CN102764897A - Method for preparing submicron silver powder for electro-conductive paste - Google Patents
Method for preparing submicron silver powder for electro-conductive paste Download PDFInfo
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- CN102764897A CN102764897A CN2012102810748A CN201210281074A CN102764897A CN 102764897 A CN102764897 A CN 102764897A CN 2012102810748 A CN2012102810748 A CN 2012102810748A CN 201210281074 A CN201210281074 A CN 201210281074A CN 102764897 A CN102764897 A CN 102764897A
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Abstract
The invention belongs to the field of electro-conductive paste and particularly relates to a method for preparing a submicron silver powder for the electro-conductive paste, comprising the step of adding a dispersing agent and a reducing agent into a silver salt aqueous solution to reduce the elemental silver. The method is characterized in that nano-silver particles are added into the silver salt aqueous solution before the dispersing agent and the reducing agent are added, wherein the nano-silver particles have the size of 5-10nm, and the addition amount of the nano-silver particles is 0.3-0.6 per mill of the mass of the silver salt which is the solute in the silver salt aqueous solution. The method is simple in process and has a low requirement for equipment. The raw materials are environmentally friendly and cause less pollution. The submicron silver powder prepared by adopting the method has uniform particle size and a narrow distribution range.
Description
Technical field
The present invention relates to the electrocondution slurry field, refer to a kind of preparation method who is used for the submicron order silver powder of electrocondution slurry especially.
Background technology
Electrocondution slurry has been widely used in the every field of electron trades such as wafer capacitance device, potentiometer, thick film hybrid integrated circuit, sensing element, surface installation technique.At present most widely used is with the conductive silver slurry of silver as conductive phase.Wherein, Silver is present in the electrocondution slurry with the form of silver powder; Powder characteristics such as the shape of silver powder, size, loose dress ratio and flowability have decisive influence to the combination property of electrocondution slurry, and the silver powder different preparation is then given powder characteristics such as the different shape of silver powder, size, pine dress ratio and flowability.
The present modal method for preparing silver powder is the wet-chemical reducing process; Be meant in the aqueous solution of silver salt or in the suspension of oxide, silver carbonate and other insoluble compounds of silver; Add certain dispersant and other morphology control agent; Utilize reducing agent that silver-colored simple substance is restored, give characteristics such as the specific shape of silver powder, size simultaneously, promptly obtain can be used for preparing the silver powder of electrocondution slurry after the oven dry.Technology is simple though the method has, processing ease, low power consumption and other advantages; Shortcomings such as but the particle size distribution range that but exists silver powder is wide, pattern is inconsistent, particle diameter is inhomogeneous, particle diameter is bigger cause adopting the performances such as electric conductivity of electrocondution slurry of this silver powder outstanding inadequately.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, a kind of preparation method who is used for the submicron order silver powder of electrocondution slurry is provided, utilize silver powder epigranular, the narrow distribution range of this method preparation.
For realizing above-mentioned purpose; The invention provides a kind of preparation method who is used for the submicron order silver powder of electrocondution slurry; Be included in the silver salt solution and add dispersant and reducing agent restores silver-colored simple substance; It is characterized in that: in silver salt solution, add nano silver particles earlier before adding dispersant and reducing agent, the particle diameter of said nano silver particles is 5 ~ 10nm, the addition of said nano silver particles be in the silver salt solution silver salt solute quality 0.3 ‰ ~ 6 ‰.
Preferably, the Ag in the said silver salt solution
+Concentration is 5 * 10
-3Mol/L ~ 5 * 10
-1Mol/L, the reaction temperature of solution is 10 ~ 60 ℃.
Preferably; Said dispersant is one or more the aqueous solution in dodecyl sodium sulfate, glycerine, propane diols and the cetomacrogol 1000 0; The mass ratio of the silver salt solute in said dispersant and the silver salt solution is 1:50 ~ 1:200, and the concentration of aqueous solution of said dispersant is 0.5g/L ~ 5g/L.
Preferably, said reducing agent is the aqueous solution of ascorbic acid, sodium ascorbate, ferrous sulfate heptahydrate, glucose, formaldehyde or sodium hypophosphite, the Ag in said reducing agent and the silver salt solution
+Mol ratio be 1:1 ~ 2:1, the concentration of aqueous solution of said reducing agent is 100g/L ~ 500g/L.
Preferably, said preparation method also comprises: after question response is complete, earlier gained solution is filtered, clean filtering resulting silver powder with deionized water and absolute ethyl alcohol respectively.
