CN106098150A - The inductor ends of low-temperature sintering low silver content is coated with formula of silver slurry and preparation method thereof - Google Patents
The inductor ends of low-temperature sintering low silver content is coated with formula of silver slurry and preparation method thereof Download PDFInfo
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- CN106098150A CN106098150A CN201610764561.8A CN201610764561A CN106098150A CN 106098150 A CN106098150 A CN 106098150A CN 201610764561 A CN201610764561 A CN 201610764561A CN 106098150 A CN106098150 A CN 106098150A
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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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- 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
Abstract
The invention discloses the present invention provides the inductor ends of a kind of low-temperature sintering low silver content to be coated with silver-colored formula starched and preparation method thereof, this chip inductor end is coated with silver slurry and is mainly made up of argentum powder, glass dust, inorganic fillings and organic carrier, organic carrier is made up of ethyl cellulose, anti-sag agent, polyvinyl butyral resin, acrylic resin and organic solvent four part, and argentum powder uses high dispersiveness spherical argentum powder, the argentum powder of part flaking and flake silver powder three part composition.By three-roll grinder, argentum powder, glass dust, inorganic fillings and organic carrier are fully ground mixing disperse i.e. to obtain chip inductor end painting silver slurry；It is full that the chip inductor end that the inventive method provides is coated with silver layer densification after silver-colored slurry has sintering, and corner angle do not leak porcelain, and end is coated with flat side down and does not stay extension, and sheet resistance is low, inducer good electrical property after end painting, the advantages such as function admirable such as adhesion is high.
Description
Technical field
The present invention relates to microelectronics electrode material field, particularly relate to the lamellar inductor of different model.
Background technology
Chip inductor end is coated with silver slurry makes the interior electrode of chip inductor draw from end as a kind of low-temperature sintering
Electrode silver plasm.Be coated with silver slurry with common chip inductor ends compared with, this silver slurry has low silver content 50%～60%, low-temperature sintering 550
DEG C～650 DEG C, can reduce the production cost of user, and the end of this silver slurry to be coated with effect graceful, end face silver layer is fine and close, side
Silver layer is smooth, and corner angle go out silver layer and wrap up the tight quality from product of having deducted a percentage in appearance, and being applied to that silver layer can be included board is various
Prepared by the termination electrode of chip inductor.
Chip inductor end be coated with silver slurry be typically made up of argentum powder, glass powder, inorganic fillings, organic carrier etc., with
Make during chip inductor termination electrode, to need good electrical property and extraordinary bond strength.Chip inductor end is coated with silver slurry at present
In use, low silver content is all liked using by most use producers, and low sintering silver slurry product is to reduce the life of product
Produce cost, so it will be a development trend that low silver content end is coated with silver slurry；The end of current domestic patent literature is coated with silver slurry base
Only focusing on glass powder and the organic carrier moieties of silver slurry in basis, of inadequate achievement do not have opposite end to be coated with silver slurry inorganic fillings, anti-current
Hang agent and argentum powder composition through going too many work.
Summary of the invention
Goal of the invention: the deficiency existed for prior art, the present invention provides the inductance of a kind of low-temperature sintering low silver content
Device end is coated with formula of silver slurry and preparation method thereof, this formula and preparation method advantages of simple, and prepared end is coated with silver slurry and has end
Painting effect is graceful, and silver layer sintering rear end face silver layer is fine and close, and side silver layer is smooth, good electrical property, and adhesion is high, resistance to soldering heat performance
Excellent advantage.
Technical scheme: the inductor ends of a kind of low-temperature sintering low silver content is coated with the formula of silver slurry, and the component of silver paste is
Organic carrier, ball shape silver powder, part flaking argentum powder, flake silver powder, lead-free glass powder and inorganic filler, wherein, have airborne
Weight mark is 20%～30%, and ball shape silver powder mass fraction is 10%～40%, and part flaking quality of cathode silver mark is
10%～40%, flake silver powder mass fraction is 1%～20%, and lead-free glass powder mass fraction is 5%～15%, inorganic fill
Thing mass fraction is 5%～15%；
Described ball shape silver powder particle diameter is 0.1～3 μm, and part flaking argentum powder particle diameter is 2 μm～5 μm, the grain of flake silver powder
Footpath is 2 μm～8 μm, and the particle size distribution range of inorganic fillings is 1～5 μm.
