CN104289728A - Preparation method of spherical superfine gold powder for electronic materials - Google Patents
Preparation method of spherical superfine gold powder for electronic materials Download PDFInfo
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- CN104289728A CN104289728A CN201410569150.4A CN201410569150A CN104289728A CN 104289728 A CN104289728 A CN 104289728A CN 201410569150 A CN201410569150 A CN 201410569150A CN 104289728 A CN104289728 A CN 104289728A
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Abstract
The invention provides a preparation method of spherical superfine gold powder for electronic materials. The preparation method includes the following steps: a), preparing a fulminic acid gold solution, b), preparing a reductant solution and a dispersant solution, c), preparing the gold powder through a reduction reaction and d), washing and drying the gold powder. The preparation method is simple and reasonable, the spherical superfine gold powder prepared according to the method has the advantages of high dispersibility, centralized granularity, small specific surface area and high tap density, and conductor paste made of the superfine gold powder has excellent electric conductivity and sintering characteristic and compact sintered membrane layers.
Description
Technical field
The present invention relates to a kind of electronic material, particularly relate to a kind of preparation method of electronic material spherical super fine bronze, belong to technical field of electronic materials.
Background technology
Electronic material is the material base of modern electronics industry and scientific technological advance, mainly refer to the material used in electronic technology and microelectric technique, comprise dielectric material, semi-conducting material, piezoelectricity and ferroelectric material, conducting metal and alloy material, magnetic material, photoelectron material and other associated materials.Electronic material covering scope is extensive, and its major function is that this is as ray machine energy, maybe can affect the material of product electrical properties.Current, electronic material is mainly used in the industries such as IC manufacture, flat-panel screens, structure dress, printed circuit board (PCB), solar cell.
As the electrocondution slurry of one of electronic material, apply more because possessing many excellent properties.Current, gold conductive paste is with its good conductivity, Fine line resolution is high, good with the adhesive strength of alumina substrate, the premium properties that printing is good, film surface is smooth, backlight porosity is little, film edge withdraw rate is little and tangent plane density is high, becomes the thick film conductor material of electronics integrated technology middle ideal.The key technical index of gold conductive paste is all determined by the bronze performance as gold conductive paste function phase, and bronze performance depends primarily on its appearance structure feature, the granularity of powder, the morphological feature such as tap density and distribution thereof.At present, the bronze of domestic production, due to the defect in preparation method, batching, technological parameter etc., causes in the performances such as appearance structure feature, tap density, granularity not ideal enough.
Summary of the invention
For the demand, the invention provides a kind of preparation method of electronic material spherical super fine bronze, this preparation method's advantages of simple, the obtained advantage that spherical super fine bronze has good dispersion, granularity is concentrated, specific area is little and tap density is large, the conductor paste adopting this ultrafine gold powder to prepare has the sintering rete of excellent electric conductivity and sintering characteristic and densification.
The present invention is a kind of preparation method of electronic material spherical super fine bronze, and described preparation method comprises the steps: a) to prepare fulminating gold solution, and b) prepare reductant solution and dispersant solution, c) reduction reaction produces bronze, d) the dry process of washing.
In a preferred embodiment of the present invention, in described step a), preparation fulminating gold solution comprises the steps: 1) dissolve gold bullion, preparation mass concentration is the gold solution of 30 g/L; 2) add ammoniacal liquor and form fulminating gold solution and adjusted to ph to 3.5.
In a preferred embodiment of the present invention, in described step b), the reductant solution of preparation is ascorbic acid solution, and it is dissolved in deionized water by ascorbic acid and is prepared from, and concentration is 0.5mol/L.
In a preferred embodiment of the present invention, described ascorbic acid is 1:2 with the quality proportioning of gold.
In a preferred embodiment of the present invention, in described step b), the dispersant solution of preparation is polyvinylpyrrolidonesolution solution, and it is dissolved in deionized water by polyvinylpyrrolidone and is prepared from, and concentration is 3g/L.
