CN107790739A - A kind of preparation method of electronic material ultrafine gold powder - Google Patents
A kind of preparation method of electronic material ultrafine gold powder Download PDFInfo
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- CN107790739A CN107790739A CN201610736106.7A CN201610736106A CN107790739A CN 107790739 A CN107790739 A CN 107790739A CN 201610736106 A CN201610736106 A CN 201610736106A CN 107790739 A CN107790739 A CN 107790739A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a kind of preparation method of electronic material ultrafine gold powder, comprise the following steps：Fulminating gold solution, preparation reducing agent and dispersant solution, reduction reaction is prepared to produce bronze, prepare reducing solution, reaction precipitate processing.It the advantage is that：The preparation method is simple and safe, efficiency high and cost are low, and obtained ultrafine gold powder purity height, epigranular, particle diameter is small, is easy to mass produce；The preparation method advantages of simple, obtained ultrafine gold powder has the advantages of good dispersion, granularity are concentrated, specific surface area is small and tap density is big, and the conductor paste prepared using the ultrafine gold powder has the sintering film layer of excellent electric conductivity and sintering characteristic and densification.
Description
Technical field
The invention belongs to technical field of electronic materials, and in particular to a kind of preparation method of electronic material ultrafine gold powder.
Background technology
Electronic material is the material base of modern electronics industry and scientific technological advance, is primarily referred to as in electronic technology and micro-
The material used in electronic technology, including dielectric material, semi-conducting material, piezoelectricity and ferroelectric material, conducting metal and its alloy
Material, magnetic material, photoelectron material and other associated materials.Electronic material covering scope is extensive, and its major function is
This is as ray machine energy, or can influence the material of product electrical properties.Currently, electronic material is mainly used in IC manufactures, plane
The industries such as display, structure dress, printed circuit board (PCB), solar cell.The electric slurry product of form various kinds in the art now be present, so
And for existing electric slurry product, it is difficult to be provided simultaneously with sintering temperature is low, sintering time is short, energy-conserving and environment-protective, resistance
It is worth the combination property that low, adhesive force is good, solderability is good.
As the electrocondution slurry of one of electronic material, applied more because possessing many excellent properties.Conductive silver paste film forming
The key technical index such as rear high conductivity and compactness is determined by the performance of ultrafine gold powder, and ultrafine gold powder performance master
To depend on the morphological features such as its morphological structure, the granularity of powder and its distribution.At present, the preparation method master of ultrafine gold powder
There are Physical and chemical method.Physical mainly has gas evaporation coacervation, polishing and atomization etc.；Although Physical is easy
Easy to implement, cost is also low, but the ultrafine gold powder combination property prepared is not good enough.Chemical method is one or more of with reducing agent
Metal is deposited in the form of a powder from their salt or the complex aqueous solution, and now industrial ultrafine gold powder used is most
Prepared using this method, but due to the difference of dispensing, technological parameter etc., many ultrafine gold powders prepared using chemical method are pure
It is not ideal enough in the performances such as degree, granularity.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide a kind of preparation of electronic material ultrafine gold powder
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of system of electronic material ultrafine gold powder
Preparation Method, its innovative point are：Comprise the following steps：
（1）Prepare fulminating gold solution：Gold bullion is dissolved, prepares the gold solution that mass concentration is 20g/L, then ammonification water shape again
Into fulminating gold solution and pH values are adjusted to 3.0；
（2）Prepare reducing agent and dispersant solution：The reductant solution of preparation is ascorbic acid solution, and it is dissolved in by ascorbic acid
It is prepared in deionized water, concentration is 0.5~0.7mol/L；
（3）Prepare reducing solution：The dispersant solution of preparation is oleic acid solutions, its be dissolved in by oleic acid in absolute ethyl alcohol prepare and
Into concentration is 4~6g/L；
（4）Reduction reaction produces bronze：Dispersant solution is added into fulminating gold solution, is sufficiently stirred with 400r/min speed；
Reductant solution is added, with the min of 500r/min speed stirring reaction 25；
（5）Reaction precipitate processing：With 4 washing reaction sediments of deionized water and 96% ethanol point；Again will be anti-after washing
Answer sediment to be placed in 50 DEG C of vacuum drying chambers and dry 1h, powdered bronze is made.
Further, described step（2）In, the dispersant solution of preparation is polyvinylpyrrolidonesolution solution, and it is by gathering
Vinylpyrrolidone, which is dissolved in deionized water, to be prepared, concentration 2.5g/L.
