CN110246605A - A kind of anti-oxidative conductive paste composition and conductive coating and preparation method thereof - Google Patents
A kind of anti-oxidative conductive paste composition and conductive coating and preparation method thereof Download PDFInfo
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- CN110246605A CN110246605A CN201910371335.7A CN201910371335A CN110246605A CN 110246605 A CN110246605 A CN 110246605A CN 201910371335 A CN201910371335 A CN 201910371335A CN 110246605 A CN110246605 A CN 110246605A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The invention belongs to technical field of material, and in particular to a kind of anti-oxidative conductive paste composition and conductive coating and preparation method thereof.The conductive paste composition contains by weight: 75-95 parts of boron nickel powder, 5-15 parts of boracic inorganic binder, 1-5 parts of organic carrier, 10-30 parts of solvent, the boron nickel powder is the conductive metal powder that surface is coated with nickel boron, wherein, boron content is 2-8% in boron nickel powder；Boron content 2-20% in the boracic inorganic binder.The conductive paste composition may be implemented to be sintered under air atmosphere, have extremely excellent antioxygenic property；It can be sintered at 600 degree or so, technique for applying is simple, and low energy consumption for process；Have the characteristics that at low cost, good conductivity, adhesive force are good by the conductive coating that the conductive paste composition is prepared, can be widely applied to RFID antenna production.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of anti-oxidative conductive paste composition and conductive painting
Layer and preparation method thereof.
Background technique
Electrocondution slurry can be widely applied to the row such as solar battery, electronic tag, ceramic capacitor using extremely wide
As the core material of electrode fabrication in industry.Currently, due to the good conductivity of silver, conductive silver slurry is widely adopted.But it is silver-colored
Expensive for precious metal material, silver paste application cost is very high, and lowpriced metallization is the inexorable trend of electrocondution slurry future development.
Metallic nickel is from a wealth of sources, cheap, is had broad application prospects using the nickel base conductive pulp of nickel conductive metal powder development.
Such as prior art CN101290824A provides a kind of preparation method of nickel based conductive slurry, with sodium hypophosphite
The mixed solution of reduction nickel salt aqueous solution and aqueous solution of chromium salt prepares submicron order nickel chromium triangle mixed metal powder, in submicron order nickel chromium triangle
Mixed metal powder surface coats nano silver and nickel based metal powder is made.
A kind of Thick-film Nickel Conductive Paste of CN87100475A, group are divided into (weight %): boron powder 1.0~8.0, and aluminium powder 0.1~
1.0, zinc powder 0.5~3.0 and aequum nickel powder, the sum of each component are 100.
However, nickel base conductive pulp is easy to oxidize during the sintering process, even more it is difficult to be sintered in air atmosphere, develops novel
The nickel base conductive pulp with high anti-oxidation characteristic have highly important value and significance.
Summary of the invention
In view of the problems existing in the prior art, the present invention is achieved through the following technical solutions:
A kind of anti-oxidative conductive paste composition provided by the invention, the conductive paste composition contain: boron nickel powder 75-
95 parts, 5-15 parts of boracic inorganic binder, 1-5 parts of organic carrier, 10-30 parts of solvent, which is characterized in that the boron nickel powder is
Surface is coated with the conductive metal powder of nickel boron, wherein boron content is 2-8% in boron nickel powder；The boracic is inorganic
Boron content 2-15% in binder.
Conductive metal powder in electrocondution slurry is mostly important, pure nickel metal powder, if being sintered in air atmosphere,
Spontaneous combustion can occur, become the oxide of nickel after being oxidized by oxygen, and the electric conductivity of the oxide of nickel is very poor, this is highly detrimental to
Form the conductive coating of high conductivity, it is difficult to meet application requirement.This patent uses boron nickel powder for the conductive metal powder of core,
This powder is the conductive metal powder that surface is coated with nickel boron, with good oxidation resistance, while by its table
The interfacial wettability of metal powder and boracic inorganic binder and compatible can be substantially improved in the boron in face in high-temperature sintering process
Property, further increase the oxidation resistance of nickel.
Boron content is too low in this kind of boron nickel powder conductive metal powder, and especially less than 2%, this kind of metal powder can be made
Last oxidation resistance is poor, it is difficult to it is sintered in air atmosphere, boron content is excessively high in this kind of boron nickel powder conductive metal powder,
Especially higher than 8%, this kind of metal powder surface anti oxidation layer can be made blocked up, influence whether metal powder and metal powder it
Between contact, be unfavorable for forming the conductive coating of high conductivity.This kind of boron nickel powder conductive metal powder content is too low, especially low
If 75 parts, it may result in conductive coating conductive network and build imperfect, electric conductivity is bad, this kind of boron nickel powder conductive metal
Content of powder is excessively high, and if especially higher than 95 powder, it is bad with substrate bonding to may result in conductive coating, is easy to fall off.