Specifically, the component of described lead-free glass powder and mass fraction are silicon dioxide 8%～10%, zinc oxide 15%～
25%, antimony oxide 1%～3%, bismuth oxide 40%～60% and diboron trioxide 5%～10%.
Specifically, during described inorganic filler is iron sesquioxide, nikel powder, nickel oxide powder, copper powder and cupric oxide powder one
Kind or several assemblys.
More specifically, described organic carrier is made up of thixotropic agent, anti-sag agent and organic solvent；Wherein, thixotropic agent
For based on ethyl cellulose, also include polyethylene acetal butyral and acrylic resin；Organic solvent by butyl carbitol,
Butyl carbitol acetate, terpineol, tributyl citrate forms.
More specifically, the component of described organic carrier and mass fraction: the mass fraction of ethyl cellulose be 5%～
10%, the mass fraction of polyvinyl butyral resin is 1%～2%, and the mass fraction of acrylic resin is 0.5%～2%, Oleum Pini
The mass fraction of alcohol is 20%～40%, and the mass fraction of butyl carbitol is 20%～40%, butyl carbitol acetate
Mass fraction is 20%～40%, and the mass fraction of tributyl citrate is 5%～10%, and anti-sag agent mass fraction is
0.1%～0.5%.
Specifically, described anti-sag agent is bentonite, organobentonite, nano-aluminium oxide, nano silicon, illiteracy
One or more combination in de-stone forms.
The inductor ends of described low-temperature sintering low silver content is coated with the preparation method of silver slurry, including the system of described organic carrier
The standby component according to above-mentioned organic carrier and mass fraction proportioning configuration raw material, heat under the conditions of 60～90 DEG C and stir always
Mixing, becoming transparent molten silver until being completely dissolved；The preparation of described lead-free glass powder claims according to each component of above-mentioned lead-free glass powder
Take and stir with powder beater, being contained in alumina crucible and be positioned over melting in Muffle furnace, smelting temperature be 1200 DEG C～
1300 DEG C, it is incubated 0.5～1h, uses shrend to be cooled down by high-temperature liquid state glass, after drying, use ethanol as medium, planetary ball mill
Machine 300rmp ball milling 4h～6h, i.e. can obtain meeting the glass powder of size distribution requirements；Finally, end be coated with silver slurry preparation be by
Described organic carrier, ball shape silver powder, the ball shape silver powder of part flaking, flake silver powder, glass powder, inorganic filler is by upper
The proportioning stated uses batch mixer mix homogeneously, carries and uses three-high mill grinding distribution 8 times, and by terrible fineness≤5 μm, viscosity is 25
～the finished product end of 40Pa.s is coated with slurry.
Specifically, described glass dust is a kind of crown glass powder body meeting 550 DEG C～650 DEG C sintering.
Beneficial effect: compared with prior art, it is an advantage of the current invention that: the present invention use can gradient volatilization organic molten
Agent system, and in organic carrier, add solvable inorganic anti-sag agent, in the drying course of the end painting silver slurry being, bottom is relatively
Thick silver layer has the gradient volatilization of organic solvent be unlikely to cracking or have the possibility of cracking, the consistency after doing after promoting silver layer,
And owing to the addition of anti-sag agent substantially increases the aesthetics after silver slurry end is coated with；The glass that 550 DEG C～650 DEG C sintering use
System can make end be coated with silver slurry can well meet the agglomerant of different users at wider sintering temperature sintering
Skill；Due to ball shape silver powder, part flaking argentum powder and the ratio optimization of three kinds of argentum powder of flake silver powder and inorganic filler
It is full that use makes silver starch silver layer densification after sintering, can meet the inductor product of different size size.
Detailed description of the invention
Below in conjunction with detailed description of the invention, it is further elucidated with the present invention.
