CN106851872A - A kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry and preparation method thereof - Google Patents
A kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry and preparation method thereof Download PDFInfo
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- CN106851872A CN106851872A CN201611129402.7A CN201611129402A CN106851872A CN 106851872 A CN106851872 A CN 106851872A CN 201611129402 A CN201611129402 A CN 201611129402A CN 106851872 A CN106851872 A CN 106851872A
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- 239000002002 slurry Substances 0.000 title claims abstract description 70
- 238000005245 sintering Methods 0.000 title claims abstract description 51
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 50
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000007613 slurry method Methods 0.000 title abstract 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000011521 glass Substances 0.000 claims abstract description 58
- 239000000853 adhesive Substances 0.000 claims abstract description 56
- 230000001070 adhesive effect Effects 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 54
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 50
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 22
- 229920002521 macromolecule Polymers 0.000 claims abstract description 18
- 239000002667 nucleating agent Substances 0.000 claims abstract description 18
- 239000002562 thickening agent Substances 0.000 claims abstract description 17
- 239000013530 defoamer Substances 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 30
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 26
- 238000003723 Smelting Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000156 glass melt Substances 0.000 claims description 19
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229920000570 polyether Polymers 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 18
- 239000010703 silicon Substances 0.000 claims description 18
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 150000001408 amides Chemical class 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000005611 electricity Effects 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 6
- 239000001393 triammonium citrate Substances 0.000 claims description 6
- 235000011046 triammonium citrate Nutrition 0.000 claims description 6
- -1 alkene ester Chemical class 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- 239000001856 Ethyl cellulose Substances 0.000 claims description 4
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229920000180 alkyd Polymers 0.000 claims description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920001249 ethyl cellulose Polymers 0.000 claims description 4
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 4
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 4
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229920005749 polyurethane resin Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 238000005202 decontamination Methods 0.000 claims description 3
- 230000003588 decontaminative effect Effects 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical group O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 2
- 239000001293 FEMA 3089 Substances 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 2
- FUGIIBWTNARRSF-UHFFFAOYSA-N decane-5,6-diol Chemical compound CCCCC(O)C(O)CCCC FUGIIBWTNARRSF-UHFFFAOYSA-N 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 125000005375 organosiloxane group Chemical group 0.000 claims description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 2
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims 1
- 241000196324 Embryophyta Species 0.000 claims 1
- JOUGPOOKAWFCTH-UHFFFAOYSA-N OC1(S(=O)(=O)O)C=CC(C=C1)(N)O Chemical class OC1(S(=O)(=O)O)C=CC(C=C1)(N)O JOUGPOOKAWFCTH-UHFFFAOYSA-N 0.000 claims 1
- 229960000583 acetic acid Drugs 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 3
- 238000007639 printing Methods 0.000 abstract description 3
- 239000004677 Nylon Substances 0.000 description 16
- 239000012535 impurity Substances 0.000 description 16
- 229920001778 nylon Polymers 0.000 description 16
- 238000002386 leaching Methods 0.000 description 13
- 239000004411 aluminium Substances 0.000 description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 12
- 238000002791 soaking Methods 0.000 description 10
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 8
- 239000000758 substrate Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000000075 oxide glass Substances 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229950000244 sulfanilic acid Drugs 0.000 description 2
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
Landscapes
- Conductive Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry and preparation method thereof, the resistance slurry includes inorganic adhesive phase, complex function phase, organic carrier, and inorganic bond is mutually by Bi2O3、B2O3, the microcrystalline glass powder that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide, complex function is made up of spherical silver powder, flake silver powder, three kinds of materials of nano Pd powder, and organic carrier is made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent；The preparation method is mutually prepared including inorganic bond, complex function is mutually prepared, organic carrier is prepared, prepares resistance slurry.The resistance slurry have good thixotropy, mobility and sintering temperature is low, burn till after resistive layer structure it is smooth, fine and close, do not ftracture, pin-free, bubble-free, leadless environment-friendly, adhesive force is strong, ageing-resistant, sheet resistance is adjustable, temperature-coefficient of electrical resistance is relatively low and adjustable, printing characteristic and burns till characteristic good.
Description
Technical field
The present invention relates to thick film circuit technique field, more particularly to a kind of aluminium alloy base plate middle temperature of large power thick film circuit
Silver-colored palladium resistance slurry of sintering and preparation method thereof.
