CN108296478A - Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder - Google Patents
Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder Download PDFInfo
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- CN108296478A CN108296478A CN201810026562.1A CN201810026562A CN108296478A CN 108296478 A CN108296478 A CN 108296478A CN 201810026562 A CN201810026562 A CN 201810026562A CN 108296478 A CN108296478 A CN 108296478A
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- silver
- nickel
- particles
- nickel powder
- reducing agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic 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
- 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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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of silver-nickel powder, and wherein for nickel particles particle size at 0.1 μm 5.0 μm, silver-colored weight accounts for the 0 60% of silver-colored nickel particles total weight；The method for preparing the silver-nickel powder is so that silver particles is tentatively precipitated to which presoma be prepared on nickel particles surface using reducing agent I first, again by presoma and dispersant, complexing agent, the reducing agent II of silver particles and silver particles comes into full contact in deionized water, to make silver further replace precipitation on the surface of the presoma, using the silver coating compactness extent height on silver-colored its surface of nickel particles that the above method is prepared, hole is few, therefore the resistance that can well control nickel particles surface oxidation and silver-nickel powder declines, ensure that silver-nickel powder electric conductivity after long-time preserves storage is still good, it can be applied in electrocondution slurry.
Description
Technical field
The present invention relates to electronic functional material, metal powder material fields, more particularly, to the alloy powder of silver cladding nickel
And its manufacturing method.
Background technology
Conductive filler as conductive coating and electrocondution slurry has the noble metals such as silver, palladium, gold, wherein electric conductivity most excellent
Surely belong to silver powder, and the price of silver powder is compared with bronze with palladium powder and wants much lower, therefore it uses model in electronics industry at present
It encloses than wide.Although silver powder is a kind of important raw and processed materials being widely used in the electronics industry, fly with the price of silver
Rise, the cost of many electronic components is caused also to rise rapidly, so we need how to subtract from the point of view of production cost
The usage amount of few noble metal, thus find it is a kind of can replace silver powder and price cheaper powder just seems reasonably necessary again
.Metal nickel powder just have good electric conductivity and electromagnetic wave shielding, and price be compared to silver it is also less expensive；But pure metallic nickel
Powder is unstable at high temperature to be easier to aoxidize, and the oxidation film of one layer of insulating properties is formed in powder surface, to make its electric conductivity
It is unstable to substantially reduce it using possible.So by coating the noble metal of nanometer layer in cheap lowpriced metal surface, to right
Its surface be modified improve inoxidizability be improve nickel powder conductive stability with expand its application feasible method.Than if any
Document it is proposed that the electroconductive powder in nickel powder coated with silver on surface layer preparation method, specially make the complex solution of silver ion
It is mixed and made into suspended emulsion with the slurry containing nickel powder, complexing agent and dispersant, makes silver ion equal on the surface of nickel powder by stirring
Even precipitation, this method make the precipitation of silver ion to be coated on nickel powder surface, but the powder prepared by the reaction using displacement reaction
Body overlay coating porosity is high, and cladding is not fine and close.
Invention content
In order to solve the above technical problems, a kind of electroless plating method of present invention offer, which prepares silver, is coated on silver made of nickel powder surface
Nickel alloy powder.
The technical solution of the present invention is to provide a kind of silver-nickel powder, wherein nickel particles particle size at 0.1 μm -5.0 μm,
Silver-colored weight accounts for the 0-60% of silver-colored nickel particles total weight.
It is a further object to provide the preparation methods of silver-nickel powder, (may be used using reducing agent I first
Organic reducing agent) make silver particles tentatively be precipitated to be prepared presoma on nickel particles surface, then by presoma and dispersant,
The reducing agent II (acid organic reducing agent is shown when using dissolving in deionized water) of complexing agent, silver particles and silver particles exists
It is come into full contact in deionized water, to make silver further replace precipitation on the surface of the presoma.The silver-nickel powder of the present invention
It can be used in a variety of electrocondution slurries, using conventional electrocondution slurry preparation process, the electrocondution slurry of gained can be applied to too
Positive energy battery, lithium battery, electrically conductive ink etc..
