CN105810291A - Rare-earth resistance paste of medium- and low-resistance high-power thick film circuit and preparation method of rare-earth resistance paste - Google Patents
Rare-earth resistance paste of medium- and low-resistance high-power thick film circuit and preparation method of rare-earth resistance paste Download PDFInfo
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- CN105810291A CN105810291A CN201610209923.7A CN201610209923A CN105810291A CN 105810291 A CN105810291 A CN 105810291A CN 201610209923 A CN201610209923 A CN 201610209923A CN 105810291 A CN105810291 A CN 105810291A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract 14
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract 14
- 238000002360 preparation method Methods 0.000 title claims abstract 5
- 239000000843 powder Substances 0.000 claims abstract 14
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract 7
- 229920002521 macromolecule Polymers 0.000 claims abstract 7
- 239000002562 thickening agent Substances 0.000 claims abstract 7
- 239000002270 dispersing agent Substances 0.000 claims abstract 6
- 239000002667 nucleating agent Substances 0.000 claims abstract 6
- 239000003960 organic solvent Substances 0.000 claims abstract 6
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract 6
- 239000013008 thixotropic agent Substances 0.000 claims abstract 6
- 229910011255 B2O3 Inorganic materials 0.000 claims abstract 5
- 238000005245 sintering Methods 0.000 claims abstract 5
- 229910052681 coesite Inorganic materials 0.000 claims abstract 4
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract 4
- 229910052682 stishovite Inorganic materials 0.000 claims abstract 4
- 229910052905 tridymite Inorganic materials 0.000 claims abstract 4
- 239000002002 slurry Substances 0.000 claims 13
- 239000000203 mixture Substances 0.000 claims 12
- 239000000463 material Substances 0.000 claims 9
- 239000000853 adhesive Substances 0.000 claims 6
- 230000001070 adhesive effect Effects 0.000 claims 6
- 239000011521 glass Substances 0.000 claims 6
- 239000002245 particle Substances 0.000 claims 6
- 239000013530 defoamer Substances 0.000 claims 5
- 239000002131 composite material Substances 0.000 claims 3
- -1 NC Nitroncellulose Polymers 0.000 claims 2
- 238000003723 Smelting Methods 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 2
- 239000000156 glass melt Substances 0.000 claims 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims 1
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims 1
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims 1
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical group NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims 1
- 239000001856 Ethyl cellulose Substances 0.000 claims 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims 1
- 239000004952 Polyamide Substances 0.000 claims 1
- 239000004721 Polyphenylene oxide Substances 0.000 claims 1
- 239000004372 Polyvinyl alcohol Substances 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 150000001399 aluminium compounds Chemical class 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 229910052787 antimony Inorganic materials 0.000 claims 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims 1
- 238000000498 ball milling Methods 0.000 claims 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims 1
- 229910001634 calcium fluoride Inorganic materials 0.000 claims 1
- 239000001768 carboxy methyl cellulose Substances 0.000 claims 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims 1
- 239000004359 castor oil Substances 0.000 claims 1
- 235000019438 castor oil Nutrition 0.000 claims 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical group O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 150000001869 cobalt compounds Chemical class 0.000 claims 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000004205 dimethyl polysiloxane Substances 0.000 claims 1
- 239000012153 distilled water Substances 0.000 claims 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 229920001249 ethyl cellulose Polymers 0.000 claims 1
- 235000019325 ethyl cellulose Nutrition 0.000 claims 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims 1
- 229920002647 polyamide Polymers 0.000 claims 1
- 229920000570 polyether Polymers 0.000 claims 1
- 229920002451 polyvinyl alcohol Polymers 0.000 claims 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 238000005096 rolling process Methods 0.000 claims 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 229940116411 terpineol Drugs 0.000 claims 1
- 150000003606 tin compounds Chemical class 0.000 claims 1
- 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 1
- 235000011046 triammonium citrate Nutrition 0.000 claims 1
- 239000001393 triammonium citrate Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 150000003752 zinc compounds Chemical class 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 abstract 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910001220 stainless steel Inorganic materials 0.000 abstract 1
- 239000010935 stainless steel Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
Classifications
-