Background technology
As thick film circuit element is to multiple stratification and the development of miniaturization, corresponding mechanics and thermal property are proposed to substrate
It is required that, the particularly thermal conductivity requirement of substrate；Although BeO, Al2O3, the ceramic substrate such as AlN there is thermal conductivity factor higher, but
BeO substrates are limited because of its toxicity and used, Al2O3With AlN substrate because mechanical performance is poor, assemble difficult and apply limited.Aluminium is closed
The property such as density that gold base has is small, the cold and hot working processability that ductility is good, thermal conductivity is good, excellent and good toughness
Can make it possible to be used as baseplate material；Yet with aluminium alloy base plate thermal coefficient of expansion it is high, while fusing point is low（It is less than
660℃）, therefore high-temperature standard firing process can not be selected（850℃）；It requires that corresponding resistance slurry can only be less than aluminium
Fusion temperature under sinter, and have good adhesive force, matching, screen printing property and multiple refiring capability so that aluminium base electricity
The development of resistance paste becomes extremely difficult.
Earlier 1900s, thick film circuit is prepared on anodization aluminium sheet for solar cell, LED substrates, for direct current
Low-voltage, succeeds, yet with power is small, hot property, insulating properties it is poor, it is dangerous the problems such as, it is impossible to for electric heating unit
Part.At present, be applied to aluminium alloy base plate thick film circuit heating, especially specialty for aluminium alloy base plate system resistance
Slurry, country's report is less.United States Patent (USP) US62221661B1 discloses a kind of aluminium base thick film heating, invention use etc.
Plasma spray method is by Al2O3And ZrO2Mixture be attached on aluminium base as insulating medium layer, then using silk-screen printing
Be printed on pure Ag or Ag/Pd resistance slurries in insulated Aluminium based plates by mode, then 10-15min is sintered at 580 DEG C, as resistance
Heating layer；Plasma spraying method high cost used by this method, and in the sintering process of later stage resistance slurry, insulating medium layer is easy
There is diffusion with resistive layer, influence the resistance of aluminium base heater element and the stability of power.Additionally, the burning of the resistance slurry
Junction temperature is higher, can cause aluminium base gross distortion during sintering, influences the resistance and power of aluminium base heater element
Stability.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art and providing a kind of aluminium alloy base plate high-power thick-film electricity
Road intermediate sintering temperature silver palladium resistance slurry, aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry has good
Good rheological characteristic, thixotropy and sintering temperature is low, the resistive layer after burning till has that structure is smooth, fine and close, do not ftracture, it is pin-free,
Bubble-free, the advantage of leadless environment-friendly, while resistive layer adhesive force after burning till is strong, ageing-resistant, sheet resistance is adjustable, temperature-coefficient of electrical resistance
Relatively low and adjustable, printing characteristic and characteristic good is burnt till, i.e., the advantages of can matching with aluminium alloy base plate well.
Another object of the present invention is to provide a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium electricity
The preparation method of resistance paste, the preparation method can be produced effectively in preparing above-mentioned aluminium alloy base plate large power thick film circuit
The silver-colored palladium resistance slurry of temperature sintering.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, includes following weight portion
Material, specially：
Inorganic adhesive phase 10%-30%
Complex function phase 50%-70%
Organic carrier 20%-25%；
Wherein, inorganic bond is mutually by Bi2O3、B2O3, the unleaded crystallite glass that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide
Glass powder, Bi in inorganic adhesive phase2O3、B2O3, BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by
40%-60%、20%-30%、5%-15%、5%-10%、1%-5%、1%-5%；
The mixed powder that complex function is mutually made up of spherical silver powder, flake silver powder, nano Pd powder, spherical silver in complex function phase
Powder, flake silver powder, the weight portion of three kinds of materials of nano Pd powder are followed successively by 40%-50%, 40%-50%, 1-10%；
The mixing that organic carrier is made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent
Thing, organic solvent, macromolecule thickener, dispersant, defoamer, the weight portion of five kinds of materials of thixotropic agent are followed successively by organic carrier
50%-70%、25%-35%、1%-5%、1%-5%、1%-5%。
Preferably, the Nucleating Agent is CaF2、TiO2、ZrO2、P2O5、Sb2O3、V2O5、NiO、Fe2O3In one kind or extremely
Few two kinds of mixtures for being constituted.
Preferably, the rare earth oxide is La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3
In one kind, the particle size values of rare earth oxide are 1 μm -3 μm.
