CN101695757A - Method for preparing aluminium powder with high tap density - Google Patents
Method for preparing aluminium powder with high tap density Download PDFInfo
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- CN101695757A CN101695757A CN200910218664A CN200910218664A CN101695757A CN 101695757 A CN101695757 A CN 101695757A CN 200910218664 A CN200910218664 A CN 200910218664A CN 200910218664 A CN200910218664 A CN 200910218664A CN 101695757 A CN101695757 A CN 101695757A
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- silver
- deionized water
- sodium carbonate
- tap density
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Abstract
The invention discloses a method for preparing aluminum powder with high tap density, which comprises the following steps: dissolving 100 weight parts of silver nitrate and one weight part of hydrogen nitrite in deionized water to form 30 to 60 percent silver nitrate solution; dissolving 60 weight parts of sodium carbonate in deionized water to form 5 to 25 percent sodium carbonate solution; adding the silver nitrate solution into the sodium carbonate solution under the condition of continuous stirring to prepare a precursor silver carbonate system, wherein the mixture is alkalescent; keeping the temperature of the precursor silver carbonate system at 15-25 DEG C, quickly adding a formidable reductant to complete the reduction reaction under the condition of continuous stirring; washing the obtained product for 15-20 times by using deionized water after reaction, and then filtering the deionized water, and drying to consequently obtain the required silver powder. Compared with the conventional vacuum atomization method, the invention has the advantages of low cost and simple operation.
Description
Technical field
The invention belongs to technical field of electronic materials, be specifically related to a kind of silver powder preparation method of high-bulk-density.
Background technology
Silver powder is because the high conductivity and the low-cost characteristics that self have have more and more important use in the electronics and information industry field, as is applied to the filler, electric slurry, electrically conductive ink, shielding coating etc. of conductive rubber.
The filling perforation electrocondution slurry of using in the present electronics and information industry, because matrix does not shrink in sintering process, therefore require slurry in use, there is not the sintering shrinkage phenomenon yet, and the most of kind slurry of present employed feel, owing to the powder metallization processes is arranged in the high temperature sintering stage, therefore behind the sintering, there is shrinkage phenomenon in the capital, and in order to control the generation of this phenomenon, the best way just is to use the silver powder of high-bulk-density.
Preparing at present both at home and abroad the method that aluminium powder with high tap density generally adopts is physics methods such as vacuum atomizing method, because a whole set of production equipment costliness of vacuum atomizing method, cost is higher relatively, be unfavorable for the popularization of industrialization, therefore seek a kind of suitable, cheaply, the chemical method easy and simple to handle silver powder for preparing high-bulk-density is very necessary.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of cost aluminium powder with high tap density low, simple to operate.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of aluminium powder with high tap density, in deionized water, forming concentration is the liquor argenti nitratis ophthalmicus of 30-60% with the nitric acid dissolve of the silver nitrate of 100 weight portions and 1 weight portion; The 50-65 weight parts of sodium carbonate is dissolved in the deionized water, and forming concentration is the sodium carbonate liquor of 5-25%; Under lasting stirring condition, above-mentioned liquor argenti nitratis ophthalmicus is added in the described sodium carbonate liquor, make presoma silver carbonate system, the mixed liquor of this moment is alkalescent; Control above-mentioned presoma silver carbonate system temperature at 15 ℃-25 ℃, add strong reductant fast and finish reduction reaction under the stirring condition continuing, after reduction is finished, spend deionised water 15-20 all over after, leach deionized water, drying obtains the silver powder that needs.
Further technical scheme of the present invention is, described strong reductant can be selected a kind of in formaldehyde, hydrazine hydrate, the sodium borohydride.
The present invention takes the chemical reduction reaction legal system to be equipped with aluminium powder with high tap density, and the particle diameter that makes silver powder is the 0.5-1.5 micron, and bulk density is the 3.0-5.0 grams per milliliter, compares with conventional vacuum atomization method, and the present invention has the low and advantages of simple operation of cost.
The specific embodiment:
A kind of preparation method of aluminium powder with high tap density, in deionized water, forming concentration is the liquor argenti nitratis ophthalmicus of 30-60% with the nitric acid dissolve of the silver nitrate of 100 weight portions and 1 weight portion; The 50-65 weight parts of sodium carbonate is dissolved in the deionized water, and forming concentration is the sodium carbonate liquor of 5-25%; Under lasting stirring condition, above-mentioned liquor argenti nitratis ophthalmicus is added in the described sodium carbonate liquor, make presoma silver carbonate system, the mixed liquor of this moment is alkalescent; Control above-mentioned presoma silver carbonate system temperature at 15 ℃-25 ℃, add strong reductant fast and finish reduction reaction under the stirring condition continuing, after reduction is finished, spend deionised water 15-20 all over after, leach deionized water, drying obtains the silver powder that needs.