- 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
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Abstract
The invention discloses rear-earth resistance paste of a medium- and low-resistance high-power thick film circuit and a preparation method of the rare-earth resistance paste. The rear-earth resistance paste of the medium- and low-resistance high-power thick film circuit comprises a functional phase, an inorganic binding phase, a sintering accelerant and an organic carrier, wherein the functional phase comprises nanometer silver powder and ruthenium oxide powder, the inorganic binding phase comprises SiO2, CaO, B2O3, Al2O3, Bi2O3, a rare-earth oxide and a nucleation agent, and the organic carrier comprises an organic solvent, a macromolecule thickening agent, a dispersing agent, a defoaming agent and a thixotropic agent. The rear-earth resistance paste of the medium- and low-resistance high-power thick film circuit is low and adjustable in square resistance, relatively low and adjustable in resistance temperature coefficient, has excellent printing characteristic and calcination property, and can be matched with an insulation stainless steel substrate. The preparation method sequentially comprises the process steps of preparing the inorganic binding phase, preparing the functional phase, preparing the organic carrier and preparing the resistance paste and can be used for effectively producing and preparing the above rare-earth resistance paste.
Description
Technical field
The present invention relates to technical field of electronic materials, particularly relate to a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry and preparation method thereof, this medium or low resistance section large power thick film circuit rare earth resistance slurry is based on stainless steel substrate.
Background technology
In electric heating field, heating element wants that cube is little, power is big, thermal inertia is little, surface thermal load is big, power consumption is low, the thermal efficiency is high, thermal starting is fast, power stability, stationary field uniformly, good manufacturability, body temp auto-controlled, safe and reliable to operation, life-span length, applied widely, it is therefore desirable to use thick-film heating element.
Current thick film heating resistance is usually with the noble metal powders such as gold, silver, platinum, ruthenic oxide or its oxide for matrix, add the glassy phase as inorganic binder, and it is mixed to form heating resistor slurry with organic carrier, then silk screen process is to ceramic substrate, sinters and be prepared from air atmosphere, 300 DEG C of-1200 DEG C of temperature ranges.In thick film circuit technique field, traditional substrate has polymeric substrates and ceramic substrate, but both has its limitation, and excellent mechanical performance, hot property, the large scale of insulating stainless steel substrate and can be made into the rare characteristics such as complicated shape, make its probability applied on high-power thick-film device of people's special concern.
At present, high-power resistance (> 100W-1000W), large power, electrically thermal element (> 100W-1000W) etc. the generally individually wire resistor silk making of the components and parts that have a large capacity and a wide range of application, it has the features such as size is big, the life-span is shorter, thermal design is difficult, and is increasingly difficult to meet the rigors such as each electric appliances miniaturization, high reliability, long-life.The increasingly mature urgent need of thick film circuit element preparation and application technology develops the thick-film resistor paste matched with insulating stainless steel substrate performance and thick film conductor paste, to design the high-power thick-film element of preparation small size, planarization, high reliability, long-life, low cost, to meet the growing market demand.
The resistance track of high-power thick-film resistive element and heating and electrode trace are burnt till acquisition by resistance slurry and electrocondution slurry through silk screen printing and drying respectively.High power characteristics requires that component resistance track area is relatively big, resistance is relatively low and should have alap temperature-coefficient of electrical resistance, therefore, to the requirement of resistance slurry except necessary resistance and temperature-coefficient of electrical resistance, the requirement of its firing process performance is also high than low power ceramic substrate thick film circuit element.Owing to the coefficient of expansion of stainless steel substrate is much larger than ceramic substrate, therefore the resistance track rete after burning till based on the thick-film resistor paste of stainless steel substrate should have the bigger coefficient of expansion to match with rustless steel, simultaneously the glassy phase in slurry also should with based on the solid-phase component chemical compatibility in the dielectric paste of stainless steel substrate and electrocondution slurry.