Preferably, the particle size values of the leadless crystallizing glass powder are 1 μm -3 μm, and softening point is 350-480 DEG C, and average line is swollen
Swollen coefficient is 18-25 × 10-6/℃。
Preferably, the particle size values of spherical silver powder are 1 μm -3 μm in the complex function phase, and apparent density is 1.0-2.0 g/
cm3, tap density is 1.0-2.0 g/cm3；The particle size values of the flake silver powder are 1 μm -3 μm, and apparent density is 1.0-2.0 g/
cm3, tap density is 1.0-2.0 g/cm3；The particle size values of the nano Pd powder are 10nm-50nm, and apparent density is 2.0-2.5
g/cm3, tap density is 3.5-4.0 g/cm3。
Preferably, the organic solvent is turpentine oil, terpinol, hexadecanol, butyl carbitol, butyl carbitol acetic acid
Ester, diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, ethylene glycol ether acetate, ATBC, tributyl phosphate, 1,
4- butyrolactone, mixed dibasic acid ester, 1-METHYLPYRROLIDONE, DMF, DMA, diformazan are sub-
A kind of or at least two mixtures for being constituted in sulfone.
Preferably, the macromolecule thickener is ethyl cellulose, polyethylene glycol 2000, polyvinyl butyral resin, poly-vinegar
One kind in vinyl acetate, polyvinylpyrrolidone, hydrogenated rosin resin, acrylate, epoxy resin, polyurethane resin
Or at least two mixtures for being constituted.
Preferably, the dispersant be triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae-dihydroxy sulfanilic acid in one kind or
The mixture that person at least two is constituted；The defoamer be organosiloxane, polyethers, polyethylene glycol, ethylene-acrylic acid copolymer,
A kind of or at least two mixtures for being constituted in polyglyceryl fatty acid ester, dimethyl silicone polymer, organic silicon modified by polyether.
Preferably, the thixotropic agent is hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organic swelling
A kind of or at least two mixtures for being constituted in soil or aerosil.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, include with
Lower processing step, specially：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3, BaO, ZnO, Nucleating Agent, rare earth oxide in three-dimensional material mixer be well mixed,
Bi in mixture2O3、B2O3, BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by 40%-60%, 20%-30%,
5%-15%、5%-10%、1%-5%、1%-5%；Treat Bi2O3、B2O3, the mixture mixing that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide
After uniform, mixture is placed in carries out melting treatment in smelting furnace, and smelting temperature is 1200-1400 DEG C, and soaking time is 2-4 hours,
To obtain glass melts；Glass melts are then carried out into Water Quenching again, to obtain glass dregs, finally by glass dregs it is broken and with
Distilled water carries out ball-milling treatment 6 hours for medium to glass dregs, that is, obtain the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are placed in batch mixing and are stirred mixing, to obtain
Complex function phase is obtained, spherical silver powder, flake silver powder, the weight portion of three kinds of materials of nano Pd powder are followed successively by 40%- in complex function phase
50%th, 40%-50%, 1%-10%, the particle size values of spherical silver powder are 1 μm -3 μm in mixed powder, and the particle size values of flake silver powder are 1 μm of -3 μ
M, the particle size values of nano Pd powder are 10 nm-50 nm；
C, prepare organic carrier：By organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent in 80 DEG C of water bath conditions
Middle dissolving, to obtain organic carrier, and by adjusting the content of macromolecule thickener so that the viscosity of organic carrier is controlled 200
In the range of mPas -300 mPas；Wherein, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer,
The weight portion of five kinds of materials of thixotropic agent is followed successively by 50%-70%, 25%-35%, 1%-5%, 1%-5%, 1%-5%；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, will then stir
The inorganic adhesive phase after dispersion, complex function phase, organic carrier mixture is mixed to be placed in three-roll grinder and ground repeatedly, with
Acquisition range of viscosities is the resistance slurry of 80-150Pas, average fineness less than 8 μm, finally again by the filter screen of 500 mesh to electricity
Resistance paste carries out filtration treatment to go out decontamination；Wherein, inorganic adhesive phase, complex function phase, organic carrier three in resistance slurry
The weight portion for planting material is followed successively by 10%-30%, 50%-70%, 20%-25%.