Described strong reductant can be a kind of in formaldehyde, hydrazine hydrate, the sodium borohydride.
The concentration of described liquor argenti nitratis ophthalmicus is 50%.
The concentration of described sodium carbonate liquor is 15%.
Presoma silver carbonate system temperature is controlled to be 20 ℃ in the described reduction reaction.
Below by embodiment the present invention is described in further detail.
Embodiment 1
1. weighing silver nitrate 100 weight portions are dissolved in the deionized water of 150 parts of weight, add the nitric acid of 1 weight portion again in liquor argenti nitratis ophthalmicus, and fully stirring and evenly mixing is standby;
2. weighing 60 weight parts of sodium carbonate are dissolved in the deionized water of 200 weight portions, stir, and are standby,
3. under lasting stirring condition,, be added in the sodium carbonate liquor, make the presoma silver carbonate liquor argenti nitratis ophthalmicus;
4. the hydrazine hydrate of weighing 10 weight portions is dissolved in 10 parts by weight of deionized water, stirs, and is standby;
5. with the method for water-bath, adjust the silver carbonate solution system temperature to 15 ℃ in the 3rd step, continue under the stirring condition, the hydrazine hydrate solution with the 4th step is added in the silver carbonate solution fast, finishes reduction;
6. the silver powder mixed liquor after will reducing spends deionised water 20 times, filters ionized water, and drying obtains the silver powder that needs.The particle diameter of test silver powder is 1.3 microns, and bulk density is 4.6 grams per milliliters.
Embodiment 2
1. weighing silver nitrate 100 weight portions are dissolved in the deionized water of 100 parts of weight, add the nitric acid of 1 weight portion again in liquor argenti nitratis ophthalmicus, and fully stirring and evenly mixing is standby;
2. weighing 60 weight parts of sodium carbonate are dissolved in the deionized water of 240 weight portions, stir, and are standby,
3. under lasting stirring condition,, be added in the sodium carbonate liquor, make the presoma silver carbonate liquor argenti nitratis ophthalmicus;
4. the hydrazine hydrate of weighing 10 weight portions is dissolved in 10 parts by weight of deionized water, stirs, and is standby;
5. with the method for water-bath, adjust the silver carbonate solution system temperature to 20 ℃ in the 3rd step, continue under the stirring condition, the hydrazine hydrate solution with the 4th step is added in the silver carbonate solution fast, finishes reduction;
6. the silver powder mixed liquor after will reducing spends deionised water 20 times, filters ionized water, and drying obtains the silver powder that needs.The particle diameter of test silver powder is 1.0 microns, and bulk density is 4.0 grams per milliliters.
Embodiment 3
1. weighing concentration is 60% liquor argenti nitratis ophthalmicus 160 weight portions, and is standby;
2. weighing concentration is 15% sodium carbonate liquor 420 weight portions, and is standby;
3. weighing concentration is 80% sodium borohydride solution 20 weight portions;
4. under lasting stirring condition,, be added in the sodium carbonate liquor, make the presoma silver carbonate liquor argenti nitratis ophthalmicus;
5. with the method for water-bath, adjust the silver carbonate solution system temperature to 25 ℃ in the 4th step, continue under the stirring condition, the sodium borohydride solution with the 3rd step is added in the silver carbonate solution fast, finishes reduction;
6. the silver powder mixed liquor after will reducing spends deionised water 20 times, filters ionized water, and drying obtains the silver powder that needs.The particle diameter of test silver powder is 0.6 micron, and bulk density is 3.5 grams per milliliters.
Embodiment 4
1. weighing silver nitrate 100 weight portions are dissolved in the deionized water of 100 weight portions, add the nitric acid of 1 weight portion again in liquor argenti nitratis ophthalmicus, and fully stirring and evenly mixing is standby;
2. weighing 60 weight parts of sodium carbonate are dissolved in the deionized water of 300 weight portions, stir, and are standby;
3. under lasting stirring condition,, be added in the sodium carbonate liquor, make the presoma silver carbonate liquor argenti nitratis ophthalmicus;
4. the formaldehyde of weighing 50 weight portions is dissolved in 50 parts by weight of deionized water, stirs, and is standby;
5. with the method for water-bath, adjust the silver carbonate solution system temperature to 20 ℃ in the 3rd step, continue under the stirring condition, the formaldehyde in the 4th step is added in the silver carbonate solution fast, finish reduction;
6. the silver powder mixed liquor after will reducing spends deionised water 20 times, filters ionized water, and drying obtains the silver powder that needs.The particle diameter of test silver powder is 1.1 microns, and bulk density is 4.8 grams per milliliters.