In a preferred embodiment of the present invention, described polyvinylpyrrolidone is 1:50 with the quality proportioning of gold.
In a preferred embodiment of the present invention, in described step c), reduction reaction is produced bronze and is comprised the steps: 1) in fulminating gold solution, add dispersant solution, fully stir with 350r/min speed; 2) reductant solution is added, with 450r/min speed stirring reaction 30 min.
In a preferred embodiment of the present invention, in described step d), the dry process of washing comprises the steps: 1) divide 3 washing reaction sediments with deionized water and absolute ethyl alcohol; 2) dry 1h in 50 DEG C of vacuum drying chambers.
Present invention is disclosed a kind of preparation method of electronic material spherical super fine bronze, this preparation method's advantages of simple, the obtained advantage that spherical super fine bronze has good dispersion, granularity is concentrated, specific area is little and tap density is large, the conductor paste adopting this ultrafine gold powder to prepare has the sintering rete of excellent electric conductivity and sintering characteristic and densification.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation:
Fig. 1 is the process figure of embodiment of the present invention electronic material spherical super fine bronze preparation method.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Fig. 1 is the process figure of embodiment of the present invention electronic material spherical super fine bronze preparation method; This preparation method comprises the steps: a) to prepare fulminating gold solution, and b) prepare reductant solution and dispersant solution, c) reduction reaction produces bronze, d) the dry process of washing.
Embodiment
Concrete preparation method is as follows:
A) prepare fulminating gold solution, concrete process for preparation is: first a certain amount of gold bullion is placed in dissolution vessel, adds a small amount of deionized water, low-grade fever, more repeatedly adds appropriate aqua regia dissolution gold bullion, after gold bullion dissolves completely, repeatedly adds concentrated hydrochloric acid, carries out catching up with nitre; When without brown fume, repeatedly add deionized water and catch up with acid; Solution being concentrated into concentration after without sharp aroma is after 30 g/L, for subsequent use.Then in gold solution, ammoniacal liquor adjusted to ph is added to alkalescent, fully to form fulminating gold solution; Finally by hydrochloric acid adjustment fulminating gold solution ph to 3.5.
B) prepare reductant solution and dispersant solution, concrete process for preparation is: first get a certain amount of ascorbic acid, and it is 1:2 with the quality proportioning of gold, is dissolved in deionized water, is made into the reductant solution that concentration is 0.5mol/L; Then get appropriate polyvinylpyrrolidone, its quality is 2% of gold, is dissolved in deionized water and is made into the dispersant solution that concentration is 3g/L.
C) reduction reaction produces bronze, and concrete preparation process is: first poured into by the fulminating gold solution that step a) is prepared and be provided with in the special container of agitating device, then add dispersant solution in fulminating gold solution, fully stir with 350r/min speed; Then add reductant solution rapidly, with 450r/min speed stirring reaction 30 min, reacted product forms bronze sediment after natural subsidence, and takes out.
D) the dry process of washing, concrete processing procedure is: first spend deionized water reaction precipitation thing 3 times, then uses absolute ethanol washing reaction precipitation thing 3 times; Then be placed in vacuum drying chamber by the reaction precipitation thing after washing, at 50 DEG C, dry 1h obtains Powdered bronze.
Present invention is disclosed a kind of preparation method of electronic material spherical super fine bronze, this preparation method's advantages of simple, the obtained advantage that spherical super fine bronze has good dispersion, granularity is concentrated, specific area is little and tap density is large, the conductor paste adopting this ultrafine gold powder to prepare has the sintering rete of excellent electric conductivity and sintering characteristic and densification.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope disclosed by the present invention; the change can expected without creative work or replacement, all should be encompassed within protection scope of the present invention.Therefore, the protection domain that protection scope of the present invention should limit with claims is as the criterion.
Claims (8)
1. the electronic material preparation method of spherical super fine bronze, it is characterized in that, described preparation method comprises the steps: a) to prepare fulminating gold solution, b) prepares reductant solution and dispersant solution, c) reduction reaction produces bronze, d) the dry process of washing.