Summary of the invention
Present invention aims to the deficiencies in the prior art and a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry is provided, medium or low resistance section large power thick film circuit rare earth resistance slurry sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is relatively low and adjustable for this, printing characteristic and burn till characteristic good, and can match with insulating stainless steel substrate.
Another object of the present invention is to provide a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method can prepare above-mentioned medium or low resistance section large power thick film circuit rare earth resistance slurry effectively, and prepared by medium or low resistance section large power thick film circuit rare earth resistance slurry sheet resistance low and adjustable, temperature-coefficient of electrical resistance is relatively low and adjustable, printing characteristic and burn till characteristic good, and can match with insulating stainless steel substrate.
For reaching above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, includes the material of following weight portion, particularly as follows:
Function phase 60%-70%
Inorganic adhesive phase 10%-15%
Sintering aids 0.5%-5%
Organic carrier 10%-29.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3, the mixture that forms of rare earth oxide, Nucleating Agent, inorganic adhesive mutually in SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, seven kinds of materials of Nucleating Agent weight portion be followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10%；
Organic carrier is the mixture that organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent form, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%.
Wherein, described sintering aids is the mixture that a kind of or at least two in zinc, stannum, aluminum, cobalt, antimony, zinc compound, tin compound, aluminium compound, cobalt compound, antimonial forms.
Wherein, described rare earth oxide is CeO2、Sm2O3、Gd2O3、Nd2O3、Dy2O3、Eu2O3In the mixture that forms of a kind of or at least two.
Wherein, described Nucleating Agent is TiO2、ZrO2、MoO3、Fe2O3、CaF2、P2O5, the mixture that forms of a kind of or at least two in ZnO.
Wherein, the particle size values of described leadless crystallizing glass powder is 3 μm-5 μm.
Wherein, described organic solvent is the mixture that a kind of or at least two in terpineol, butyl carbitol, butyl carbitol acetate, tributyl citrate, GBL, mixed dibasic acid ester, N-Methyl pyrrolidone forms.
Wherein, described macromolecule thickener is the mixture that a kind of or at least two in ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, NC Nitroncellulose, polyvinyl alcohol, polyvinyl butyral resin, polyvinylpyrrolidone forms.
Wherein, described dispersant is the mixture that a kind of or at least two in triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae-dihydroxy sulfanilic acid forms.
Wherein, described defoamer is the one in polydimethylsiloxane, organic silicon modified by polyether, and described thixotropic agent is the one in castor oil hydrogenated, polyamide wax.
A kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, includes following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, Nucleating Agent mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, the weight portion of seven kinds of materials is followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10% in Nucleating Agent, then at smelting furnace melting after mix homogeneously, smelting temperature is 1100 DEG C-1500 DEG C, temperature retention time is namely obtain glass melts in 3-6 hour, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 4-6 hour, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: by organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting the content of macromolecule thickener, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, sintering aids, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 200Pa s ± 20Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, sintering aids, four kinds of materials of organic carrier weight portion be followed successively by 60%-70%, 10%-15%, 0.5%-5%, 10%-29.5%.
The invention have the benefit that a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry of the present invention, it includes the material of following weight portion, particularly as follows: function phase 60%-70%, inorganic adhesive phase 10%-15%, sintering aids 0.5%-5%, organic carrier 10%-29.5%；Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%；Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3, the mixture that forms of rare earth oxide, Nucleating Agent, inorganic adhesive mutually in SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, seven kinds of materials of Nucleating Agent weight portion be followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10%；Organic carrier is the mixture that organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent form, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%.By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry sheet resistance of the present invention is low and adjustable, temperature-coefficient of electrical resistance is relatively low and adjustable, printing characteristic and burn till characteristic good, and can match with insulating stainless steel substrate.
