CN105880628B - A kind of preparation method of Bright Silver Powder for jewellery industry - Google Patents

A kind of preparation method of Bright Silver Powder for jewellery industry Download PDF

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Publication number
CN105880628B
CN105880628B CN201610320064.9A CN201610320064A CN105880628B CN 105880628 B CN105880628 B CN 105880628B CN 201610320064 A CN201610320064 A CN 201610320064A CN 105880628 B CN105880628 B CN 105880628B
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China
Prior art keywords
silver powder
preparation
bright
silver
solution
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Expired - Fee Related
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CN201610320064.9A
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Chinese (zh)
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CN105880628A (en
Inventor
周全法
黄继忠
王自伟
孙洪波
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Jiangsu University of Technology
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Jiangsu University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cosmetics (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention relates to a kind of preparation method of the Bright Silver Powder for jewellery industry, comprise the following steps:(1) compound concentration is 1 1.5mol/L silver nitrate solution;(2) sodium hydroxide solution that mass fraction is 5 10% is added into silver nitrate solution, adjusts pH to 8 12;(3) triethanolamine solution is instilled in step silver nitrate solution, silver powder slurries is made;(4) the stearic acid ethanol solution that mass fraction is 5 10% is added to silver powder slurries, drying the dried silver powder of (5) ball milling after ultrasonic disperse produces Bright Silver Powder.The present invention is the ball milling after silver powder drying, ensure that big the Bright Silver Powder bright in color of preparation, density, good mechanical property, specific surface area are big, available for jewellery industry, can be used for the fields such as other silver coatings, conducting resinl.Preparation method of the present invention is simple, and production cost is low, is easy to volume production, is suitable for industrially mass producing.

Description

A kind of preparation method of Bright Silver Powder for jewellery industry
Technical field
The present invention relates to the preparation side of a kind of preparation method of silver powder, particularly a kind of Bright Silver Powder for jewellery industry Method.
Background technology
With the progress in epoch and the development of technology, new technology has an immense impact on to metal surface technique, in the past can not Nowadays the technological effect of realization can put into effect.New technology has driven the change of traditional metal surface technique, many occurs New works, original time consuming artisan craftsmanship is set to become quickly easily.New decorative pattern, mass production, more multicolour, More moulding, metal surface technique is set there are more business opportunities, business opportunity has driven the progress of technological level in itself, adds technique sheet The change of body.Powdery paints has the characteristic such as energy-conservation, the performance of VOC free discharge, good decorative property, safe to use, domestic in recent years Powder coating technology is quickly grown.Powdery paints is as decorative material, as the continuous improvement of living standard, people are no longer full Decoration, the protection of powdery paints single color are enough to, and proposes higher requirement, the Nano Silver with bright metal outward appearance Powder, it is the expensive goods in art of powder coatings to be known as by people, by application fields such as jewellery, household electrical appliances, furniture and automobiles Favorable comment, and slowly promote come.
Silver powder can be divided into flake silver powder and ball shape silver powder.Flake silver powder refers to one-dimensional thickness < 100nm flakelike powder, its Preparation method is different, can be divided into reduction ball-milling method, light inducible and chemical reduction method.Wherein reduce ball-milling method:It is to be gone back with chemistry Nano-scale particle shape silver powder prepared by former method is raw material, sheet is pressed into through ball milling, so as to obtain the method for flake silver powder.Ball Bright Silver Powder bright in color prepared by mill method, density are big, good mechanical property, specific surface area are big.It is prepared by relevant reduction ball-milling method The report of flake silver powder is a lot, the difference is that changing the species of reducing agent, reducing condition, ball milling condition etc. to prepare different requirements Flake silver powder.Sheet is made with obtained dendroid or spherical silver powder, then the ball milling by certain time is first reduced in the present invention Bright Silver Powder, it can be widely used for jewellery industry, can be used for the fields such as other silver coatings, conducting resinl.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the Bright Silver Powder for jewellery industry, obtained bright sheet The average grain diameter of silver powder is 2-12 μm, can be used for the fields such as other silver coatings, conducting resinl.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of preparation method of Bright Silver Powder for jewellery industry, comprises the following steps:
(1) silver nitrate solution is prepared, the concentration of silver nitrate is 1-1.5mol/L in solution;
(2) sodium hydroxide solution that mass fraction is 5-10%, regulation are added in the silver nitrate solution that step (1) is prepared PH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with 0.5-1mL/min speed, silver is made Slurry liquid;
(4) the silver powder slurries that step (3) obtains first are filtered, the stearic acid second that mass fraction is 5-10% is added after washing Alcoholic solution, ultrasonic disperse 1-2h, dry and remove etoh solvent;
(5) it is 1 by step (4) dried silver powder and mass ratio:3-5 a diameter of 1mm and 3mm mixed oxidizations zirconium ball, By 1:It is put into after 4-6 ratio of grinding media to material mixing in hexagon ball grinder, rotational speed of ball-mill is 80~100r/min, ball milling 20h, produces light Silver lustre powder.
Specifically, the step (2), the constant temperature of (3) system are 25-40 DEG C.
Specifically, the ratio between amount of material of triethanolamine and silver nitrate is (1.5-5) in the step (3):1.
Specifically, concentration of the stearic acid in silver powder slurries is 0.5-1.5% in the step (4).
Specifically, the average grain diameter for the flake silver powder that the step (5) obtains is 2-12 μm.
Beneficial effects of the present invention:
(1) when preparing ultrapure silver powder, centre does not have to add any protective agent and dispersant the present invention, without any organic The residual of thing, meet the use demand of jewellery product.
(2) present invention is to add ball-milling additive before silver powder is dried, and ball milling is carried out after drying, and ensure that the light silver of preparation Powder bright in color.
(3) preparation method of the present invention is simple, and production cost is low, is easy to volume production, is suitable for industrially mass producing.
(4) preparation method of the present invention controls ratio of grinding media to material 1:4-6, ball milling effect is ensure that, and make silver powder particle diameter point Cloth is in narrower scope.
Embodiment
Presently in connection with embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of preparation method of Bright Silver Powder for jewellery industry, comprises the following steps:
(1) silver nitrate solution is prepared, the concentration of silver nitrate is 1-1.5mol/L in solution;
(2) sodium hydroxide solution that mass fraction is 5-10%, regulation are added in the silver nitrate solution that step (1) is prepared PH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with 0.5-1mL/min speed, silver is made The ratio between amount of material of slurry liquid, wherein triethanolamine and silver nitrate is 1.5-5:1
(4) the silver powder slurries that step (3) obtains first are filtered, the stearic acid second that mass fraction is 5-10% is added after washing Alcoholic solution, ultrasonic disperse 1-2h, dry and remove etoh solvent;Concentration of the stearic acid in silver powder slurries is 0.5-1.5%,
(5) it is 1 by step (4) dried silver powder and mass ratio:3-5 a diameter of 1mm and 3mm mixed oxidizations zirconium ball, By 1:It is put into after 4-6 ratio of grinding media to material mixing in hexagon ball grinder, rotational speed of ball-mill is 80~100r/min, ball milling 20h, produces light Silver lustre powder, average grain diameter are 2-12 μm;
Wherein, it is 25-40 DEG C that step (2), the temperature of (3) system are constant.
Embodiment 2-6 and scheme other conditions with embodiment 1, difference such as following table:
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.