The inductor ends of a kind of low-temperature sintering low silver content is coated with formula of silver slurry and preparation method thereof, end be coated with silver by component
And mass fraction be organic carrier be 20%～30%, ball shape silver powder 10%～40%, part flaking argentum powder be 10%～
40%, flake silver powder is 1%～20%, and crown glass powder body is 5%～15%, and inorganic filler is 5%～15%；Wherein,
Ball shape silver powder particle diameter is 0.1～3 μm, and part flaking argentum powder particle diameter is 2 μm～5 μm, and the particle diameter of flake silver powder is 2 μm～8 μm；
The component of lead-free glass powder and mass fraction are silicon dioxide 8%～10%, zinc oxide 15%～25%, antimony oxide 1%
～3%, bismuth oxide 40%～60%, diboron trioxide 5%～10%；Inorganic fillings is iron sesquioxide, nikel powder, oxygen
Changing nikel powder, copper powder, the assembly of one or more in cupric oxide powder, the particle size distribution range of inorganic fillings is 1～5 μm；On
The inorganic fillings stated is the elemental composition in the ferrite ceramics that chip inductor uses, and so can make silver slurry in sintering process
Contraction and ferrite ceramics more mate, have been provided that more preferable electric current draw and adhesion；Lead-free glass powder is a kind of permissible
Meet the crown glass powder body of 550 DEG C～650 DEG C sintering
Organic carrier moieties is thixotropic agent, anti-sag agent and organic solvent composition, and wherein, thixotropic agent is with ethyl cellulose
Element is main body, and polyethylene acetal butyral and acrylic resin are slurry rheological property energy accelerator and improve slurry drying caudacoria layer
Compactness；Anti-sag agent is the one in bentonite, organobentonite, nano-aluminium oxide, nano silicon, montmorillonite
Or several cooperation forms；Organic solvent is butyl carbitol, butyl carbitol acetate, terpineol, and tributyl citrate presses one
The organic solvent combination solution of the gradient volatilization of certainty ratio composition；The component of organic carrier and mass fraction: ethyl cellulose
Mass fraction is 5%～10%, and the mass fraction of polyvinyl butyral resin is 1%～2%, and the mass fraction of acrylic resin is
0.5%～2%, the mass fraction of terpineol is 20%～40%, and the mass fraction of butyl carbitol is 20%～40%, butyl
The mass fraction of carbitol acetate is 20%～40%, and the mass fraction of tributyl citrate is 5%～10%, anti-sag agent
Mass fraction is 0.1%～0.5%.
Preparation method is:
1) ethyl cellulose, polyvinyl butyral resin, acrylic resin are substantially dissolved in a certain amount of organic solvent
Being configured to organic carrier, in organic carrier, the mass fraction of ethyl cellulose is 5%～10%, the quality of polyvinyl butyral resin
Mark is 1%～2%, and the mass fraction of acrylic resin is 0.5%～2%, and the mass fraction of terpineol is 20%～40%,
The mass fraction of butyl carbitol is 20%～40%, and the mass fraction of butyl carbitol acetate is 20%～40%, Fructus Citri Limoniae
The mass fraction of acid tributyl is 5%～10%, and anti-sag agent uses bentonite, organobentonite, nano-aluminium oxide, receives
Rice silicon dioxide, montmorillonite in one or more, consumption be mass fraction for 0.1%～0.5%；
2) use Muffle furnace smelting glass, use ball mill ball milling to be referred to as the ratio of certain particle size distribution in the glass after quenching
Example powder body；
The key component of glass dust is: silicon dioxide 8%～10%, zinc oxide 15%～25%, antimony oxide
1%～3%, bismuth oxide 40%～60%, diboron trioxide 5%～10%.
Smelting temperature is 1200 DEG C～1300 DEG C, is incubated 0.5～1h, and shrend post-drying uses ethanol as medium, uses
Planetary ball mill 300rmp ball milling 4h～6h, i.e. can obtain meeting the glass powder of size distribution requirements；
3) requirement of argentum powder: the surface area of spherical argentum powder is 3～4m2/ g, particle diameter is distributed as D10 ＜ 0.5 μm, D50 ＜ 1.5
μm, D90 ＜ 3 μm；The particle size distribution range of part flaking argentum powder is 2～5 μm, the radius-thickness ratio of main body argentum powder control be 1 1～
14, the size distribution profile of flake silver powder is 2～8 μm, and specific surface area is less than 4m2/g。
4) inorganic fillings is iron sesquioxide, nikel powder, nickel oxide powder, copper powder, the group of one or more in cupric oxide powder
Fit.
The particle size distribution range of inorganic fillings is 1～5 μm.