The advantages of the present invention：It is 0.1 μm -5.0 μm of nickel particles in its coated with silver on surface layer to use grain size,
And the 0-60% that silver layer weight is silver-colored nickel particles total weight is controlled, the compactness extent of clad can be preferably controlled, silver is promoted
Nickel particles performance；Nickel particles are handled using dual reducting agents (reducing agent I and reducing agent II), the cladding of silver particles is made to give birth to
Growth process copies silver particles Growing Process of Crystal Particles, i.e., part silver is made to be coated on nickel particles surface first, when subsequent deposition of silver with
These silver first coated are condensation nucleus, and nickel particles surface, different directions growth are gradually filled up according to certain grain growth direction
Silver particles mutually blend formation one, the final hole that obtains is few, the good silver-colored nickel particles of compactness.
Description of the drawings
Fig. 1 is the amplification high power scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 2.
Fig. 2 is the scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 1.
Fig. 3 is the scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 2.
Fig. 4 is the scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 3.
Fig. 5 is the scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 4.
Fig. 6 is the scanning electron microscope image of the silver-colored nickel particles obtained in embodiment 5.
Specific implementation mode
Present invention will be further explained below with reference to the attached drawings and specific embodiments.
The present invention provides a kind of silver-nickel powder, is configured to nickel particles surface continuous uniform and is densely coated with silver-colored cladding
Layer, nickel particles are completely capped, and the whole surface of the core particle by being coated on nickel composition with silver coating can control nickel as possible
The oxidation on surface can make silver-colored nickel particles preserve storage for a long time, so the silver-nickel powder of the present invention can control its resistance as possible
Decline.
The shape of nickel particles is not particularly limited, such as the nickel powder as core particle can be orbicule, sheet, no
The particle of the shapes such as rule body；In addition covering core particle surface is silver-colored since its overburden cover is smaller, thus silver-colored nickel particles
Shape and the shape of core particle are substantially consistent.
Silver-nickel powder of the present invention is with the surface of the very thin core particle for being coated on nickel composition of silver coating, therefore core particles
There is no big difference, the grain size laser diffraction formula particle size distribution of core particle between the grain size of son and the grain size of silver-colored nickel particles
Volume-cumulative grain size D50 under the 50 capacity % of cumulative volume that method measures indicates that this method is equally applicable to measure silver-colored Nickel particle
Seed diameter D50.
The present invention limits ratio silver-colored in silver-colored nickel particles as 0-60%, in the densification for being conducive to preferably control silver coating
Degree, the use for the noble silver that practices every conceivable frugality under the premise of promoting silver-colored nickel particles performance.The assay method of ratio shared by silver can
To be：So that silver-colored nickel particles is all dissolved using nitric acid, ICP emission spectrographic analyses then are carried out to solution to be measured.
Embodiment 1
300nm globular powdered nickels (production of Ningbo extensive nanometer new material company) raw material 15.8g is weighed, is added in reactor,
Then the dilute sulfuric acid 500ml that mass concentration is 5% is added, 30min is to remove the oxide on nickel powder core particle surface for ultrasonic agitation,
Then filtering cleans 3 times and obtains for use nickel powder after pickling；Weigh the poly- second of 38g glucose, triethylene tetramine 38g and 11.3g two
Alcohol 400 is added in 2000ml deionized waters and forms complex liquid, and then for use nickel powder is added in enveloping agent solution and is stirred evenly
Referred to as solution A；
It weighs silver nitrate 23.5g and is added in the deionization of 100ml and fully dissolve, concentrated ammonia liquor is added and is adjusted to clear silver-colored ammonium
It is B solution after solution, then after being added drop-wise in nickel powder complex solution with the rate of addition of 5ml/min；
Weigh 9.5g ascorbic acids be added 1900ml deionized water stir after be C solution；
In the case where power is the stirring of 300W ultrasonic dispersers, C solution is added to B solution with the rate of addition of 10ml/min
In so that it is reacted, reaction temperature control is at 70 DEG C, reaction time 30min；It waits carrying out reaction solution after the completion of reacting
Filtering cleaning 3 times, absolute ethyl alcohol washes twice, then 80 DEG C of forced air dryings, obtains silver-nickel powder.
