 is in step 2).
Weighing 800g of 15% sucrose solution, 100g of the mixed powder A and 730g of gamma-alumina, and performing planetary ball milling twice at a rotation speed of 250r/min for 60min to obtain a mixed solution B.
As shown in fig. 11, a polarization microscope and SEM scanning microscope image of the resistive sheet obtained in this example is shown. As can be seen, the conductive phase C is uniformly distributed in the dielectric phase, and a network structure is formed between the two phases.
TABLE 3 Vickers hardness of carbon composite ceramic resistance card
| 1 | 2 | 3 | 4 | 5 | Average | |
| HV | 42.38 | 40.93 | 41.61 | 42.05 | 48.38 | 43.07 |
As can be seen from table 2, the uniformity of the composite resistive sheet was very excellent.
The square resistance of the carbon composite ceramic resistance chip is 74.3 omega/□.
Comparative example 1
According to the procedure of example 1, only anorthite used in 1 was replaced with calcium carbonate, and the XRD and SEM of the obtained resistive card are shown in FIG. 6 and 7, respectively. As can be seen from the figure, the resistor disc has no cordierite phase and also has a spinel phase, and the spinel phase is not beneficial to improving the mechanical property of the material.
The hardness is a characterization mode of mechanical properties, and the general hardness can be used for representing the mechanical properties such as tensile strength, impact toughness and the like.
The resistance card obtained in the comparative example was tested using a digital display microhardness tester HV-1000, and the results are shown in Table 3.
Vickers hardness of the resistance card obtained in Table 3 and comparative example 1
| 1 | 2 | 3 | 4 | 5 | Average out | |
| HV | 15.2 | 14.8 | 17.9 | 16.3 | 19.2 | 16.68 |
As is apparent from Table 3, the Vickers hardness of 16.68 in comparative example 1 is very small compared to that of 109.5HV in example 1.
Table 4 change in resistivity of the resistive sheet obtained in comparative example 1
As can be seen from Table 4, the resistance sheets obtained in this comparative example had a large fluctuation range in resistivity and had poor resistance uniformity. The surface of the product after use had craters formed by arc ablation, as shown in fig. 13. FIG. 14 is an electron micrograph of a comparative example. As can be seen from the figure, the long-sized product of the comparative example was silicon carbide whisker. The existence of whiskers deteriorates the performance of the composite material, while avoiding the formation of silicon carbide whiskers, which is the reason why clay minerals are used instead of general binders in the present invention.
Claims (10)
1. A carbon composite ceramic resistance card is obtained by mixing and molding a conductive phase and a dielectric phase; the method is characterized in that: the conductive phase is uniformly distributed in the dielectric phase;
the conductive phase is generated in situ by an organic carbon source;
the dielectric phase is made of a dielectric material and a binder.
2. The carbon composite ceramic resistor sheet of claim 1, wherein: the organic carbon source is at least one of sucrose, fructose, glucose, lignosulfonate, naphthalene sulfonate-formaldehyde condensate salt, water-soluble starch and water-soluble cellulose derivative;
the dielectric material is at least one of aluminum oxide, zinc oxide and magnesium oxide; the alumina is specifically gamma-alumina;
the average grain diameter of the alumina is 5-15 μm; in particular 8-12 μm;
the binder is at least one of metakaolin, talcum powder, anorthite, lignosulfonate, naphthalenesulfonate-formaldehyde condensate salt, monosaccharide, oligosaccharide, water-soluble starch and water-soluble cellulose derivative;
the lignosulfonate is specifically calcium lignosulfonate or sodium lignosulfonate;
the particle size of the metakaolin is 4-8 μm; specifically 5 μm;
in the mixture of the metakaolin and the talcum powder, the molar ratio of magnesium to silicon is 1;
the mass ratio of the metakaolin to the anorthite is 4:1.
3. the carbon composite ceramic resistor sheet according to claim 1 or 2, wherein: the mass percentage of the organic carbon source in the mixture of the organic carbon source, the dielectric material and the binder is 12-15%; specifically 12.6 to 13 percent;
the dielectric material accounts for 70-78% of the mass of the mixture consisting of the organic carbon source, the dielectric material and the binder; in particular 75-77%;
the mass percentage of the binder in the mixture of the organic carbon source, the dielectric material and the binder is 10-15%; in particular 10.5-12%.