Further, the quality proportioning of described polyvinylpyrrolidone and gold is 1：55.
Beneficial effects of the present invention are as follows：
A kind of preparation method of electronic material ultrafine gold powder, the preparation method is simple and safe, efficiency high and cost are low, obtained
Ultrafine gold powder purity height, epigranular, particle diameter is small, is easy to mass produce；The preparation method advantages of simple, it is obtained ultra-fine
Bronze has the advantages of good dispersion, granularity are concentrated, specific surface area is small and tap density is big, is led using prepared by the ultrafine gold powder
Somaplasm material has the sintering film layer of excellent electric conductivity and sintering characteristic and densification.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
A kind of preparation method of electronic material ultrafine gold powder, comprises the following steps：
（1）Prepare fulminating gold solution：Gold bullion is dissolved, prepares the gold solution that mass concentration is 20g/L, then ammonification water shape again
Into fulminating gold solution and pH values are adjusted to 3.0；
（2）Prepare reducing agent and dispersant solution：The reductant solution of preparation is ascorbic acid solution, and it is dissolved in by ascorbic acid
It is prepared in deionized water, concentration 0.5mol/L；
（3）Prepare reducing solution：The dispersant solution of preparation is oleic acid solutions, its be dissolved in by oleic acid in absolute ethyl alcohol prepare and
Into concentration 4g/L；
（4）Reduction reaction produces bronze：Dispersant solution is added into fulminating gold solution, is sufficiently stirred with 400r/min speed；
Reductant solution is added, with the min of 500r/min speed stirring reaction 25；
（5）Reaction precipitate processing：With 4 washing reaction sediments of deionized water and 96% ethanol point；Again will be anti-after washing
Answer sediment to be placed in 50 DEG C of vacuum drying chambers and dry 1h, powdered bronze is made.
Embodiment 2
A kind of preparation method of electronic material ultrafine gold powder, comprises the following steps：
（1）Prepare fulminating gold solution：Gold bullion is dissolved, prepares the gold solution that mass concentration is 20g/L, then ammonification water shape again
Into fulminating gold solution and pH values are adjusted to 3.0；
（2）Prepare reducing agent and dispersant solution：The reductant solution of preparation is ascorbic acid solution, and it is dissolved in by ascorbic acid
It is prepared in deionized water, concentration 0.7mol/L；
（3）Prepare reducing solution：The dispersant solution of preparation is oleic acid solutions, its be dissolved in by oleic acid in absolute ethyl alcohol prepare and
Into concentration 6g/L；
（4）Reduction reaction produces bronze：Dispersant solution is added into fulminating gold solution, is sufficiently stirred with 400r/min speed；
Reductant solution is added, with the min of 500r/min speed stirring reaction 25；
（5）Reaction precipitate processing：With 4 washing reaction sediments of deionized water and 96% ethanol point；Again will be anti-after washing
Answer sediment to be placed in 50 DEG C of vacuum drying chambers and dry 1h, powdered bronze is made.
Embodiment 3
A kind of preparation method of electronic material ultrafine gold powder, comprises the following steps：
（1）Prepare fulminating gold solution：Gold bullion is dissolved, prepares the gold solution that mass concentration is 20g/L, then ammonification water shape again
Into fulminating gold solution and pH values are adjusted to 3.0；
（2）Prepare reducing agent and dispersant solution：The reductant solution of preparation is ascorbic acid solution, and it is dissolved in by ascorbic acid
It is prepared in deionized water, concentration 0.6mol/L；
（3）Prepare reducing solution：The dispersant solution of preparation is oleic acid solutions, its be dissolved in by oleic acid in absolute ethyl alcohol prepare and
Into concentration 5g/L；
（4）Reduction reaction produces bronze：Dispersant solution is added into fulminating gold solution, is sufficiently stirred with 400r/min speed；
Reductant solution is added, with the min of 500r/min speed stirring reaction 25；
（5）Reaction precipitate processing：With 4 washing reaction sediments of deionized water and 96% ethanol point；Again will be anti-after washing
Answer sediment to be placed in 50 DEG C of vacuum drying chambers and dry 1h, powdered bronze is made.