Beneficial effects of the present invention are：A kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature of the present invention
Silver-colored palladium resistance slurry, its material for including following weight portion：It is inorganic adhesive phase 10%-30%, complex function phase 50%-70%, organic
Carrier 20%-25%；Inorganic bond is mutually by Bi2O3、B2O3, the unleaded crystallite that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide
Glass dust, Bi in inorganic adhesive phase2O3、B2O3, BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by
40%-60%、20%-30%、5%-15%、5%-10%、1%-5%、1%-5%；Complex function is mutually spherical silver powder, flake silver powder, nanometer
The mixed powder that palladium powder is constituted, spherical silver powder, flake silver powder, three kinds of weight portions of material of nano Pd powder are successively in complex function phase
It is 40%-50%, 40%-50%, 1-10%；Organic carrier is organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent
The mixture that five kinds of materials are constituted, organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent five in organic carrier
The weight portion for planting material is followed successively by 50%-70%, 25%-35%, 1%-5%, 1%-5%, 1%-5%.By above-mentioned material proportion, the present invention
Aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry there is advantages below, specially：
1st, from Bi2O3-B2O3- BaO-ZnO systems leadless crystallizing glass powder as Binder Phase, by Bi2O3-B2O3-BaO-ZnO
The differential thermal of microcrystalline glass in series, thermal coefficient of expansion, density, dielectric constant, dielectric loss, glass transition temperature, transition temperature and softening
The regulation of temperature etc. is allowed to the heat of the thick-film resistor track layer that composition is combined with rare earth oxide, complex function phase, organic carrier
The coefficient of expansion is matched and with good binding ability with aluminium alloy base plate, while resistive layer can be made between 450-570 DEG C
Sintering, it is to avoid lead is researching and developing, the injury that uses and caused to environment, human body after discarded, can solve high-power resistance or electricity
Thermal element manufacturing urgent problem, meets RoHS Directive（2002/95/EC）It is required that；
2nd, the addition of rare earth oxide, can not only reduce the cost of leadless crystallizing glass powder and improve the comprehensive utilization of rare earth resources
Benefit, can also reduce Bi2O3-B2O3Glass transition temperature, the softening temperature of-BaO-ZnO systems leadless crystallizing glass powder, while it is swollen to improve its heat
Swollen coefficient, makes it preferably relatively low with fusing point（660℃）, thermal coefficient of expansion（23×10-6/℃）Aluminium alloy base plate very high matches；
3rd, the mixed powder constituted using spherical silver powder, flake silver powder, nano Pd powder is mutually used to prepare aluminium conjunction as complex function
Gold base aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, the printing characteristic of the resistance slurry
It is good, burn till characteristic good, have that adhesive force is strong, ageing-resistant, electric conductivity is good with its resistance track for preparing, heating efficiency it is high with
And the advantage compatible with aluminium alloy base plate, while by change the composition of inorganic adhesive phase and complex function phase, weight proportion and
Sintering curre, can not only be effectively reduced sintering temperature, the sheet resistance of regulation resistive layer of resistive layer, while causing resistive layer again
Sheet resistance reheating rate of change be less than 5%, temperature-coefficient of electrical resistance be less than 200 × 10-6/℃；
4th, the intermediate sintering temperature resistance slurry, can be used to preparing that light weight, thermal conductivity be good, high-power aluminium alloy base plate thick film circuit electricity
Thermal element, is widely used in industry, household electrical appliance, war industry field, is greatly enhanced efficiency of energy utilization.
It is of the invention another to have the beneficial effect that：A kind of aluminium alloy base plate of the present invention middle temperature of large power thick film circuit
The preparation method of the silver-colored palladium resistance slurry of sintering, it includes following processing step, specially：A, prepare inorganic adhesive phase：Will
Bi2O3、B2O3, BaO, ZnO, Nucleating Agent, rare earth oxide in three-dimensional material mixer be well mixed, Bi in mixture2O3、B2O3、
BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by 40%-60%, 20%-30%, 5%-15%, 5%-10%,
1%-5%、1%-5%；Treat Bi2O3、B2O3, the mixture that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide it is well mixed after, will
Mixture is placed in and melting treatment is carried out in smelting furnace, and smelting temperature is 1200-1400 DEG C, and soaking time is 2-4 hours, to obtain glass
Glass liquation；Glass melts are then carried out into Water Quenching again, it is finally that glass dregs are broken and with distilled water be to obtain glass dregs
Medium carries out ball-milling treatment 6 hours to glass dregs, that is, obtain the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；B, preparation are multiple
Close function phase：Spherical silver powder, flake silver powder, nano Pd powder are placed in batch mixing and are stirred mixing, to obtain complex function phase,
In complex function phase spherical silver powder, flake silver powder, the weight portion of three kinds of materials of nano Pd powder be followed successively by 40%-50%, 40%-50%,