2. the preparation method of electronic material spherical super fine bronze according to claim 1, is characterized in that, in described step a), preparation fulminating gold solution comprises the steps: 1) dissolve gold bullion, preparation mass concentration is the gold solution of 30 g/L; 2) add ammoniacal liquor and form fulminating gold solution and adjusted to ph to 3.5.
3. the preparation method of electronic material spherical super fine bronze according to claim 1, it is characterized in that, in described step b), the reductant solution of preparation is ascorbic acid solution, it is dissolved in deionized water by ascorbic acid and is prepared from, and concentration is 0.5mol/L.
4. the preparation method of electronic material spherical super fine bronze according to claim 3, is characterized in that, described ascorbic acid is 1:2 with the quality proportioning of gold.
5. the preparation method of electronic material spherical super fine bronze according to claim 1, it is characterized in that, in described step b), the dispersant solution of preparation is polyvinylpyrrolidonesolution solution, it is dissolved in deionized water by polyvinylpyrrolidone and is prepared from, and concentration is 3g/L.
6. the preparation method of electronic material spherical super fine bronze according to claim 5, is characterized in that, described polyvinylpyrrolidone is 1:50 with the quality proportioning of gold.
7. the preparation method of electronic material spherical super fine bronze according to claim 1, it is characterized in that, in described step c), reduction reaction is produced bronze and is comprised the steps: 1) in fulminating gold solution, add dispersant solution, fully stir with 350r/min speed; 2) reductant solution is added, with 450r/min speed stirring reaction 30 min.
8. the preparation method of electronic material spherical super fine bronze according to claim 1, is characterized in that, in described step d), the dry process of washing comprises the steps: 1) divide 3 washing reaction sediments with deionized water and absolute ethyl alcohol; 2) dry 1h in 50 DEG C of vacuum drying chambers.
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| CN201410569150.4A CN104289728A (en) | 2014-10-23 | 2014-10-23 | Preparation method of spherical superfine gold powder for electronic materials |
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| CN201410569150.4A CN104289728A (en) | 2014-10-23 | 2014-10-23 | Preparation method of spherical superfine gold powder for electronic materials |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114247896A (en) * | 2021-12-28 | 2022-03-29 | 成都市天甫金属粉体有限责任公司 | Simple preparation method and application of 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 |
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| CN1227148A (en) * | 1999-01-19 | 1999-09-01 | 沈阳黎明发动机制造公司 | High purity high dispersiveness spherical super fine silver powder and its producing method |
| JP2001107101A (en) * | 1999-10-12 | 2001-04-17 | Mitsui Mining & Smelting Co Ltd | High dispersibility spherical silver powder and its producing method |
| CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
| CN101774026A (en) * | 2009-10-21 | 2010-07-14 | 电子科技大学 | Solid-phase reaction superfine silver powder preparation method |
| CN102000835A (en) * | 2010-12-20 | 2011-04-06 | 昆明理工大学 | Method for preparing micron spherical silver powder |
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2014
- 2014-10-23 CN CN201410569150.4A patent/CN104289728A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1227148A (en) * | 1999-01-19 | 1999-09-01 | 沈阳黎明发动机制造公司 | High purity high dispersiveness spherical super fine silver powder and its producing method |
| JP2001107101A (en) * | 1999-10-12 | 2001-04-17 | Mitsui Mining & Smelting Co Ltd | High dispersibility spherical silver powder and its producing method |
| CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
| CN101774026A (en) * | 2009-10-21 | 2010-07-14 | 电子科技大学 | Solid-phase reaction superfine silver powder preparation method |
| CN102000835A (en) * | 2010-12-20 | 2011-04-06 | 昆明理工大学 | Method for preparing micron spherical silver powder |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114247896A (en) * | 2021-12-28 | 2022-03-29 | 成都市天甫金属粉体有限责任公司 | Simple preparation method and application of 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: 20150121 |