CN101088676A - Prepn process of flaky silver powder - Google Patents

Prepn process of flaky silver powder Download PDF

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Publication number
CN101088676A
CN101088676A CN200710049489.1A CN200710049489A CN101088676A CN 101088676 A CN101088676 A CN 101088676A CN 200710049489 A CN200710049489 A CN 200710049489A CN 101088676 A CN101088676 A CN 101088676A
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China
Prior art keywords
silver powder
ball milling
flake silver
hours
microns
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CN200710049489.1A
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Chinese (zh)
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CN100506437C (en
Inventor
王自森
杨玉祥
汪云林
詹刚
王刚
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China Banknote Printing and Minting Group Co Ltd
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China Banknote Printing and Minting Corp
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Priority to CNB2007100494891A priority Critical patent/CN100506437C/en
Publication of CN101088676A publication Critical patent/CN101088676A/en
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Publication of CN100506437C publication Critical patent/CN100506437C/en
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The preparation process of flaky silver powder belongs to the field of conducting material preparing technology. The preparation process includes ball milling silver powder material with silver content over 99.95 %, ball milling medium of 3 mm diameter stainless steel balls and ball milling stuffing of hexadecanol in 1 % in a ball mill in the frequency of 50Hz for 10-30 hr, detecting during ball milling, and hot state sieving in 40 mesh to obtain flaky silver powder of average powder size of 5-40 microns. The process can produce flaky silver powder of different average powder sizes.