Claims (5)
1. the preparation method of an aluminium powder with high tap density is characterized in that: in deionized water, forming concentration is the liquor argenti nitratis ophthalmicus of 30-60% with the nitric acid dissolve of the silver nitrate of 100 weight portions and 1 weight portion; The 50-65 weight parts of sodium carbonate is dissolved in the deionized water, and forming concentration is the sodium carbonate liquor of 5-25%; Under lasting stirring condition, above-mentioned liquor argenti nitratis ophthalmicus is added in the described sodium carbonate liquor, make presoma silver carbonate system, the mixed liquor of this moment is alkalescent; Control above-mentioned presoma silver carbonate system temperature at 15 ℃-25 ℃, add strong reductant fast and finish reduction reaction under the stirring condition continuing, after reduction is finished, spend deionised water 15-20 all over after, leach deionized water, drying obtains the silver powder that needs.
2. the preparation method of aluminium powder with high tap density according to claim 1 is characterized in that: described strong reductant can be a kind of in formaldehyde, hydrazine hydrate, the sodium borohydride.
3. the preparation method of aluminium powder with high tap density according to claim 1, it is characterized in that: the concentration of described liquor argenti nitratis ophthalmicus is 50%.
4. the preparation method of aluminium powder with high tap density according to claim 1, it is characterized in that: the concentration of described sodium carbonate liquor is 15%.
5. the preparation method of aluminium powder with high tap density according to claim 1, it is characterized in that: presoma silver carbonate system temperature is controlled to be 20 ℃ in the described reduction reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102186644A CN101695757B (en) | 2009-10-29 | 2009-10-29 | Method for preparing aluminium powder with high tap density |
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| CN2009102186644A CN101695757B (en) | 2009-10-29 | 2009-10-29 | Method for preparing aluminium powder with high tap density |
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| CN101695757A true CN101695757A (en) | 2010-04-21 |
| CN101695757B CN101695757B (en) | 2011-10-05 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941078A (en) * | 2010-09-27 | 2011-01-12 | 彩虹集团公司 | Silver powder for electrode paste of solar cell and preparation method thereof |
| CN102133635A (en) * | 2011-05-02 | 2011-07-27 | 杨荣春 | Silver powder and manufacturing method thereof |
| CN102248176A (en) * | 2011-07-15 | 2011-11-23 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| CN102581289A (en) * | 2012-03-15 | 2012-07-18 | 中南大学 | Method for preparing monodisperse high-crystallinity 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 |
| CN105081343A (en) * | 2015-08-03 | 2015-11-25 | 佛山市顺德区百锐新电子材料有限公司 | Manufacturing method for conductive silver powder used for touch screen UV-type laser engraving silver paste |
| CN113084189A (en) * | 2021-04-08 | 2021-07-09 | 中船重工黄冈水中装备动力有限公司 | Preparation method of silver powder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003253312A (en) * | 2002-03-01 | 2003-09-10 | Murata Mfg Co Ltd | Method for manufacturing silver powder, and silver powder |
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN100519015C (en) * | 2006-06-13 | 2009-07-29 | 上海宝银电子材料有限公司 | Chemical reduction process of preparing silver powder |
| CN100506440C (en) * | 2007-07-11 | 2009-07-01 | 中国印钞造币总公司 | Preparation process of micro silver powder |
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2009
- 2009-10-29 CN CN2009102186644A patent/CN101695757B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941078A (en) * | 2010-09-27 | 2011-01-12 | 彩虹集团公司 | Silver powder for electrode paste of solar cell and preparation method thereof |
| CN102133635A (en) * | 2011-05-02 | 2011-07-27 | 杨荣春 | Silver powder and manufacturing method thereof |
| CN102248176A (en) * | 2011-07-15 | 2011-11-23 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| CN102248176B (en) * | 2011-07-15 | 2012-08-22 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| CN102581289A (en) * | 2012-03-15 | 2012-07-18 | 中南大学 | Method for preparing monodisperse high-crystallinity 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 |
| CN103143723B (en) * | 2013-03-27 | 2015-09-30 | 深圳市中金岭南科技有限公司 | A kind of method preparing the flake silver powder of low-apparent-density |
| CN105081343A (en) * | 2015-08-03 | 2015-11-25 | 佛山市顺德区百锐新电子材料有限公司 | Manufacturing method for conductive silver powder used for touch screen UV-type laser engraving silver paste |
| CN113084189A (en) * | 2021-04-08 | 2021-07-09 | 中船重工黄冈水中装备动力有限公司 | Preparation method of silver powder |
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| CN101695757B (en) | 2011-10-05 |
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