Embodiment 2
So that the grain size of nickel particles is become 600nm, in addition to this, technique identical with case study on implementation 1 is carried out, to obtain silver
Nickel alloy powder.
Embodiment 3
So that the grain size of nickel particles is become 1000nm, in addition to this, technique identical with case study on implementation 1 is carried out, to obtain
Silver-nickel powder.
Embodiment 4
Make the shape of nickel particles by spherical change slabbing, in addition to this, carries out technique identical with case study on implementation 1, to
Obtain silver-nickel powder.
Embodiment 5
So that the shape of nickel particles is become irregular by spherical, in addition to this, carry out technique identical with case study on implementation 1,
To obtain silver-nickel powder.
Fig. 2~6 are the scanning electron microscope image of Examples 1 to 5, and Fig. 1 is putting for the silver-colored nickel particles that embodiment 2 obtains
Big high power scanning electron microscope image.From Fig. 1~6 it can be seen that no matter using the nickel core particle of which kind of shape in embodiment,
Using the method for the present invention, as obtained by the preparation of the proportioning of controlling reaction temperature, time and nickel particles, silver particles, reducing agent
Silver-nickel powder, surface is continuously coated with silver layer, and is evenly coated densification, and no tiny Argent grain generates, and especially prepares step
Ultrasonic wave dispersion means are taken in rapid so that nickel core particle is fully dispersed to be opened, so that silver particles are more equal in its surface deposition
It is even, promote cladding compactness extent to improve electric conductivity.
The present embodiments relate to material, reagent and experimental facilities, unless otherwise instructed, be meet it is electric
The commercial product of Material Field.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to the scope of patent protection of the present invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (9)
1. a kind of silver-nickel powder, which is characterized in that be coated with silver layer using nickel particles as core particle and nickel particles surface and constituted silver
Nickel particles, the nickel particles grain size are 0.1 μm -5.0 μm, and silver-colored weight accounts for the 0-60% of silver-colored nickel particles total weight.
2. the method for preparing silver-nickel powder described in claim 1, which is characterized in that include the following steps：Use reducing agent I
So that silver particles is tentatively precipitated on nickel particles surface and obtain presoma, then by presoma and dispersant, complexing agent, silver particles and silver granuel
The reducing agent II of son comes into full contact in deionized water, to make silver further replace precipitation on the surface of the presoma.
3. the method as claimed in claim 2 for preparing silver-nickel powder, which is characterized in that the reducing agent I is glucose, second
It is one or more in aldehyde, tyrosine.
4. the method as claimed in claim 2 for preparing silver-nickel powder, which is characterized in that the reducing agent II is acid organic
Reducing agent, the acidity organic reducing agent is one or more in ascorbic acid, formaldehyde, oxalic acid.
5. the method as claimed in claim 2 for preparing silver-nickel powder, which is characterized in that the presoma is contacted with silver particles
Process be presoma be scattered in containing dispersant, complexing agent solution in, silver particles are configured to the shape of silver ammino solution with silver nitrate
Formula is added dropwise in forerunner's dispersion liquid, and drop rate is controlled in 3-6ml/min.
6. the method as claimed in claim 5 for preparing silver-nickel powder, which is characterized in that the reducing agent II forms solution
Afterwards, it is added dropwise in presoma and the mixed solution of silver particles, drop rate 8-12ml/min, mixed solution is adopted during dropwise addition
Disperse to stir with ultrasonic wave.