Another of the present invention has the beneficial effect that a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method of the present invention, and it includes following processing step, particularly as follows: a, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, Nucleating Agent mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, the weight portion of seven kinds of materials is followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10% in Nucleating Agent, then at smelting furnace melting after mix homogeneously, smelting temperature is 1100 DEG C-1500 DEG C, temperature retention time is namely obtain glass melts in 3-6 hour, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 4-6 hour, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；C, prepare organic carrier: by organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting the content of macromolecule thickener, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%；Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, sintering aids, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 200Pa s ± 20Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, sintering aids, four kinds of materials of organic carrier weight portion be followed successively by 60%-70%, 10%-15%, 0.5%-5%, 10%-29.5%.Being designed by above-mentioned processing step, the medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method of the present invention can produce effectively prepares above-mentioned medium or low resistance section large power thick film circuit rare earth resistance slurry.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described.
Embodiment one, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Zinc powder 2.5%
Organic carrier 12.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 95%, 5%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、CeO2、TiO2The mixture formed, inorganic adhesive is middle SiO mutually2、CaO、B2O3、A12O3、Bi2O3、CeO2、TiO2The weight portion of seven kinds of materials is followed successively by 40%, 15%, 15%, 12%, 13%, 2.5%, 2.5%；
Organic carrier is the mixture that terpineol, ethyl cellulose, triammonium citrate, polydimethylsiloxane, castor oil hydrogenated form, terpineol in organic carrier, ethyl cellulose, triammonium citrate, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment one has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、CeO2、TiO2Prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide CeO2Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment one can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、CeO2、TiO2Mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、CeO2、TiO2In the weight portion of seven kinds of materials be followed successively by 40%, 15%, 15%, 12%, 13%, 2.5%, 2.5%, then at smelting furnace melting after mix homogeneously, smelting temperature is 1200 DEG C, temperature retention time is namely obtain glass melts in 3 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 95%, 5%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: dissolve to obtain organic carrier in 80 DEG C of water-baths by terpineol, ethyl cellulose, triammonium citrate, polydimethylsiloxane, castor oil hydrogenated, and by adjusting the content of ethyl cellulose, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, terpineol in organic carrier, ethyl cellulose, triammonium citrate, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, zinc powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, zinc powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 2.5%, 12.5%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment one effectively.
Embodiment two, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Zinc powder 1%
Organic carrier 14%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 96%, 4%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、Sm2O3、ZrO2The mixture formed, inorganic adhesive is middle SiO mutually2、CaO、B2O3、A12O3、Bi2O3、Sm2O3、ZrO2The weight portion of seven kinds of materials is followed successively by 45%, 12%, 13%, 14%, 11%, 3%, 2%；
Organic carrier is the mixture that N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, polydimethylsiloxane, castor oil hydrogenated form, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 16%, 2%, 1%, 1%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment two has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、Sm2O3、ZrO2Prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide Sm2O3Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment two can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、Sm2O3、ZrO2Mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、Sm2O3、ZrO2In the weight portion of seven kinds of materials be followed successively by 45%, 12%, 13%, 14%, 11%, 3%, 2%, then at smelting furnace melting after mix homogeneously, smelting temperature is 1400 DEG C, temperature retention time is namely obtain glass melts in 4 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 96%, 4%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: dissolve to obtain organic carrier in 80 DEG C of water-baths by N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, polydimethylsiloxane, castor oil hydrogenated, and by adjusting the content of polyvinylpyrrolidone, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 16%, 2%, 1%, 1%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, zinc powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, zinc powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 1%, 14%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment two effectively.