5) by step 1) quality that requires by a certain percentage with argentum powder, glass dust, inorganic fillings of the organic carrier of gained
Ratio mix homogeneously, re-uses three-roll grinder rolling and is referred to as finely dispersed end painting silver slurry；Use side described in the claims
Method is prepared the chip inductor end of the low-temperature sintering low silver content of gained and is coated with silver slurry, and after sintering, silver layer densification is full, and corner angle do not leak
Porcelain, end is coated with flat side down and does not stay extension, sheet resistance low (＜ 20M Ω/), inducer good electrical property after end painting, the performances such as adhesion is high
The advantage such as excellent.
Embodiment 1
A) by 8% ethyl cellulose, the polyvinyl butyral resin of 1%, the acrylic resin of 0.5%, 0.5% organic
The butyl carbitol acetate of bentonite, the terpineol of 25%, the butyl carbitol of 30% and/30%, the citric acid three of 5%
Butyl ester uses agitator fully to dissolve under conditions of 80 DEG C, prepares organic carrier.
B) use Muffle furnace 1200 DEG C of insulation half an hour by silicon dioxide 8%, zinc oxide 20%, antimony oxide 2%,
Bismuth oxide 60%, diboron trioxide 10% uses planetary ball mill 300rpm ball milling after being smelted into uniform glass phase shrend
5h, prepares glass powder.
C) by ball shape silver powder, part flaking argentum powder, flake silver powder is mixed by mass fraction 331, to argentum powder warp
Row premix.Take the 1st), 2) and 3) step gained organic carrier 30g, glass powder 5g, nickel oxide powder 5g and argentum powder 60g mixing, use
After blender is sufficiently stirred for, the end i.e. obtaining 55% silver content after re-using three-roll grinder grinding distribution is coated with silver slurry.
Embodiment 2
A. by 10% ethyl cellulose, the polyvinyl butyral resin of 1%, the acrylic resin of 0.5%, 0.5% have
The butyl carbitol acetate of machine bentonite, the terpineol of 25%, the butyl carbitol of 28% and/30%, the citric acid of 5%
Tributyl uses agitator fully to dissolve under conditions of 80 DEG C, prepares organic carrier；
B. step A gained organic carrier 42g, the glass powder 4g obtained in example 1, nickel oxide powder 4g and argentum powder 50g are taken
Mixing, after using blender to be sufficiently stirred for, the end i.e. obtaining 50% silver content after re-using three-roll grinder grinding distribution is coated with silver
Slurry.
Claims (8)
1. the inductor ends of a low-temperature sintering low silver content is coated with the formula of silver slurry, it is characterised in that: the component of silver paste is
Organic carrier, ball shape silver powder, part flaking argentum powder, flake silver powder, lead-free glass powder and inorganic filler, wherein, have airborne
Weight mark is 20%～30%, and ball shape silver powder mass fraction is 10%～40%, and part flaking quality of cathode silver mark is
10%～40%, flake silver powder mass fraction is 1%～20%, and lead-free glass powder mass fraction is 5%～15%, inorganic fill
Thing mass fraction is 5%～15%；
Described ball shape silver powder particle diameter is 0.1～3 μm, and part flaking argentum powder particle diameter is 2 μm～5 μm, and the particle diameter of flake silver powder is 2
μm～8 μm, the particle size distribution range of inorganic fillings is 1～5 μm.
The inductor ends of low-temperature sintering low silver content the most according to claim 1 is coated with the formula of silver slurry, it is characterised in that: institute
Component and the mass fraction of stating lead-free glass powder are silicon dioxide 8%～10%, zinc oxide 15%～25%, antimony oxide
1%～3%, bismuth oxide 40%～60% and diboron trioxide 5%～10%.
The inductor ends of low-temperature sintering low silver content the most according to claim 1 is coated with the formula of silver slurry, it is characterised in that: institute
Stating inorganic filler is the assembly of one or more in iron sesquioxide, nikel powder, nickel oxide powder, copper powder and cupric oxide powder.
The inductor ends of low-temperature sintering low silver content the most according to claim 1 is coated with the formula of silver slurry, it is characterised in that: institute
The organic carrier stated is made up of thixotropic agent, anti-sag agent and organic solvent；Wherein, thixotropic agent is for based on ethyl cellulose
Body, also includes polyethylene acetal butyral and acrylic resin；Organic solvent by butyl carbitol, butyl carbitol acetate,
Terpineol, tributyl citrate forms.