The electric slurry produced below for the present invention in specific embodiment 1, specific embodiment 2 and specific embodiment 3
Can the index table of comparisons：
| Performance indications | Ascorbic acid concentrations | Dispersant solution concentration | Particle diameter | Purity |
| Embodiment 1 | 0.5mol/L | 4g/L | 0.3μm | 99.93% |
| Embodiment 2 | 0.7mol/L | 6g/L | 0.4μm | 99.94% |
| Embodiment 3 | 0.6mol/L | 5g/L | 0.2μm | 99.95% |
Visible according to upper table, comparative example 1, embodiment 2, embodiment 3, embodiment 3 have with respect to embodiment 1 and embodiment 2
The advantages of particle diameter is smaller, and purity is higher.
Preparation method of the invention is simple and safe, efficiency high and cost are low, and obtained ultrafine gold powder purity is high, granularity is equal
It is even, particle diameter is small, is easy to mass produce.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
The technical scheme that can be realized on the basis of above-described embodiment without creative work, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (3)
- A kind of 1. preparation method of electronic material ultrafine gold powder, it is characterised in that：Comprise the following steps：Prepare fulminating gold solution：Gold bullion is dissolved, prepares the gold solution that mass concentration is 20g/L, then ammonification water forms thunder again Sour gold solution simultaneously adjusts pH values to 3.0；Prepare reducing agent and dispersant solution：The reductant solution of preparation is ascorbic acid solution, and it is dissolved in by ascorbic acid It is prepared in ionized water, concentration is 0.5~0.7mol/L；Prepare reducing solution：The dispersant solution of preparation is oleic acid solutions, and it is dissolved in absolute ethyl alcohol by oleic acid is prepared, Concentration is 4~6g/L；Reduction reaction produces bronze：Dispersant solution is added into fulminating gold solution, is sufficiently stirred with 400r/min speed；Add Enter reductant solution, with the min of 500r/min speed stirring reaction 25；Reaction precipitate processing：With 4 washing reaction sediments of deionized water and 96% ethanol point；The reaction after washing is sunk again Starch, which is placed in 50 DEG C of vacuum drying chambers, dries 1h, and powdered bronze is made.
- A kind of 2. preparation method of electronic material ultrafine gold powder according to claim 1, it is characterised in that：Described step Suddenly（2）In, the dispersant solution of preparation is polyvinylpyrrolidonesolution solution, and it is dissolved in deionized water by polyvinylpyrrolidone It is prepared, concentration 2.5g/L.
- A kind of 3. preparation method of electronic material ultrafine gold powder according to claim 3, it is characterised in that：Described is poly- The quality proportioning of vinylpyrrolidone and gold is 1：55.
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| CN201610736106.7A CN107790739A (en) | 2016-08-29 | 2016-08-29 | A kind of preparation method of electronic material ultrafine gold powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111804905A (en) * | 2020-09-02 | 2020-10-23 | 西安宏星电子浆料科技股份有限公司 | Micron-sized spherical hollow gold powder and preparation method thereof |
| CN114160803A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-efficiency preparation method of high-dispersity spherical gold powder |
| CN114210989A (en) * | 2021-10-27 | 2022-03-22 | 长沙新材料产业研究院有限公司 | Micron-sized gold powder and preparation method thereof |
| CN114833334A (en) * | 2022-04-02 | 2022-08-02 | 有研工程技术研究院有限公司 | Method for continuously preparing micron-sized spherical gold powder |
-
2016
- 2016-08-29 CN CN201610736106.7A patent/CN107790739A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111804905A (en) * | 2020-09-02 | 2020-10-23 | 西安宏星电子浆料科技股份有限公司 | Micron-sized spherical hollow gold powder and preparation method thereof |
| CN114210989A (en) * | 2021-10-27 | 2022-03-22 | 长沙新材料产业研究院有限公司 | Micron-sized gold powder and preparation method thereof |
| CN114210989B (en) * | 2021-10-27 | 2023-11-21 | 航天科工(长沙)新材料研究院有限公司 | Micron-sized gold powder and preparation method thereof |
| CN114160803A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-efficiency preparation method of high-dispersity spherical gold powder |
| CN114833334A (en) * | 2022-04-02 | 2022-08-02 | 有研工程技术研究院有限公司 | Method for continuously preparing micron-sized spherical gold powder |
| CN114833334B (en) * | 2022-04-02 | 2023-08-15 | 有研工程技术研究院有限公司 | Method for continuously preparing micron-sized spherical gold powder |
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Application publication date: 20180313 |