Embodiment three, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Aluminium powder 2.5%
Organic carrier 12.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 97%, 3%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、Gd2O3、P2O5The mixture formed, inorganic adhesive is middle SiO mutually2、CaO、B2O3、A12O3、Bi2O3、Gd2O3、P2O5The weight portion of seven kinds of materials is followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%；
Organic carrier be N-Methyl pyrrolidone, polyvinylpyrrolidone, 1, the mixture that 4-dihydroxy sulfanilic acid, polydimethylsiloxane, castor oil hydrogenated form, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, Isosorbide-5-Nitrae-dihydroxy sulfanilic acid, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment three has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、Gd2O3、P2O5Prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide Gd2O3Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment three can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、Gd2O3、P2O5Mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、Gd2O3、P2O5In the weight portion of seven kinds of materials be followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%, then at smelting furnace melting after mix homogeneously, smelting temperature is 1400 DEG C, temperature retention time is namely obtain glass melts in 4 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 97%, 3%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: by N-Methyl pyrrolidone, polyvinylpyrrolidone, 1,4-dihydroxy sulfanilic acid, polydimethylsiloxane, castor oil hydrogenated dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting the content of polyvinylpyrrolidone, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, Isosorbide-5-Nitrae-dihydroxy sulfanilic acid, polydimethylsiloxane, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, aluminium powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, aluminium powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 2.5%, 12.5%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment three effectively.
Embodiment four, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Zinc powder 2.5%
Organic carrier 12.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 95%, 5%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、Nd2O3、CAF2The mixture formed, inorganic adhesive is middle SiO mutually2、CaO、B2O3、A12O3、Bi2O3、Nd2O3、CAF2The weight portion of seven kinds of materials is followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%；
Organic carrier is the mixture that N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, castor oil hydrogenated form, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment four has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、Nd2O3、CAF2Prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide Nd2O3Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment four can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、Nd2O3、CAF2Mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、Nd2O3、CAF2In the weight portion of seven kinds of materials be followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%, then at smelting furnace melting after mix homogeneously, smelting temperature is 1400 DEG C, temperature retention time is namely obtain glass melts in 4 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 95%, 5%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: dissolve to obtain organic carrier in 80 DEG C of water-baths by N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, castor oil hydrogenated, and by adjusting the content of polyvinylpyrrolidone, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of castor oil hydrogenated weight portion be followed successively by 80%, 17%, 1%, 1%, 1%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, zinc powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, zinc powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 2.5%, 12.5%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment four effectively.
Embodiment five, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Aluminium powder 2.5%
Organic carrier 12.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 96%, 4%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、Dy2O3, the mixture that forms of ZnO, inorganic adhesive mutually in SiO2、CaO、B2O3、A12O3、Bi2O3、Dy2O3, seven kinds of materials of ZnO weight portion be followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%；
Organic carrier is the mixture that N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, polyamide wax form, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of polyamide wax weight portion be followed successively by 75%, 22%, 1.5%, 1%, 0.5%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment five has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、Dy2O3, ZnO prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide Dy2O3Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment five can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、Dy2O3, ZnO mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、Dy2O3, the weight portion of seven kinds of materials is followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5% in ZnO, then at smelting furnace melting after mix homogeneously, smelting temperature is 1400 DEG C, temperature retention time is namely obtain glass melts in 5 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 96%, 4%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: dissolve to obtain organic carrier in 80 DEG C of water-baths by N-Methyl pyrrolidone, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, polyamide wax, and by adjusting the content of polyvinylpyrrolidone, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, N-Methyl pyrrolidone in organic carrier, polyvinylpyrrolidone, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of polyamide wax weight portion be followed successively by 75%, 22%, 1.5%, 1%, 0.5%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, aluminium powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, aluminium powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 2.5%, 12.5%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment five effectively.
Embodiment six, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry, include the material of following weight portion, particularly as follows:
Function phase 70%
Inorganic adhesive phase 15%
Zinc powder 2.5%
Organic carrier 12.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 98%, 2%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3、Eu2O3, the mixture that forms of ZnO, inorganic adhesive mutually in SiO2、CaO、B2O3、A12O3、Bi2O3、Eu2O3, seven kinds of materials of ZnO weight portion be followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5%；
Organic carrier is the mixture that N-Methyl pyrrolidone, polyvinyl butyral resin, polymethyl acid amide, organic silicon modified by polyether, polyamide wax form, N-Methyl pyrrolidone in organic carrier, polyvinyl butyral resin, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of polyamide wax weight portion be followed successively by 75%, 22%, 1%, 1%, 1%.