The inductor ends of low-temperature sintering low silver content the most according to claim 4 is coated with the formula of silver slurry, it is characterised in that: institute
State component and the mass fraction of organic carrier: the mass fraction of ethyl cellulose is 5%～10%, the matter of polyvinyl butyral resin
Amount mark be 1%～2%, the mass fraction of acrylic resin is 0.5%～2%, the mass fraction of terpineol be 20%～
40%, the mass fraction of butyl carbitol is 20%～40%, and the mass fraction of butyl carbitol acetate is 20%～40%,
The mass fraction of tributyl citrate is 5%～10%, and anti-sag agent mass fraction is 0.1%～0.5%.
The inductor ends of low-temperature sintering low silver content the most according to claim 4 is coated with the formula of silver slurry, it is characterised in that: institute
Stating anti-sag agent is the one in bentonite, organobentonite, nano-aluminium oxide, nano silicon, montmorillonite or several
Plant and combine.
7. the inductor ends of a low-temperature sintering low silver content is coated with the preparation method of silver slurry, it is characterised in that: described organic carrier
Preparation according to the component of above-mentioned organic carrier and mass fraction proportioning configuration raw material, heating always under the conditions of 60～90 DEG C
Stirring, becomes transparent molten silver until being completely dissolved；The preparation of described lead-free glass powder is according to each component of above-mentioned lead-free glass powder
Weigh and stir with powder beater, being contained in alumina crucible and be positioned over melting in Muffle furnace, smelting temperature be 1200 DEG C～
1300 DEG C, it is incubated 0.5～1h, uses shrend to be cooled down by high-temperature liquid state glass, after drying, use ethanol as medium, planetary ball mill
Machine 300rmp ball milling 4h～6h, i.e. can obtain meeting the glass powder of size distribution requirements；Finally, end be coated with silver slurry preparation be by
Described organic carrier, ball shape silver powder, the ball shape silver powder of part flaking, flake silver powder, glass powder, inorganic filler is by upper
The proportioning stated uses batch mixer mix homogeneously, carries and uses three-high mill grinding distribution 8 times, and by terrible fineness≤5 μm, viscosity is 25
～the finished product end of 40Pa.s is coated with slurry.
The inductor ends of low-temperature sintering low silver content the most according to claim 7 is coated with the preparation method of silver slurry, and its feature exists
In: described glass dust is a kind of crown glass powder body meeting 550 DEG C～650 DEG C sintering.
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| CN106847373A (en) * | 2017-03-30 | 2017-06-13 | 中国振华集团云科电子有限公司 | A kind of formula of chip resistor conductor silver paste |
| CN108788164A (en) * | 2017-04-28 | 2018-11-13 | 日亚化学工业株式会社 | The manufacturing method of metal sintered slurry and its manufacturing method and conductive material |
| CN109616242A (en) * | 2018-11-05 | 2019-04-12 | 肇庆市辰业电子有限公司 | A kind of inductance is with exempting to plate termination electrode silver paste |
| CN109841405A (en) * | 2019-04-18 | 2019-06-04 | 北京元六鸿远电子科技股份有限公司 | A kind of silver-colored terminal electrode paste of low-temperature sintering MLCC |
| CN114615798A (en) * | 2022-04-01 | 2022-06-10 | 广州三则电子材料有限公司 | Zero-shrinkage hole-filling conductive slurry and preparation method thereof |
| CN115602437A (en) * | 2022-10-24 | 2023-01-13 | 清远市海之澜电子科技有限公司（Cn） | Preparation method of inductance magnetic core |
| CN116543949A (en) * | 2023-07-04 | 2023-08-04 | 乾宇微纳技术(深圳)有限公司 | Hole filling slurry and preparation method thereof |
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| CN115602437A (en) * | 2022-10-24 | 2023-01-13 | 清远市海之澜电子科技有限公司（Cn） | Preparation method of inductance magnetic core |
| CN116543949A (en) * | 2023-07-04 | 2023-08-04 | 乾宇微纳技术(深圳)有限公司 | Hole filling slurry and preparation method thereof |
| CN116543949B (en) * | 2023-07-04 | 2023-12-22 | 乾宇微纳技术(深圳)有限公司 | Hole filling slurry and preparation method thereof |
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