Preferably, said nano silver particles adopts following method preparation: at Ag
+Concentration is 1 * 10
-4Mol/L ~ 1 * 10
-2Add dispersant in the silver salt solution of mol/L, keep system temperature, add reducing agent while stirring at 5 ~ 10 ℃; The mass ratio of the silver salt solute in the silver salt solution of the dispersant of said preparation nano silver particles and preparation nano silver particles is 0.5:1 ~ 2:1, and the concentration of aqueous solution of the dispersant of said preparation nano silver particles is 0.1g/L ~ 0.5g/L; Ag in the silver salt solution of the reducing agent of said preparation nano silver particles and preparation nano silver particles
+Mol ratio be 0.1:1 ~ 1:1.
Preferably, the dispersant of said preparation nano silver particles is one or more in polyacrylic acid, Sodium Polyacrylate, gelatin and the gum arabic.
Preferably, the reducing agent of said preparation nano silver particles is the aqueous solution of sodium borohydride, potassium borohydride or hydrazine hydrate, and the concentration of aqueous solution of the reducing agent of said preparation nano silver particles is 1g/L ~ 10g/L.
Beneficial effect:
Compared with prior art, the present invention has the following advantages:
1, the present invention improves the method for existing preparation silver powder; Through before reaction, adding certain amount of nano silver crystal seed, make the silver particles of when reaction, separating out be deposited on the Nano Silver crystal seed, and slowly grow up to the silver-colored particle of specific pattern and size; The silver powder that this kind improved one's methods and prepared; Particle diameter can reach submicron order, epigranular, narrow distribution range, and through the quantity of control crystal seed and pattern and the size that concentration can be controlled obtained silver powder well;
2, preparation method's technology provided by the invention is simple, low for equipment requirements, raw material is little than environmental protection, pollution.
Description of drawings
Fig. 1 is the particle size distribution figure of the silver powder of the embodiment of the invention 1 preparation;
Fig. 2 is the particle size distribution figure of the silver powder of the embodiment of the invention 2 preparations;
Fig. 3 is the particle size distribution figure of the silver powder of the embodiment of the invention 3 preparations;
Fig. 4 is the particle size distribution figure of the silver powder of the embodiment of the invention 4 preparations;
Fig. 5 is the particle size distribution figure of the silver powder of the embodiment of the invention 5 preparations.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further detailed description, following examples are that the present invention is not limited to following examples to explanation of the present invention.
The preparation method of submicron order silver powder provided by the invention was divided into for two steps:
The first step is the preparation of nano silver particles: at Ag
+Concentration is 1 * 10
-4Mol/L ~ 1 * 10
-2In the silver salt solution of mol/L; Mass ratio 0.5:1 ~ 2:1 according to the silver salt solute in dispersant and the silver salt solution adds dispersant; Utilize cooling device to make system temperature remain on 5 ~ 10 ℃; Add the aqueous solution that concentration is the reducing agent of 1g/L ~ 10g/L while stirring, the addition of reducing agent be with silver salt solution in Ag
+Mol ratio be 0.1:1 ~ 1:1, prepare the silver particles sol solution of 5 ~ 10nm.
Second step was the preparation of silver powder: to Ag
+Concentration is 5 * 10
-3Mol/L ~ 5 * 10
-1The nano silver particles sol solution that adds first step preparation in the silver salt solution of mol/L is as seed; The addition of seed be in the silver salt solution the silver salt quality 0.3 ‰ ~ 6 ‰; Keeping reaction temperature is 10 ~ 60 ℃, dropwise adds the aqueous solution of reducing agent and dispersant while stirring, and the mass ratio of the silver salt solute in dispersant and the silver salt solution is 1:50 ~ 1:200; The concentration of aqueous solution of dispersant is 0.5g/L ~ 5g/L, the Ag in reducing agent and the silver salt solution
+Mol ratio be 1:1 ~ 2:1, the concentration of aqueous solution of reducing agent is 100g/L ~ 500g/L; Filter after question response is complete, use earlier washed with de-ionized water, clean with absolute ethyl alcohol, place drying box at last, drying is 15 ~ 24 hours under 70 ℃, obtains submicron order silver powder.
The mensuration of granularity: measuring used instrument is the JL-1166 type laser particle analyzer that Jingxin Power Testing Apparatus Co., Ltd., Chengdu makes; Method is for getting 2 ~ 5 gram silver powder samples; Place the water of tester sample room under ultrasonic dispersion, to test; Reach between 50 ~ 80 at the instrument display density, read the D of the sample under its CF pattern
50Numerical value.