Description

The preparation method of flake silver powder
Technical field
The invention belongs to a kind of preparation method of conductive material, particularly a kind of preparation method of flake silver powder.
Background technology
Flake silver powder is mainly used in the conductive filler of electrically-conducting paint, electrically conductive ink, conducting polymer silver slurry, such as being used to make electronic devices and components such as flexible PCB, soft-touch control; It is the major function material of electronic devices and components such as monolithic capacitor, wave filter, carbon-film potentiometer, tantalum capacitor, thin film switch, semiconductor chip.
Known more about the flake silver powder preparation method, be divided into Mechanical Method and chemical method.Mechanical ball milling is divided into dry method, wet ball grinding.As adopt planetary ball mill wet production flake silver powder, and the electrical property that the auxiliary agent of employing is many, influence silver powder, under the identical conditions, it is single to produce the flake silver powder kind; Other has the planetary ball mill of employing to produce the low bulk flake silver powder, complex procedures, because the method production flake silver powder apparent density is low, it is big to be used for the thin film switch medium viscosity, constructional difficulties.Chemical method is produced flake silver powder three kinds of ammonium formate reducing process, ethylene glycol chemical reduction method and photo-induction inducing defecation by enema and suppository.Chemical method can directly prepare flake silver powder, because it is too thin to obtain powder, thickness only is that several nanometers are to tens nanometers.When silver powder and resin coupling, be rolled into slurry, be heating and curing, along with solidification temperature raises, silver strip shrinks, and forms particle and chap, loses metallic luster and is silver gray, causes zeropoint resistance to increase, and influences its practical value.
Summary of the invention
The objective of the invention is: solve the problem that the silver powder quality of the complex procedures that exists in the existing preparation flake silver powder process, production is not enough and be difficult to produce the serial flake silver powder of multiple average grain diameter, provide a kind of employing to have ball mill now, under different ball milling time conditions, obtain the flake silver powder of a series of kinds, this flake silver powder can be thin film switch, flexible circuitry slurry needed raw material, and its every index can both satisfy thin film switch, the requirement of flexible circuitry slurry.
Purpose of the present invention realizes by following technical proposals:
The preparation method of flake silver powder, silver powder raw material, ball-milling medium, ball milling filler are put into ball mill carry out ball milling, described silver powder raw material is a silver content greater than 99.95% silver powder, ball-milling medium is the stainless steel ball of 3 millimeters of diameters, the ball milling filler is the hexadecanol that quality accounts for silver powder raw material 1%, the control ball milling time obtained average grain diameter and is 5~40 microns flake silver powder between 10 hours~30 hours.
As one of optimal way of the present invention, the granularity of described silver powder raw material is 5~7 microns, and quality is 10kg, is 60kg as the quality of the stainless steel ball of ball-milling medium.
Furthermore, described ball milling also comprised the steps: in the time
Dry grinding frequency 50Hz;
Ball milling was observed after 2 hours, guaranteed not have the sticking wall of powder, did not lump;
Detect in the mechanical milling process, hot 40 orders sieve.
As one of embodiments of the present invention, the described ball milling time is 12 hours, obtains average grain diameter and be 5.21 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 15 hours, obtains average grain diameter and be 6.32 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 17 hours, obtains average grain diameter and be 7.32 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 19 hours, obtains average grain diameter and be 9.91 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 20 hours, obtains average grain diameter and be 13.28 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 21 hours, obtains average grain diameter and be 20.50 microns flake silver powder.
As one of embodiments of the present invention, the described ball milling time is 23 hours, obtains average grain diameter and be 26.80 microns flake silver powder;
As one of embodiments of the present invention, the described ball milling time is 25 hours, obtains average grain diameter and be 33.36 microns flake silver powder;
As one of embodiments of the present invention, the described ball milling time is 27 hours, obtains average grain diameter and be 39.20 microns flake silver powder.
The present invention selects silver powder raw material, ball-milling medium, ball milling filler, silver powder, the diameter of having chosen 5~7 microns is 3 millimeters stainless steel ball and 1% hexadecanol, ball milling frequency in conjunction with 50Hz, realization is 5~40 microns a flake silver powder by control ball milling time production average grain diameter, and the every index of flake silver powder of producing can both satisfy thin film switch, the requirement of flexible circuitry slurry.
As seen, adopt the method for preparing flake silver powder, compared with prior art, have under different ball milling time conditions, can obtain the advantage of a series of many kinds flake silver powders, applicable to in the middle of the production of flake silver powder as conductive material.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1: choose granularity and be 5~7 microns, silver content greater than 99.95% silver powder raw material 10kg, hexadecanol 100g, also having diameter is 3 millimeters stainless steel ball 60kg, puts into ball mill, dry grinding frequency 50Hz; Ball milling was observed after 2 hours, guaranteed not have the sticking wall of powder, did not lump; Detect in the mechanical milling process, hot 40 orders sieve.The ball milling time is 12 hours, obtains average grain diameter and be 5.21 microns flake silver powder.
Embodiment 2: basic skills such as embodiment 1, the ball milling time is 15 hours, obtains average grain diameter and be 6.32 microns flake silver powder.
Embodiment 3: basic skills such as embodiment 1, the ball milling time is 17 hours, obtains average grain diameter and be 7.32 microns flake silver powder.
Embodiment 4: basic skills such as embodiment 1, the described ball milling time is 19 hours, obtains average grain diameter and be 9.91 microns flake silver powder.
Embodiment 5: basic skills such as embodiment 1, the ball milling time is 20 hours, obtains average grain diameter and be 13.28 microns flake silver powder.
Embodiment 6: basic skills such as embodiment 1, the ball milling time is 21 hours, obtains average grain diameter and be 20.50 microns flake silver powder.
Embodiment 7: basic skills such as embodiment 1, and the ball milling time is 23 hours, obtains average grain diameter and be 26.80 microns flake silver powder;
Embodiment 8: basic skills such as embodiment 1, and the ball milling time is 25 hours, obtains average grain diameter and be 33.36 microns flake silver powder;
Embodiment 9: basic skills such as embodiment 1, the ball milling time is 27 hours, obtains average grain diameter and be 39.20 microns flake silver powder.