By above-mentioned material proportion, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment six has the following advantages, particularly as follows:
1, SiO is selected2、CaO、B2O3、A12O3、Bi2O3、Eu2O3, ZnO prepare leadless crystallizing glass powder body system, and then avoid the plumbous injury after researching and developing, using and be discarded, environment, human body caused, high-power resistance or heating manufacturing urgent problem can be solved, meet RoHS Directive (2002/95/EC) requirement；
2, rare earth oxide Eu2O3Microcrystal glass material and the sintering character of function phase, microstructure, consistency, phase composition and physical and mechanical property can be changed greatly, the compatibility of slurry, wettability, hot property, electrical property, manufacturability, adaptability is made to have a significant improvement raising, while regulating resistance slurry sintering temperature, effectively regulate sheet resistance scope and the temperature-coefficient of electrical resistance of resistive layer；
3, by the silver-ruthenic oxide composite powder of leadless crystallizing glass powder body system and proper proportion and organic carrier compound, add sintering aids simultaneously, prepare medium or low resistance section, the coefficient of expansion of resistor track layer mates with stainless steel substrate and the rare earth thick film circuit resistance slurry of good combination；
4, based on the printing characteristic of stainless steel substrate medium or low resistance section rare earth thick film circuit resistance slurry and burn till characteristic good, reheating rate of change less than 5%, the preparation of this resistance slurry have that sheet resistance is low and adjustable, temperature-coefficient of electrical resistance is low and adjustable and with the advantage such as the compatibility having had based on stainless steel substrate thick film circuit dielectric paste, electrocondution slurry.
Wherein, the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment six can adopt following preparation method to be prepared from, concrete, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3、Eu2O3, ZnO mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3、Eu2O3, the weight portion of seven kinds of materials is followed successively by 55%, 10%, 10%, 10%, 10%, 2.5%, 2.5% in ZnO, then at smelting furnace melting after mix homogeneously, smelting temperature is 1400 DEG C, temperature retention time is namely obtain glass melts in 5 hours, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 6 hours, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 98%, 2%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: dissolve to obtain organic carrier in 80 DEG C of water-baths by N-Methyl pyrrolidone, polyvinyl butyral resin, polymethyl acid amide, organic silicon modified by polyether, polyamide wax, and by adjusting the content of polyvinyl butyral resin, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, N-Methyl pyrrolidone in organic carrier, polyvinyl butyral resin, polymethyl acid amide, organic silicon modified by polyether, five kinds of materials of polyamide wax weight portion be followed successively by 75%, 22%, 1%, 1%, 1%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, zinc powder, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 150Pa s-200Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, zinc powder, four kinds of materials of organic carrier weight portion be followed successively by 70%, 15%, 2.5%, 12.5%.
Being designed by above-mentioned processing step, this medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method production can prepare the medium or low resistance section large power thick film circuit rare earth resistance slurry of the present embodiment six effectively.
Above content is only presently preferred embodiments of the present invention, for those of ordinary skill in the art, according to the thought of the present invention, all will change in specific embodiments and applications, and this specification content should not be construed as limitation of the present invention.
Claims (10)
1. a medium or low resistance section large power thick film circuit rare earth resistance slurry, it is characterised in that include the material of following weight portion, particularly as follows:
Function phase 60%-70%
Inorganic adhesive phase 10%-15%
Sintering aids 0.5%-5%
Organic carrier 10%-29.5%；
Function composite powder for being made up of nanometer silver powder, ruthenic oxide powder mutually, the particle size values of nanometer silver powder is 20nm-50nm, the particle size values of ruthenic oxide powder is 1 μm-3 μm, function mutually in nanometer silver powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%；
Inorganic adhesive is leadless crystallizing glass powder mutually, and leadless crystallizing glass powder is by SiO2、CaO、B2O3、A12O3、Bi2O3, the mixture that forms of rare earth oxide, Nucleating Agent, inorganic adhesive mutually in SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, seven kinds of materials of Nucleating Agent weight portion be followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10%；
Organic carrier is the mixture that organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent form, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%.
2. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 1, it is characterised in that: described sintering aids is the mixture that a kind of or at least two in zinc, stannum, aluminum, cobalt, antimony, zinc compound, tin compound, aluminium compound, cobalt compound, antimonial forms.
3. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 2, it is characterised in that: described rare earth oxide is CeO2、Sm2O3、Gd2O3、Nd2O3、Dy2O3、Eu2O3In the mixture that forms of a kind of or at least two.
4. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 3, it is characterised in that: described Nucleating Agent is TiO2、ZrO2、MoO3、Fe2O3、CaF2、P2O5, the mixture that forms of a kind of or at least two in ZnO.
5. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 4, it is characterised in that: the particle size values of described leadless crystallizing glass powder is 3 μm-5 μm.
6. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 5, it is characterized in that: described organic solvent is the mixture that a kind of or at least two in terpineol, butyl carbitol, butyl carbitol acetate, tributyl citrate, GBL, mixed dibasic acid ester, N-Methyl pyrrolidone forms.
7. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 6, it is characterised in that: described macromolecule thickener is the mixture that a kind of or at least two in ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, NC Nitroncellulose, polyvinyl alcohol, polyvinyl butyral resin, polyvinylpyrrolidone forms.
8. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 7, it is characterized in that: described dispersant is the mixture that a kind of or at least two in triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae-dihydroxy sulfanilic acid forms.
9. a kind of medium or low resistance section large power thick film circuit rare earth resistance slurry according to claim 8, it is characterized in that: described defoamer is the one in polydimethylsiloxane, organic silicon modified by polyether, described thixotropic agent is the one in castor oil hydrogenated, polyamide wax.
10. a medium or low resistance section large power thick film circuit rare earth resistance slurry preparation method, it is characterised in that include following processing step, particularly as follows:
A, prepare inorganic adhesive phase: by SiO2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, Nucleating Agent mix homogeneously in three-dimensional material mixer, SiO in mixture2、CaO、B2O3、A12O3、Bi2O3, rare earth oxide, the weight portion of seven kinds of materials is followed successively by 20%-70%, 10%-50%, 1%-15%, 5%-30%, 10%-30%, 1%-10%, 1%-10% in Nucleating Agent, then at smelting furnace melting after mix homogeneously, smelting temperature is 1100 DEG C-1500 DEG C, temperature retention time is namely obtain glass melts in 3-6 hour, then glass melts carried out shrend and obtain glass, last with distilled water for medium to glass ball milling 4-6 hour, namely obtain the leadless crystallizing glass powder that particle size values is 3 μm-5 μm；
B, preparation function phase: by nanometer silver powder, ruthenic oxide powder mix homogeneously to prepare silver-ruthenic oxide composite powder, nanometer silver powder in silver-ruthenic oxide composite powder, two kinds of materials of ruthenic oxide powder weight portion be followed successively by 80%-95%, 5%-20%, the particle size values of nanometer silver powder is 20nm-50nm, and the particle size values of ruthenic oxide powder is 1 μm-3 μm；
C, prepare organic carrier: by organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting the content of macromolecule thickener, so that the viscosity of organic carrier controls within the scope of 200mPa s-300mPa s, wherein, organic solvent in organic carrier, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent weight portion be followed successively by 70%-80%, 15%-20%, 1%-5%, 1%-5%, 1%-5%；
Prepared by d, resistance slurry: by function phase, inorganic adhesive phase, sintering aids, organic carrier dispersed with stirring in container, then carry out three-roll rolling again, to obtain the range of viscosities resistance slurry for 200Pa s ± 20Pa s, wherein, function phase in resistance slurry, inorganic adhesive phase, sintering aids, four kinds of materials of organic carrier weight portion be followed successively by 60%-70%, 10%-15%, 0.5%-5%, 10%-29.5%.
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