1%-10%, the particle size values of spherical silver powder are 1 μm -3 μm in mixed powder, and the particle size values of flake silver powder are 1 μm -3 μm, nano Pd powder
Particle size values are 10 nm-50 nm；C, prepare organic carrier：By organic solvent, macromolecule thickener, dispersant, defoamer, thixotroping
Agent is dissolved in 80 DEG C of water bath conditions, to obtain organic carrier, and by adjusting the content of macromolecule thickener so as to have airborne
The viscosity of body is controlled in the range of 200 mPas -300 mPas；Wherein, organic solvent, macromolecule thickening in organic carrier
Agent, dispersant, defoamer, the weight portion of five kinds of materials of thixotropic agent are followed successively by 50%-70%, 25%-35%, 1%-5%, 1%-5%, 1%-
5%；D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then will stirring
Inorganic adhesive phase, complex function phase after dispersion, organic carrier mixture are placed in three-roll grinder and are ground repeatedly, to obtain
It is the resistance slurry of 80-150Pas, average fineness less than 8 μm to obtain range of viscosities, finally again by the filter screen of 500 mesh to resistance
Slurry carries out filtration treatment to go out decontamination；Wherein, inorganic adhesive phase, complex function phase, three kinds of organic carrier in resistance slurry
The weight portion of material is followed successively by 10%-30%, 50%-70%, 20%-25%.Designed by above-mentioned processing step, aluminium alloy of the invention
The preparation method of substrate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry can effectively be produced and prepare above-mentioned aluminium conjunction
Gold base large power thick film circuit intermediate sintering temperature silver palladium resistance slurry.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
Embodiment 1, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with weight percent
Than meter, including following components：
Inorganic adhesive phase 10%
Complex function phase 70%
Organic carrier 20%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 40%
B2O3 30%
BaO 15%
ZnO 10%
TiO2 2.5%
Y2O3 2.5%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 50%
Flake silver powder 49%
Nano Pd powder 1%；
The organic carrier, by weight percentage, including following components：
Butyl carbitol 35%
Butyl carbitol acetate 35%
Ethyl cellulose 25%
Polymethyl acid amide 2%
Organic silicon modified by polyether 2%
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、TiO2And Y2O3After being well mixed in three-dimensional material mixer
Then at smelting furnace melting, smelting temperature is 1200 DEG C, and soaking time is to obtain glass melts in 4 hours, then enters glass melts
Water-filling is quenched and obtains glass dregs, finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, that is, obtain
Particle size values are 1 μm -3 μm of leadless crystallizing glass powder；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol, butyl carbitol acetate, ethyl cellulose, polymethyl acid amide, poly-
Ether modified organic silicon, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are removed by 200 mesh nylon leaching nets
Impurity, the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 2, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 10%
Complex function phase 70%
Organic carrier 20%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 40%
B2O3 30%
BaO 15%
ZnO 10%
TiO2 3%
CaF2 1%
La2O3 1%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 50%
Flake silver powder 48%
Nano Pd powder 2%.
The organic carrier, by weight percentage, including following components：
Ethylene glycol ether acetate 35%
ATBC 35%
Acrylate 25%
Polymethyl acid amide 2%
Organic silicon modified by polyether 2%
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、TiO2、CaF2And La2O3Mix in three-dimensional material mixer
Then at smelting furnace melting after uniform, smelting temperature is 1300 DEG C, and soaking time is to obtain glass melts in 3 hours, then by glass
Liquation carries out water quenching and obtains glass dregs, finally by glass dregs it is broken and with distilled water be medium to glass dregs ball milling 6 hours,
Obtain the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By ethylene glycol ether acetate, ATBC, acrylate, polymethylacrylic acid
Amine, organic silicon modified by polyether, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are filtered by 200 mesh nylon
Net goes the removal of impurity, and the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 3, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 15%
Complex function phase 65%
Organic carrier 20%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 55%
B2O3 25%
BaO 10%
ZnO 5%
ZrO2 2.5%
Eu2O3 2.5%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 50%
Flake silver powder 48%
Nano Pd powder 2%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol 45%
Butyl carbitol acetate 25%
Polyurethane resin 25%,
Isosorbide-5-Nitrae-dihydroxy sulfanilic acid 2%,
Organic silicon modified by polyether 2%,
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、ZrO2And Eu2O3After being well mixed in three-dimensional material mixer
Then at smelting furnace melting, smelting temperature is 1400 DEG C, and soaking time is to obtain glass melts in 2 hours, then enters glass melts
Water-filling is quenched and obtains glass dregs, finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, that is, obtain
Particle size values are 1 μm -3 μm of leadless crystallizing glass powder；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol, butyl carbitol acetate, polyurethane resin, 1,4- dihydroxy sulfonic acid
Amine, organic silicon modified by polyether, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are filtered by 200 mesh nylon