Inorganic binder (being commonly called as glass powder) in electrocondution slurry primarily serves cementation, on the one hand can be by conductive phase
It is bonded together to form conductive path, conductive coating and substrate are bonded together by still further aspect, boracic of the present invention
Inorganic binder, boron element can be present in boracic inorganic binder in the form of pure boron, boron oxide, boracic metal oxide etc.
In the middle, wherein convenient scheme is that boron element exists in the form of boron oxide.
Boron content is too low in boracic inorganic binder, and especially less than 2%, it will reduce conductive coating sintering process
The oxidation resistance of middle slurry, boron content is excessively high in boracic inorganic binder, and especially higher than 15%, it will reduce conductive
Cohesive force between coating and substrate.
As a preferred technical solution of the present invention, the nickel boron contains NiB, Ni2B、Ni3At least one of B
(preferred mass ratio is 1:0.1-2)；Boron content is 4-6% in the boron nickel powder；The boracic inorganic binder
Middle boron content is 5-10%.Foregoing advantages are best.
As a preferred technical solution of the present invention, in the present invention, boracic inorganic binder can select boron oxide
7-25%, zinc oxide 10-14%, silica 3-5%, aluminium oxide 0.2-1.5%, lanthana 05-1.5%, lithia 0.5-
1.5%, remaining be bismuth oxide system, can also select boron oxide 7-30%, zinc oxide 3-6%, aluminium oxide 0.2-1.5%,
Copper oxide 0.5-1.5%, sodium oxide molybdena 0.5-2%, the system that remaining is lead oxide.The boracic inorganic binder can pass through city
Acquisition is sold, can also voluntarily be modulated, but the present invention is not limited to this.
Organic carrier (sometimes referred to as organic bond) in electrocondution slurry, can be by conductive phase and the nothing for being used as bonding
Machine binder (being commonly called as glass powder) and the mixing of other solid powders are dispersed into paste slurry, and main function is to improve gluing for slurry
Consistence and plasticity.In the more suitable scheme of the present invention, it is contemplated that second is selected in cost, the feature of environmental protection and performance, organic carrier suggestion
Based on base cellulose, methylcellulose etc., but the present invention is not limited to this.
Organic carrier content is too low, if especially less than 1 part, does not have the apparent effect for increasing system toughness,
Organic carrier too high levels if especially higher than 5 parts, can make system excessively sticky, inconvenience construction.
Solvent in electrocondution slurry primarily serves the effect of adjustment conductive paste composition viscosity and volatility, passes through tune
The content and classification of whole solvent reach the working viscosity requirement for being applicable in different coated techniques and equipment, while being adjusted by solvent
Whole conductive paste composition is in drying and sintering process, the planarization of coating surface, if solvent boiling point is too low, work progress
May exist due to the too fast caused related defects of drying, if solvent boiling point is excessively high, so that conductive paste composition is dry
Slowly, it may result in sintering process and generate related defects, influence coated conductive and adhesive force.The more suitable side of the present invention
In case, it is contemplated that cost, the feature of environmental protection and performance, solvent suggestion select terpinol, based on gylcol ether etc., but the present invention not office
It is limited to this.
Organic solvent content is too low, if especially less than 10 parts, is unfavorable for the dissolution of organic carrier, can also make system
It is excessively sticky, it is unfavorable for construction in later period, organic carrier too high levels if especially higher than 30 parts, can make system liquidity
Very good, application property is also bad, and later period application volatilization is difficult.
As a preferred technical solution of the present invention, surface is coated with the particle size range of the conductive metal powder of nickel boron
It is 0.5-5 microns.The core of conductive metal powder is nickel or at least one of nickeline or ambrose alloy.It can be by physics or chemical
Synthesizing mean obtain this conductive metal powder, existing powder in the market can also be bought, also can purchase existing in the market
Nickel or nickeline or ambrose alloy powder, then by physics or chemical means carry out the processing of surface cladding, obtain this conductive metal
Powder.