Claims (10)

1, the preparation method of flake silver powder, silver powder raw material, ball-milling medium, ball milling filler are put into ball mill carry out ball milling, it is characterized in that: described silver powder raw material is a silver content greater than 99.95% silver powder, ball-milling medium is the stainless steel ball of 3 millimeters of diameters, the ball milling filler is the hexadecanol that quality accounts for silver powder raw material 1%, the control ball milling time obtained average grain diameter and is 5~40 microns flake silver powder between 10 hours~30 hours.
2, the preparation method of flake silver powder according to claim 1, it is characterized in that: the granularity of described silver powder raw material is 5~7 microns, quality is 10kg, is 60kg as the quality of the stainless steel ball of ball-milling medium.
3, the preparation method of flake silver powder as claimed in claim 1 or 2 is characterized in that: described ball milling comprises the steps in the time,
A. the frequency of dry grinding 50Hz;
B. ball milling was observed after 2 hours, guaranteed not have the sticking wall of powder, did not lump;
C. detect in the mechanical milling process, hot 40 orders sieve.
4, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 12 hours, obtains average grain diameter and be 5.21 microns flake silver powder.
5, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 15 hours, obtains average grain diameter and be 6.32 microns flake silver powder.
6, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 17 hours, obtains average grain diameter and be 7.32 microns flake silver powder.
7, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 19 hours, obtains average grain diameter and be 9.91 microns flake silver powder.
8, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 20 hours, obtains average grain diameter and be 13.28 microns flake silver powder.
9, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that: the described ball milling time is 21 hours, obtains average grain diameter and be 20.50 microns flake silver powder.
10, as the preparation method of flake silver powder as described in the claim 3, it is characterized in that:
The described ball milling time is 23 hours, obtains average grain diameter and be 26.80 microns flake silver powder;
The described ball milling time is 25 hours, obtains average grain diameter and be 33.36 microns flake silver powder;
The described ball milling time is 27 hours, obtains average grain diameter and be 39.20 microns flake silver powder.
CNB2007100494891A 2007-07-11 2007-07-11 Preparation process of flaky silver powder Active CN100506437C (en)

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Application Number Priority Date Filing Date Title
CNB2007100494891A CN100506437C (en) 2007-07-11 2007-07-11 Preparation process of flaky silver powder

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CN100506437C CN100506437C (en) 2009-07-01

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104722751A (en) * 2013-12-20 2015-06-24 有研亿金新材料股份有限公司 Flaky platinum powder, and preparation method and application thereof
CN105478788A (en) * 2015-12-25 2016-04-13 广东羚光新材料股份有限公司 Method of producing flake silver powder
CN108405869A (en) * 2018-04-03 2018-08-17 金川集团股份有限公司 A kind of preparation method of small particle flake silver powder
CN111774575A (en) * 2020-07-30 2020-10-16 金川集团股份有限公司 Preparation method of high-tap-density large-sheet-diameter flaky silver powder

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104722751A (en) * 2013-12-20 2015-06-24 有研亿金新材料股份有限公司 Flaky platinum powder, and preparation method and application thereof
CN105478788A (en) * 2015-12-25 2016-04-13 广东羚光新材料股份有限公司 Method of producing flake silver powder
CN108405869A (en) * 2018-04-03 2018-08-17 金川集团股份有限公司 A kind of preparation method of small particle flake silver powder
CN111774575A (en) * 2020-07-30 2020-10-16 金川集团股份有限公司 Preparation method of high-tap-density large-sheet-diameter flaky silver powder

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Assignee: The Great Wall Gold & Silver Refinery

Assignor: CHINA BANKNOTE PRINTING AND MINTING Corp.

Contract record no.: 2011510000337

Denomination of invention: Prepn process of flaky silver powder

Granted publication date: 20090701

License type: Exclusive License

Open date: 20071219

Record date: 20111229

CP01 Change in the name or title of a patent holder
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Address after: 610000 No. 189, Golden Road, Wenjiang District, Sichuan, Chengdu

Patentee after: China Banknote Printing and Minting Group Co.,Ltd.

Address before: 610000 No. 189, Golden Road, Wenjiang District, Sichuan, Chengdu

Patentee before: CHINA BANKNOTE PRINTING AND MINTING Corp.