Net goes the removal of impurity, and the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 4, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 15%
Complex function phase 65%
Organic carrier 20%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 55%
B2O3 25%
BaO 10%
ZnO 5%
V2O5 2%
CeO2 3%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 48.5%
Flake silver powder 48.5%
Nano Pd powder 3%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol acetic acid 35%
ATBC 35%
Polyvinyl butyral resin 25%
Triammonium citrate 2%
Organic silicon modified by polyether 2%
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、V2O5And CeO2After being well mixed in three-dimensional material mixer
Then at smelting furnace melting, smelting temperature is 1200 DEG C, and soaking time is to obtain glass melts in 4 hours, then enters glass melts
Water-filling is quenched and obtains glass dregs, finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, that is, obtain
Particle size values are 1 μm -3 μm of leadless crystallizing glass powder；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol acetate, ATBC, polyvinyl butyral resin, triammonium citrate,
Organic silicon modified by polyether, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are gone by 200 mesh nylon leaching nets
The removal of impurity, the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 5, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 15%
Complex function phase 60%
Organic carrier 25%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 60%
B2O3 15%
BaO 15%
ZnO 5%
Fe2O3 2.5%
Nd2O3 2.5%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 50%
Flake silver powder 48%
Nano Pd powder 2%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol acetate 40%
Dibutyl phthalate 30%
Epoxy resin 25%
Triammonium citrate 2%
Organic silicon modified by polyether 2%
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、Fe2O3And Nd2O3It is well mixed in three-dimensional material mixer
Afterwards then at smelting furnace melting, smelting temperature is 1200 DEG C, and soaking time is to obtain glass melts in 4 hours, then by glass melts
Carry out water quenching and obtain glass dregs, it is finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, obtain final product
To the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol acetate, dibutyl phthalate, epoxy resin, triammonium citrate, poly-
Ether modified organic silicon, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are removed by 200 mesh nylon leaching nets
Impurity, the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 6, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 20%
Complex function phase 55%
Organic carrier 25%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 45%
B2O3 25%
BaO 15%
ZnO 10%
Sb2O3 2.5%
Pr2O3 2.5%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 48%
Flake silver powder 48%
Nano Pd powder 4%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol acetate 50%
Tributyl phosphate 20%
Polyvinyl acetate 25%
Polymethyl acid amide 2%
Organic silicon modified by polyether 2%
Polyamide wax 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、Sb2O3And Pr2O3It is well mixed in three-dimensional material mixer
Afterwards then at smelting furnace melting, smelting temperature is 1200 DEG C, and soaking time is to obtain glass melts in 4 hours, then by glass melts
Carry out water quenching and obtain glass dregs, it is finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, obtain final product
To the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol acetate, tributyl phosphate, polyvinyl acetate, polymethyl acid amide,
Organic silicon modified by polyether, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, then are removed by 200 mesh nylon leaching nets
Impurity, the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 7, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 25%
Complex function phase 50%
Organic carrier 25%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 50%
B2O3 20%
BaO 15%
ZnO 10%
NiO 2%
Sb2O3 1%
Gd2O3 2%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 40%
Flake silver powder 50%
Nano Pd powder 5%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol acetate 40%
ATBC 30%
Polyethylene glycol 2000 25%
Polymethyl acid amide 2%
Organic silicon modified by polyether 2%
Rilanit special 1%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、NiO、Sb2O3And Gd2O3Mix in three-dimensional material mixer
Then at smelting furnace melting after uniform, smelting temperature is 1400 DEG C, and soaking time is to obtain glass melts in 2 hours, then by glass
Liquation carries out water quenching and obtains glass dregs, finally by glass dregs it is broken and with distilled water be medium to glass dregs ball milling 6 hours,
Obtain the leadless crystallizing glass powder that particle size values are 1 μm -3 μm；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol acetate, ATBC, polyethylene glycol 2000, polymethylacrylic acid
Amine, organic silicon modified by polyether, rilanit special dissolve to obtain organic carrier in 80 DEG C of water-baths, then are filtered by 200 mesh nylon
Net goes the removal of impurity, and the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Embodiment 8, a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, with percentage by weight
Meter, including following components：
Inorganic adhesive phase 30%
Complex function phase 50%
Organic carrier 20%.
The inorganic adhesive phase, by weight percentage, including following components：
Bi2O3 50%
B2O3 20%
BaO 15%
ZnO 10%
P2O5 3%
Sc2O3 2%。
The complex function phase, by weight percentage, including following components：
Spherical silver powder 45%
Flake silver powder 45%
Nano Pd powder 10%.