Embodiment 1
The preparation of silver powder: in agitated reactor, add 50 liters of deionized waters, dissolve in 450 gram silver nitrates, system temperature remains on 30 ℃; Take by weighing 450 gram ascorbic acid and 3 gram glycerine and 1.5 gram polyethylene glycol, 2 liters of deionized water dissolvings, temperature remains on 30 ℃; Be added drop-wise in the liquor argenti nitratis ophthalmicus slowly; Dripped off in about 30 minutes, and stirred again 10 minutes, until reacting completely.Stop to stir,, with 2 liters of washed with de-ionized water 5 times, with 500 milliliters of absolute ethyl alcohols cleanings 2 times, place vacuum drying chamber more earlier,, dried 20 hours, obtain silver powder, D in 70 ℃ with the suspension suction filtration
50=0.37 micron.
Embodiment 2
The preparation of nano silver particles: in agitated reactor, add 5 liters of deionized waters, dissolve in 1.8 gram silver nitrates, add 1.8 gram gelatin, dissolving, cooling device makes system cool to 5 ℃; Take by weighing 0.3 gram sodium borohydride, be dissolved in 100 ml waters, also cool to 5 ℃, join fast then in the liquor argenti nitratis ophthalmicus, stir, obtain the sol solution of nano silver particles until reacting completely.
The preparation of silver powder: in another agitated reactor, add 50 liters of deionized waters, dissolve in 450 gram silver nitrates, in the vigorous stirring process, above-mentioned nano silver particles sol solution is added wherein as seed, system temperature remains on 30 ℃; Take by weighing 450 gram ascorbic acid and 3 gram glycerine and 1.5 gram polyethylene glycol, 2 liters of deionized water dissolvings, temperature remains on 30 ℃, is added drop-wise to slowly in the liquor argenti nitratis ophthalmicus, drips off in about 30 minutes, stirs 10 minutes, until reacting completely again.Stop to stir,, with 2 liters of washed with de-ionized water 5 times, with 500 milliliters of absolute ethyl alcohols cleanings 2 times, place vacuum drying chamber more earlier,, dried 20 hours, obtain silver powder, D in 70 ℃ with the suspension suction filtration
50=0.21 micron.
Embodiment 3
The preparation of nano silver particles: in agitated reactor, add 5 liters of deionized waters, dissolve in 1.8 gram silver nitrates, add 2.0 gram Sodium Polyacrylates, dissolving, cooling device makes system cool to 5 ℃; Take by weighing 0.25 gram hydrazine hydrate, be dissolved in 100 ml waters, also cool to 5 ℃, join fast then in the liquor argenti nitratis ophthalmicus, stir, obtain the sol solution of nano silver particles until reacting completely.
The preparation of silver powder: in another agitated reactor, add 50 liters of deionized waters, dissolve in 450 gram silver nitrates, in the vigorous stirring process, above-mentioned nano silver particles sol solution is added wherein as seed, system temperature remains on 25 ℃.Take by weighing 695 gram ferrous sulfate heptahydrates, 5 gram propane diols and 2 gram polyethylene glycol, 2 liters of deionized water dissolvings maintain the temperature at 25 ℃, are added drop-wise to slowly in the liquor argenti nitratis ophthalmicus, drip off in about 30 minutes, stir 10 minutes, until reacting completely again.Stop to stir,, with 2 liters of washed with de-ionized water 5 times, with 500 milliliters of absolute ethyl alcohols cleanings 2 times, place vacuum drying chamber more earlier the suspension suction filtration, 70 ℃, dried 20 hours, obtain silver powder, D
50=0.19 micron.
Embodiment 4
The preparation of nano silver particles: in agitated reactor, add 5 liters of deionized waters, dissolve in 2.7 gram silver nitrates, add 0.5 gram gelatin and 0.5 gram Sodium Polyacrylate, 0.5 gram gum arabic, dissolving, cooling device makes system cool to 5 ℃; Take by weighing 0.4 gram sodium borohydride, be dissolved in 100 ml waters, also cool to 5 ℃, join fast then in the liquor argenti nitratis ophthalmicus, stir, obtain the sol solution of nano silver particles until reacting completely.