Claims (5)

1. a kind of preparation method of Bright Silver Powder for jewellery industry, comprises the following steps:
(1) silver nitrate solution is prepared, the concentration of silver nitrate is 1-1.5mol/L in solution;
(2) step (1) prepare silver nitrate solution in add mass fraction be 5-10% sodium hydroxide solution, regulation pH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with 0.5-1mL/min speed, aluminium paste is made Liquid;
(4) the silver powder slurries that step (3) obtains first are filtered, it is molten that the stearic acid ethanol that mass fraction is 5-10% is added after washing Liquid, ultrasonic disperse 1-2h, dry and remove etoh solvent;
(5) it is 1 by step (4) dried silver powder and mass ratio:3-5 a diameter of 1mm and 3mm mixed oxidizations zirconium ball, by 1: It is put into after 4-6 ratio of grinding media to material mixing in hexagon ball grinder, rotational speed of ball-mill is 80~100r/min, ball milling 20h, produces bright silver Powder.
A kind of 2. preparation method of Bright Silver Powder for jewellery industry as claimed in claim 1, it is characterised in that:The step Suddenly (2), the constant temperature of (3) system are 25-40 DEG C.
A kind of 3. preparation method of Bright Silver Powder for jewellery industry as claimed in claim 1, it is characterised in that:The step Suddenly the ratio between amount of material of triethanolamine and silver nitrate is 1.5-5 in (3):1.
A kind of 4. preparation method of Bright Silver Powder for jewellery industry as claimed in claim 1, it is characterised in that:The step Suddenly concentration of the stearic acid in silver powder slurries is 0.5-1.5% in (4).
A kind of 5. preparation method of Bright Silver Powder for jewellery industry as claimed in claim 1, it is characterised in that:The step Suddenly the average grain diameter for the flake silver powder that (5) obtain is 2-12 μm.
CN201610320064.9A 2016-05-13 2016-05-13 A kind of preparation method of Bright Silver Powder for jewellery industry Expired - Fee Related CN105880628B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102784927A (en) * 2012-08-28 2012-11-21 苏州东旭弘业新材料科技有限公司 Method for preparing high-performance sheet silver powder
CN103143723A (en) * 2013-03-27 2013-06-12 深圳市中金岭南科技有限公司 Method for preparing flake silver powder with low bulk density
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4862180B2 (en) * 1999-08-13 2012-01-25 Dowaエレクトロニクス株式会社 Method for producing silver powder and method for producing flaky silver powder
JP3874634B2 (en) * 2001-08-10 2007-01-31 福田金属箔粉工業株式会社 Flake-like silver powder for conductor paste and conductor paste using the same
JP5330724B2 (en) * 2008-03-31 2013-10-30 三井金属鉱業株式会社 Method for producing flake silver powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102784927A (en) * 2012-08-28 2012-11-21 苏州东旭弘业新材料科技有限公司 Method for preparing high-performance sheet silver powder
CN103143723A (en) * 2013-03-27 2013-06-12 深圳市中金岭南科技有限公司 Method for preparing flake silver powder with low bulk density
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste

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