The organic carrier, by weight percentage, including following components：
Butyl carbitol acetate 45%
Dibutyl phthalate 25%
Polyvinylpyrrolidone 20%
Polymethyl acid amide 4%
Organic silicon modified by polyether 3%
Thixotropy alkyd resin 3%.
A kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it include with
Lower step：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3、BaO、ZnO、P2O5And Sc2O3After being well mixed in three-dimensional material mixer
Then at smelting furnace melting, smelting temperature is 1400 DEG C, and soaking time is to obtain glass melts in 2 hours, then enters glass melts
Water-filling is quenched and obtains glass dregs, finally that glass dregs are broken and be medium to glass dregs ball milling 6 hours with distilled water, that is, obtain
Particle size values are 1 μm -3 μm of leadless crystallizing glass powder；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are well mixed to prepare complex function phase；
C, prepare organic carrier：By butyl carbitol acetate, dibutyl phthalate, polyvinylpyrrolidone, poly- methyl
Acrylic amine, organic silicon modified by polyether, thixotropy alkyd resin dissolve to obtain organic carrier in 80 DEG C of water-baths, then pass through
200 mesh nylon leaching nets go the removal of impurity, and the viscosity of organic carrier is 200 ± 20 mPas；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, starched with obtaining thick-film resistor of the range of viscosities as 110 ± 20Pas, average fineness less than 8 μm
Material, then the removal of impurity is gone by the nylon leaching net of 500 mesh.
Following table is the performance of the aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry of embodiment 1-8
Parameter：
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to thought of the invention,
Will change in specific embodiments and applications, this specification content should not be construed as to limit of the invention
System.
Claims (10)
1. a kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, it is characterised in that include with
The material of lower weight portion, specially：
Inorganic adhesive phase 10%-30%
Complex function phase 50%-70%
Organic carrier 20%-25%；
Wherein, inorganic bond is mutually by Bi2O3、B2O3, the leadless crystallizing glass that is constituted of BaO, ZnO, Nucleating Agent, rare earth oxide
Powder, Bi in inorganic adhesive phase2O3、B2O3, BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by 40%-
60%、20%-30%、5%-15%、5%-10%、1%-5%、1%-5%；
The mixed powder that complex function is mutually made up of spherical silver powder, flake silver powder, nano Pd powder, spherical silver in complex function phase
Powder, flake silver powder, the weight portion of three kinds of materials of nano Pd powder are followed successively by 40%-50%, 40%-50%, 1-10%；
The mixing that organic carrier is made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent
Thing, organic solvent, macromolecule thickener, dispersant, defoamer, the weight portion of five kinds of materials of thixotropic agent are followed successively by organic carrier
50%-70%、25%-35%、1%-5%、1%-5%、1%-5%。
2. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The Nucleating Agent is CaF2、TiO2、ZrO2、P2O5、Sb2O3、V2O5、NiO、Fe2O3In one kind or at least two
Plant constituted mixture.
3. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The rare earth oxide is La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3In
One kind, the particle size values of rare earth oxide are 1 μm -3 μm.
4. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The particle size values of the leadless crystallizing glass powder are 1 μm -3 μm, and softening point is 350-480 DEG C, average line expansion system
Number is 18-25 × 10-6/℃。
5. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The particle size values of spherical silver powder are 1 μm -3 μm in the complex function phase, and apparent density is 1.0-2.0 g/cm3,
Tap density is 1.0-2.0 g/cm3；The particle size values of the flake silver powder are 1 μm -3 μm, and apparent density is 1.0-2.0 g/cm3,
Tap density is 1.0-2.0 g/cm3；The particle size values of the nano Pd powder are 10nm-50nm, and apparent density is 2.0-2.5 g/
cm3, tap density is 3.5-4.0 g/cm3。
6. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The organic solvent is turpentine oil, terpinol, hexadecanol, butyl carbitol, butyl carbitol acetate, two
Glycol monoethyl ether, dibutyl ethylene glycol ether, ethylene glycol ether acetate, ATBC, tributyl phosphate, Isosorbide-5-Nitrae-Ding Nei
In ester, mixed dibasic acid ester, 1-METHYLPYRROLIDONE, DMF, DMA, dimethyl sulfoxide
A kind of or at least two mixtures for being constituted.
7. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The macromolecule thickener is ethyl cellulose, polyethylene glycol 2000, polyvinyl butyral resin, poly-vinegar acid second
One kind in alkene ester, polyvinylpyrrolidone, hydrogenated rosin resin, acrylate, epoxy resin, polyurethane resin or
At least two mixtures for being constituted.
8. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The dispersant be triammonium citrate, polymethyl acid amide, 1,4- dihydroxy sulfanilic acids in one kind or
The mixture that person at least two is constituted；The defoamer is organosiloxane, polyethers, polyethylene glycol, ethylene-acrylic acid copolymer
A kind of in thing, polyglyceryl fatty acid ester, dimethyl silicone polymer, organic silicon modified by polyether or at least two constituted it is mixed
Compound.
9. a kind of aluminium alloy base plate according to claim 1 large power thick film circuit intermediate sintering temperature silver palladium resistance slurry,
It is characterized in that：The thixotropic agent be hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organobentonite or
A kind of or at least two mixtures for being constituted in aerosil.
10. a kind of aluminium alloy base plate preparation method of large power thick film circuit intermediate sintering temperature silver palladium resistance slurry, its feature exists
In including following processing step, specially：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3, BaO, ZnO, Nucleating Agent, rare earth oxide mix in three-dimensional material mixer
It is even, Bi in mixture2O3、B2O3, BaO, ZnO, Nucleating Agent, the weight portion of six kinds of materials of rare earth oxide be followed successively by 40%-60%,
20%-30%、5%-15%、5%-10%、1%-5%、1%-5%；Treat Bi2O3、B2O3, BaO, ZnO, Nucleating Agent, rare earth oxide constituted
Mixture it is well mixed after, mixture is placed in carries out melting treatment in smelting furnace, smelting temperature is 1200-1400 DEG C, insulation
Time is 2-4 hours, to obtain glass melts；Glass melts are then carried out into Water Quenching again, to obtain glass dregs, finally will
Glass dregs are broken and carry out ball-milling treatment 6 hours to glass dregs by medium of distilled water, that is, obtain the nothing that particle size values are 1 μm -3 μm
Lead microcrystalline glass powder；
B, preparation complex function phase：Spherical silver powder, flake silver powder, nano Pd powder are placed in batch mixing and are stirred mixing, to obtain
Complex function phase is obtained, spherical silver powder, flake silver powder, the weight portion of three kinds of materials of nano Pd powder are followed successively by 40%- in complex function phase
50%th, 40%-50%, 1%-10%, the particle size values of spherical silver powder are 1 μm -3 μm in mixed powder, and the particle size values of flake silver powder are 1 μm of -3 μ
M, the particle size values of nano Pd powder are 10 nm-50 nm；
C, prepare organic carrier：By organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent in 80 DEG C of water bath conditions
Middle dissolving, to obtain organic carrier, and by adjusting the content of macromolecule thickener so that the viscosity of organic carrier is controlled 200
In the range of mPas -300 mPas；Wherein, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer,
The weight portion of five kinds of materials of thixotropic agent is followed successively by 50%-70%, 25%-35%, 1%-5%, 1%-5%, 1%-5%；
D, prepare resistance slurry：By inorganic adhesive phase, complex function phase, organic carrier dispersed with stirring in container, will then stir
The inorganic adhesive phase after dispersion, complex function phase, organic carrier mixture is mixed to be placed in three-roll grinder and ground repeatedly, with
Acquisition range of viscosities is the resistance slurry of 80-150Pas, average fineness less than 8 μm, finally again by the filter screen of 500 mesh to electricity
Resistance paste carries out filtration treatment to go out decontamination；Wherein, inorganic adhesive phase, complex function phase, organic carrier three in resistance slurry
The weight portion for planting material is followed successively by 10%-30%, 50%-70%, 20%-25%.
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| CN107424661A (en) * | 2017-06-28 | 2017-12-01 | 西安英诺维特新材料有限公司 | A kind of devitrified glass heating plate medium temperature resistance slurry |
| CN108901089A (en) * | 2018-08-22 | 2018-11-27 | 湖南海曙科技有限公司 | A kind of thick film heating element and its operating temperature method for improving |
| CN110970151A (en) * | 2019-12-18 | 2020-04-07 | 广东顺德弘暻电子有限公司 | High-weldability anti-warping thick film conductor slurry for stainless steel base material and preparation method thereof |
| CN112670009A (en) * | 2020-11-30 | 2021-04-16 | 北京无线电测量研究所 | Electrical heating resistance paste and preparation method and application thereof |
| CN113793715A (en) * | 2021-11-16 | 2021-12-14 | 西安宏星电子浆料科技股份有限公司 | Low-temperature coefficient resistance paste |
| CN114283961A (en) * | 2021-12-30 | 2022-04-05 | 中国人民解放军国防科技大学 | High-temperature resistance slurry and preparation method and application thereof |
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Application publication date: 20170613 |