7. the method as claimed in claim 6 for preparing silver-nickel powder, which is characterized in that reaction temperature is 65~80 DEG C, instead
It is 20~35min between seasonable.
8. the method as claimed in claim 5 for preparing silver-nickel powder, which is characterized in that the mass ratio of each raw material is as follows：Nickel
Particle:Silver nitrate=1:1.45-1.6；And when reducing agent I use glucose, reducing agent II use ascorbic acid when, silver nitrate with
The mass ratio of glucose is 1:The mass ratio of 1.60-1.70, silver nitrate and ascorbic acid is 0.40-0.45:1.
9. a kind of conductive silver paste, which is characterized in that contain silver-nickel powder described in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810026562.1A CN108296478A (en) | 2018-01-11 | 2018-01-11 | Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810026562.1A CN108296478A (en) | 2018-01-11 | 2018-01-11 | Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder |
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| Publication Number | Publication Date |
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| CN108296478A true CN108296478A (en) | 2018-07-20 |
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| CN201810026562.1A Pending CN108296478A (en) | 2018-01-11 | 2018-01-11 | Silver-nickel powder and preparation method thereof and electrocondution slurry containing the silver-nickel powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
| CN115533096A (en) * | 2022-10-18 | 2022-12-30 | 温州伟达贵金属粉体材料有限公司 | Silver-nickel mixed powder and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1416986A (en) * | 2002-12-13 | 2003-05-14 | 西安理工大学 | High temperature antioxidant base metal composition and its production process |
| JP2011144441A (en) * | 2010-01-18 | 2011-07-28 | Namics Corp | Silver-coated nickel powder and method for producing the same |
| CN102407329A (en) * | 2011-11-18 | 2012-04-11 | 江苏大学 | Method for preparing nickel-silver coreshell structure nanoparticles |
| CN102672168A (en) * | 2012-01-06 | 2012-09-19 | 河南科技大学 | Preparation method for core-shell structural nickel-silver bimetallic powder |
| CN102723142A (en) * | 2012-04-24 | 2012-10-10 | 江苏大学 | Preparation method of nickel-based silver conductive slurry |
| CN104328295A (en) * | 2014-10-29 | 2015-02-04 | 东莞市中一合金科技有限公司 | Preparation method of silver-nickel alloy material |
| CN104837582A (en) * | 2013-05-08 | 2015-08-12 | 三井金属矿业株式会社 | Silver-coated nickel particles and method for producing same |
-
2018
- 2018-01-11 CN CN201810026562.1A patent/CN108296478A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1416986A (en) * | 2002-12-13 | 2003-05-14 | 西安理工大学 | High temperature antioxidant base metal composition and its production process |
| JP2011144441A (en) * | 2010-01-18 | 2011-07-28 | Namics Corp | Silver-coated nickel powder and method for producing the same |
| CN102407329A (en) * | 2011-11-18 | 2012-04-11 | 江苏大学 | Method for preparing nickel-silver coreshell structure nanoparticles |
| CN102672168A (en) * | 2012-01-06 | 2012-09-19 | 河南科技大学 | Preparation method for core-shell structural nickel-silver bimetallic powder |
| CN102723142A (en) * | 2012-04-24 | 2012-10-10 | 江苏大学 | Preparation method of nickel-based silver conductive slurry |
| CN104837582A (en) * | 2013-05-08 | 2015-08-12 | 三井金属矿业株式会社 | Silver-coated nickel particles and method for producing same |
| CN104328295A (en) * | 2014-10-29 | 2015-02-04 | 东莞市中一合金科技有限公司 | Preparation method of silver-nickel alloy material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
| CN115533096A (en) * | 2022-10-18 | 2022-12-30 | 温州伟达贵金属粉体材料有限公司 | Silver-nickel mixed powder and preparation method thereof |
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Application publication date: 20180720 |