The preparation of silver powder: in another agitated reactor, add 50 liters of deionized waters, dissolve in 300 gram silver nitrates, in the vigorous stirring process, above-mentioned nano silver particles sol solution is added wherein as seed, system temperature remains on 40 ℃.Take by weighing 500 gram sodium ascorbates and 2 gram dodecyl sodium sulfates, 2 gram glycerine, 2 liters of deionized water dissolvings, temperature remains on 40 ℃, is added drop-wise to slowly in the liquor argenti nitratis ophthalmicus, drips off in about 30 minutes, stirs 10 minutes, until reacting completely again.Stop to stir,, with 2 liters of washed with de-ionized water 5 times, with 500 milliliters of absolute ethyl alcohols cleanings 2 times, place vacuum drying chamber more earlier the suspension suction filtration, 70 ℃, dried 20 hours, obtain silver powder, D
50=0.17 micron.
Embodiment 5
The preparation of nano silver particles: in agitated reactor, add 5 liters of deionized waters, dissolve in 3.6 gram silver nitrates, add 1.0 gram gelatin and 1.0 gram Sodium Polyacrylates, dissolving, cooling device makes system cool to 5 ℃; Take by weighing 0.86 gram potassium borohydride, be dissolved in 100 ml waters, also cool to 5 ℃, join fast then in the liquor argenti nitratis ophthalmicus, stir, obtain the sol solution of nano silver particles until reacting completely.
The preparation of silver powder: in another agitated reactor, add 50 liters of deionized waters, dissolve in 450 gram silver nitrates, in the vigorous stirring process, above-mentioned nano silver particles sol solution is added wherein as seed, system temperature remains on 50 ℃.Take by weighing 450 gram glucose and 4.5 gram dodecyl sodium sulfates, 2 liters of deionized water dissolvings, temperature remains on 50 ℃, is added drop-wise to slowly in the liquor argenti nitratis ophthalmicus, drips off in about 30 minutes, stirs 10 minutes, until reacting completely again.Stop to stir, with the suspension suction filtration, earlier with 2 liters of washed with de-ionized water 5 times, again with 500 milliliters of absolute ethyl alcohols cleanings 2 times, 70 ℃, dried 20 hours, obtain silver powder, D
50=0.16 micron.
Size distribution detects:
Embodiment 1 to embodiment 5 prepared silver powder is carried out size distribution to be detected; Detecting used instrument is the JL-1166 type laser particle analyzer that Jingxin Power Testing Apparatus Co., Ltd., Chengdu makes;, method places the water of tester sample room under ultrasonic dispersion, to test for getting 2 ~ 5 gram silver powder samples; Reach between 50 ~ 80 at the instrument display density, measure size distribution curve figure.Testing result is seen the particle size distribution figure of accompanying drawing 1 to accompanying drawing 5: Fig. 1 for the prepared silver powder of embodiment 1, i.e. blank test, as can be seen from the figure; The size distribution peak of the silver powder of this method preparation is short, mild; The distribution broad of silver powder granularity is described, granule size is inhomogeneous, in addition; The silver powder granularity has part only to reach micron order, does not reach the required submicron order of electrocondution slurry; Fig. 2 to Fig. 5 is respectively the particle size distribution figure of the prepared silver powder of embodiment 2 to embodiment 5; As can be seen from the figure, the size distribution peak of the silver powder that four embodiment are prepared point and high is explained the narrow particle size distribution of silver powder; Good uniformity, and the granularity of silver powder is all in the submicron order scope.
Claims (8)
1. preparation method who is used for the submicron order silver powder of electrocondution slurry; Be included in the silver salt solution and add dispersant and reducing agent restores silver-colored simple substance; It is characterized in that: before adding dispersant and reducing agent, in silver salt solution, add earlier nano silver particles; The particle diameter of said nano silver particles is 5 ~ 10nm, the addition of said nano silver particles be in the silver salt solution silver salt solute quality 0.3 ‰ ~ 6 ‰.
2. preparation method according to claim 1 is characterized in that: the Ag in the said silver salt solution
+Concentration is 5 * 10
-3Mol/L ~ 5 * 10
-1Mol/L, the reaction temperature of solution is 10 ~ 60 ℃.
3. preparation method according to claim 1 and 2; It is characterized in that: said dispersant is one or more the aqueous solution in dodecyl sodium sulfate, glycerine, propane diols and the cetomacrogol 1000 0; The mass ratio of the silver salt solute in said dispersant and the silver salt solution is 1:50 ~ 1:200, and the concentration of aqueous solution of said dispersant is 0.5g/L ~ 5g/L.
4. preparation method according to claim 1 and 2 is characterized in that: said reducing agent is the aqueous solution of ascorbic acid, sodium ascorbate, ferrous sulfate heptahydrate, glucose, formaldehyde or sodium hypophosphite, the Ag in said reducing agent and the silver salt solution
+Mol ratio be 1:1 ~ 2:1, the concentration of aqueous solution of said reducing agent is 100g/L ~ 500g/L.