4. The carbon composite ceramic resistor sheet according to any one of claims 1 to 3, wherein: the carbon composite ceramic resistance card is of a porous structure, and the aperture is 1-10 mu m;
the porosity is 20-30%; specifically 24.98%, 25.02 or 26.22%.
5. A method for preparing the carbon composite ceramic resistor disc of any one of claims 1 to 4, comprising the following steps:
1) Mixing the binder of claims 1-4 according to the proportion to obtain mixed powder A;
2) Mixing the mixed powder A, the dielectric material and the organic carbon source according to the proportion to obtain a mixed solution B;
or,
preparing an organic carbon source solution a by taking 2-5% of the total mass of the organic carbon source;
mixing the residual organic carbon source with the mixed powder A and the dielectric material according to a ratio to obtain a mixed solution B1;
mixing the organic carbon source solution a with the mixed solution B1 to obtain a mixed solution B2;
3) Drying, sieving and vacuum drying the mixed solution B or the mixed solution B2 to obtain mixed powder, and pressing to obtain a formed body green body;
4) And sequentially carrying out glue removal and sintering on the green molded body blank to obtain the carbon composite ceramic resistance card.
6. The method of claim 5, wherein: in the step 1), in the mixing, the mixing method is ball milling; specifically, during ball milling, the rotating speed is 350r/min; the time is 30-60min;
in the step 2), in the mixing, the mixing method is ball milling; specifically, the rotating speed in the ball milling is 250r/min; the time is 30-60min;
in the mixed solution B, the organic carbon source exists in the form of aqueous solution;
in the organic carbon source solution a, the mass percentage concentration of the organic carbon source is 10-15%;
in the step 3), drying is carried out until the water content is 2-5wt%; the temperature is 160 ℃; the time is 10h;
in the sieving, the mesh number of the sieve pores is 80-120; in particular to 100 meshes;
in the vacuum drying, the temperature is 140-180 ℃; in particular to 160 ℃; the time is 1-3h; in particular for 2h;
in the pressing, the pressure intensity is 3MPa; the time is 60-180s; specifically 120s;
the step 4) of glue discharging comprises the following steps: firstly, putting the green compact into a vacuum furnace, sealing a furnace door, vacuumizing until the vacuum degree of the furnace is less than or equal to 9Pa, filling 60Pa nitrogen or argon for atmosphere replacement, repeating for 2-4 times, starting to heat according to a glue discharging curve, and filling enough argon while vacuumizing to keep 15KPa argon continuously flowing in the furnace;
the rubber discharge curve is as follows: raising the temperature of room temperature to 160 ℃ at a heating rate of 1 ℃/min, preserving heat at 160 ℃ for 2h, raising the temperature of 160 ℃ to 800 ℃ at 20 ℃/min, raising the temperature of 800 ℃ to 1200 ℃ at 10 ℃/min, raising the temperature of 1200 ℃ to 1450 ℃ at 5 ℃/min, preserving heat at 1450 ℃ for 2h, reducing the temperature of 1450 ℃ to 800 ℃ at 10 ℃/min, and reducing the temperature below 800 ℃ along with the furnace;
in the sintering process, the sintering atmosphere is inert atmosphere; the sintering temperature is 1400-1480 ℃; particularly 1450 ℃; the time is 1-3h; in particular for 2h; the pressure of the inert atmosphere is 12-18KPa; specifically 15KPa.
7. The method according to claim 5 or 6, characterized in that: the method further comprises the following steps: after the step 4), naturally cooling the ceramic wafer obtained by sintering at the temperature of less than 800 ℃, spraying sand, and spraying an electrode layer;
in the sand blasting, the thickness of the sand blasting is 1-1.5mm.
8. A resistor comprising the carbon composite ceramic resistor sheet according to any one of claims 1 to 4.
9. Use of the carbon composite ceramic resistor sheet as claimed in any one of claims 1 to 4 in the manufacture of a resistor.
10. The resistor according to claim 8 or the use according to claim 9, characterized in that: the resistor is a carbon composite resistor.
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