The material of this grain size specification is selected, mainly considers actual application.Partial size is too small, granule surface area compared with
Greatly, easy to oxidize in later period sintering process, partial size is too big, and the fineness of conductive paste composition can be made bigger than normal.Conductive metal
The core of powder must be nickeliferous, and nickel and surface cover nickel boron have measured compatibility, and only core is nickeliferous could make conduction
The core and clad interface cohesion of metal powder are good, are also beneficial to the raising of its oxidation resistance.
Another object of the present invention is to provide a kind of preparation method of conductive coating, which includes: will be aforementioned
Anti-oxidative conductive paste composition applied on substrate；After toasting 20-40min under 100-150 degree, in 600-800 degree
Lower sintering 10-40min obtains conductive coating.
A further object of the present invention is to provide a kind of conductive coatings, which is characterized in that the conductive coating system above-mentioned
Preparation Method is prepared.
The coating can be sintered at 600 degree or so, good conductivity, and resistance is less than 75 millis in specific optimal technical scheme
Europe/, adhesive force is good, and adhesive force is 0 grade in specific optimal technical scheme.
Compared with the prior art, the beneficial effects of the invention include:
(1) conductive paste composition may be implemented to be sintered under air atmosphere, have extremely excellent antioxygenic property；
(2) conductive paste composition can be sintered at 600 degree or so, and technique for applying is simple, and low energy consumption for process；
(3) conductive coating has the characteristics that at low cost, good conductivity, adhesive force are good, can be widely applied to RFID days
Line production.
Specific embodiment
The present invention is explained combined with specific embodiments below, but the present invention is not limited to this.
Embodiment 1
A kind of anti-oxidative conductive paste composition, by weight, comprising: 75 parts of boron nickel powder, boracic inorganic binder (oxygen
Change boron 7-25%, zinc oxide 10-14%, silica 3-5%, aluminium oxide 0.2-1.5%, lanthana 05-1.5%, lithia
0.5-1.5%, the system that remaining is bismuth oxide) 5 parts, 1.5 parts of organic carrier (ethyl cellulose), 15 parts of solvent (terpinol),
Wherein the boron nickel powder is the conductive metal powder that surface is coated with nickel boron, and core is nickel.Boron nickel powder surface contains NiB, boron nickel
Boron content 2.2% in powder, boron content 4% in boracic inorganic binder.
By above-mentioned conductive paste composition in alumina ceramic plate surface coating filmform, 40min is toasted under 100 degree, then
It is sintered 40min under 600 degree, obtains conductive coating of the present invention.
Embodiment 2
A kind of anti-oxidative conductive paste composition, by weight, comprising: 95 parts of boron nickel powder, boracic inorganic binder (oxygen
Change boron 15%, zinc oxide 12%, silica 5%, aluminium oxide 1.5%, lanthana 0.5%, lithia 1%, remaining be bismuth oxide
System) 15 parts, 4.5 parts of organic carrier (ethyl cellulose), 30 parts of solvent (terpinol), wherein the boron nickel powder is surface
It is coated with the conductive metal powder of nickel boron, core is nickel.Boron nickel powder surface contains NiB and Ni2B (mass ratio 1:1), boron nickel
Boron content 7% in powder, boron content 10% in boracic inorganic binder.
By above-mentioned conductive paste composition in alumina ceramic plate surface coating filmform, 20min is toasted under 150 degree, then
It is sintered 10min under 800 degree, obtains conductive coating of the present invention.
Embodiment 3
A kind of anti-oxidative conductive paste composition, by weight, comprising: 80 parts of boron nickel powder, boracic inorganic binder (oxygen
Change boron 30%, zinc oxide 5%, aluminium oxide 0.2%, copper oxide 0.5%, sodium oxide molybdena 2%, the system that remaining is lead oxide) 7.5
Part, 3 parts of organic carrier (methylcellulose), 20 parts of solvent (terpinol), wherein the boron nickel powder is that surface is coated with nickel
The conductive metal powder of boron, core are nickeline.Boron nickel powder surface contains NiB and Ni2B (mass ratio 1:2), boron member in boron nickel powder
Cellulose content 5%, boron content 7.5% in boracic inorganic binder.
By above-mentioned conductive paste composition in alumina ceramic plate surface coating filmform, 30min is toasted under 120 degree, then
It is sintered 15min under 700 degree, obtains conductive coating of the present invention.
Comparative example 1
A kind of anti-oxidative conductive paste composition, by weight, comprising: 80 parts of nickel powder, inorganic binder (specially oxygen
Change boron 12%, zinc oxide 6%, aluminium oxide 1%, copper oxide 1%, sodium oxide molybdena 2%, the system that remaining is lead oxide) 7.5 parts, have
Airborne 3 parts of body (methylcellulose), 20 parts of solvent (terpinol).