5. preparation method according to claim 1 and 2 is characterized in that, said preparation method also comprises: after question response is complete, earlier gained solution is filtered, clean filtering resulting silver powder with deionized water and absolute ethyl alcohol respectively.
6. preparation method according to claim 1 and 2 is characterized in that, said nano silver particles adopts following method preparation: at Ag
+Concentration is 1 * 10
-4Mol/L ~ 1 * 10
-2Add dispersant in the silver salt solution of mol/L, keep system temperature, add reducing agent while stirring at 5 ~ 10 ℃; The mass ratio of the silver salt solute in the silver salt solution of the dispersant of said preparation nano silver particles and preparation nano silver particles is 0.5:1 ~ 2:1, and the concentration of aqueous solution of the dispersant of said preparation nano silver particles is 0.1g/L ~ 0.5g/L; Ag in the silver salt solution of the reducing agent of said preparation nano silver particles and preparation nano silver particles
+Mol ratio be 0.1:1 ~ 1:1.
7. preparation method according to claim 6 is characterized in that: the dispersant of said preparation nano silver particles is one or more in polyacrylic acid, Sodium Polyacrylate, gelatin and the gum arabic.
8. preparation method according to claim 6 is characterized in that: the reducing agent of said preparation nano silver particles is the aqueous solution of sodium borohydride, potassium borohydride or hydrazine hydrate, and the concentration of aqueous solution of the reducing agent of said preparation nano silver particles is 1g/L ~ 10g/L.
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| CN104384526A (en) * | 2014-12-11 | 2015-03-04 | 成都明日星辰科技有限公司 | Preparation method for submicron monodisperse silver-palladium composite powder |
| CN105345027A (en) * | 2015-11-30 | 2016-02-24 | 成都市天甫金属粉体有限责任公司 | Production method of high-dispersion submicron silver powder |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101834004A (en) * | 2010-05-28 | 2010-09-15 | 中国乐凯胶片集团公司 | Silver powder for conductive silver paste of solar battery electrode and preparation method thereof |
| CN102407342A (en) * | 2011-10-31 | 2012-04-11 | 山东大学 | Preparation method of nano silver powder with accurately controllable particle size |
-
2012
- 2012-08-09 CN CN201210281074.8A patent/CN102764897B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101834004A (en) * | 2010-05-28 | 2010-09-15 | 中国乐凯胶片集团公司 | Silver powder for conductive silver paste of solar battery electrode and preparation method thereof |
| CN102407342A (en) * | 2011-10-31 | 2012-04-11 | 山东大学 | Preparation method of nano silver powder with accurately controllable particle size |
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| CN102974837B (en) * | 2012-11-29 | 2016-01-06 | 江苏理工学院 | The preparation method of flaky nanometer silver powder |
| CN104384526A (en) * | 2014-12-11 | 2015-03-04 | 成都明日星辰科技有限公司 | Preparation method for submicron monodisperse silver-palladium composite powder |
| CN105345027A (en) * | 2015-11-30 | 2016-02-24 | 成都市天甫金属粉体有限责任公司 | Production method of high-dispersion submicron silver powder |
| CN105642916A (en) * | 2016-04-07 | 2016-06-08 | 江西农业大学 | Method for preparing feather-like gold micron material by using chemical method |
| CN111438369A (en) * | 2019-01-16 | 2020-07-24 | 北京氦舶科技有限责任公司 | Silver powder, preparation method thereof and laser etching silver paste |
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| CN111659901A (en) * | 2020-06-17 | 2020-09-15 | 中船重工黄冈贵金属有限公司 | Preparation method of submicron silver powder |
| CN112475311A (en) * | 2020-10-30 | 2021-03-12 | 山东建邦胶体材料有限公司 | Quasi-spherical silver powder with accurately controllable particle size and preparation method thereof |
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| CN113976907A (en) * | 2021-10-26 | 2022-01-28 | 西安交通大学 | High-concentration silver microspheres and synthesis method thereof |
| CN114619039A (en) * | 2022-03-15 | 2022-06-14 | 江苏连银新材料有限公司 | Spherical silver powder, preparation method thereof and conductive paste |
| CN115475952A (en) * | 2022-09-09 | 2022-12-16 | 淮阴师范学院 | Preparation method of silver nanobelt |
| CN115475952B (en) * | 2022-09-09 | 2024-01-26 | 淮阴师范学院 | Preparation method of silver nanoribbon |
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