By above-mentioned conductive paste composition in alumina ceramic plate surface coating filmform, 30min is toasted under 120 degree, then
It is sintered 15min under 700 degree, obtains conductive coating.
Embodiment 4
Performance detection, testing result are as follows:
Table 1 is embodiment and comparative example, correlated performance comparison
| Serial number | Coated conductive | Coating adhesion |
| Embodiment 1 | Sheet resistance: 75 milliohms/ | 0 grade |
| Embodiment 2 | Sheet resistance: 55 milliohms/ | 0 grade |
| Embodiment 3 | Sheet resistance: 25 milliohms/ | 0 grade |
| Comparative example 1 | It is non-conductive | 2 grades |
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of anti-oxidative conductive paste composition, which is characterized in that by weight, comprising: 75-95 parts of boron nickel powder contains
5-15 parts of boron inorganic binder, 1-5 parts of organic carrier, 10-30 parts of solvent, which is characterized in that the boron nickel powder is surface packet
It is covered with the conductive metal powder of nickel boron, wherein boron content is 2-8% in boron nickel powder；The boracic inorganic binder
Middle boron content 2-15%.
2. anti-oxidative conductive paste composition according to claim 1, which is characterized in that the nickel boron contains
NiB、Ni2B、Ni3At least one of B；Boron content is 4-6% in the boron nickel powder；The boracic inorganic binder
Middle boron content is 5-10%.
3. anti-oxidative conductive paste composition according to claim 1, which is characterized in that the boracic inorganic binder
Select boron oxide 7-25%, zinc oxide 10-14%, silica 3-5%, aluminium oxide 0.2-1.5%, lanthana 05-1.5%, oxygen
Change lithium 0.5-1.5%, the system that remaining is bismuth oxide；Or select boron oxide 7-30%, zinc oxide 3-6%, aluminium oxide 0.2-
1.5%, copper oxide 0.5-1.5%, sodium oxide molybdena 0.5-2%, the system that remaining is lead oxide.
4. anti-oxidative conductive paste composition according to claim 1, which is characterized in that the organic carrier is selected from second
Base cellulose, methylcellulose.
5. anti-oxidative conductive paste composition according to claim 1, which is characterized in that the solvent is selected from pine tar
Alcohol, glycol ether.
6. anti-oxidative conductive paste composition according to claim 1, which is characterized in that surface is coated with nickel boron
The particle size range of conductive metal powder is 0.5-5 microns, and the core of conductive metal powder is at least one in nickel or nickeline or ambrose alloy
Kind.
7. a kind of preparation method of conductive coating, which is characterized in that the preparation method includes: by any one of claim 1-6 institute
The anti-oxidative conductive paste composition stated applies on substrate；After toasting 20-40min under 100-150 degree, in 600-800
Degree is lower to be sintered 10-40min, obtains conductive coating.
8. a kind of conductive coating, which is characterized in that the conductive coating is prepared by preparation method according to any one of claims 8
It arrives.
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| CN201910371335.7A CN110246605B (en) | 2019-05-06 | 2019-05-06 | Anti-oxidation conductive paste composition, conductive coating and preparation method of conductive coating |
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| CN201910371335.7A CN110246605B (en) | 2019-05-06 | 2019-05-06 | Anti-oxidation conductive paste composition, conductive coating and preparation method of conductive coating |
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| CN110246605B CN110246605B (en) | 2021-01-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114255904A (en) * | 2021-11-26 | 2022-03-29 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Nickel electrode paste, resistor and preparation method of resistor |
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| US4070517A (en) * | 1976-07-08 | 1978-01-24 | Beckman Instruments, Inc. | Low fired conductive compositions |
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| US4016447A (en) * | 1974-11-13 | 1977-04-05 | E. I. Du Pont De Nemours And Company | Dielectric substrate bearing nickel boride conductor |
| US4070517A (en) * | 1976-07-08 | 1978-01-24 | Beckman Instruments, Inc. | Low fired conductive compositions |
| CN1405791A (en) * | 2001-09-20 | 2003-03-26 | 株式会社村田制作所 | Conductive paste, lamina ceramic electronic element producing method and lamina ceramic electronic element |
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| CN114255904A (en) * | 2021-11-26 | 2022-03-29 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Nickel electrode paste, resistor and preparation method of resistor |
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