CN1235706C - Industrialized preparation technology of nm-class silver powder - Google Patents
Industrialized preparation technology of nm-class silver powder Download PDFInfo
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- CN1235706C CN1235706C CN 200410009079 CN200410009079A CN1235706C CN 1235706 C CN1235706 C CN 1235706C CN 200410009079 CN200410009079 CN 200410009079 CN 200410009079 A CN200410009079 A CN 200410009079A CN 1235706 C CN1235706 C CN 1235706C
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Abstract
The present invention provides an industrialized preparation technology of a nanosized silver powder, in which a microwave activation and aqueous solution reduction process is adopted. Firstly, salt AgNo3 containing silver ions is dissolved in water, the characteristic that N2H4. H2O hydrazine can provide electrons in an aqueous solution is utilized to accelerate reaction speed under the activation condition of a microwave field; trace polyvinyl alcohol dusting agent is added to a reaction solution in order to prevent silver particles from growing and being aggregated in the time of precipitation, so that Ag<+2>ions are rapidly reduced to very fine Ag particles; NO3 <2-> radical ions in reagents are cleaned out by distilled water, alcohol is used to remove residual water, and simultaneously, a particle dispersing agent is added; a highly active and continuous rapid centrifugal separation method is adopted to separate a silver powder from waste liquid; finally, the silver powder is dried at a low temperature in a vacuum dryer to obtain the silver powder with the average particle size of at most 50 nm. The present invention has the advantages of rapid reduction reaction and high efficiency of centrifugation, and is suitable for the mass commercial process of nanosized ultra-fine silver powders.
Description
Technical field
The invention belongs to metal dust preparing technical field in the metal material, a kind of industrialized process for preparing of nano-scale silver powder particularly is provided, be applicable to the suitability for industrialized production of nano-scale silver powder.
Background technology
Nano-scale silver powder is widely used in the electron trade, and the particularly develop rapidly of microelectric technique in the information industry in recent years is to the demand of nanometer-level silver paste paint, rapid growth.About 1000 tons of U.S.'s year requirement, about 2500 tons of Japan and Europe year requirement.300 tons of China's year requirements, about 200 tons of Taiwan.World demand amount every year is with 20～28% speed increment.In addition, nano-scale silver powder is used also very extensive at tungsten-Yin superhigh temperature transpiration material in electrical contact material, silver-cubond material and the computer CPU heat sink materials such as silver-cadmium oxide, silver-tungsten carbide, silver-chromium, silver-copper.In medical dental alloy, also begin applying nano level silver-bearing copper tin alloy powder in recent years.Simultaneously in chemical fibre, tableware washes on the ware utensil, begin to adopt bactericidal nano-silver coating, so the technology of preparing of nano-silver powder has great importance.
The literature search in nearly ten years as can be known, the production method of silver powder mainly contains physics method and chemical method two big classes.Mainly contain in the physics method: evaporation-condensation method, mechanical milling method, atomization, (contain high pressure gas atomizing, hydraulic atomized, ultrasonic atomizatio, rotating disc centrifugal atomizing, electric power atomizing, plasma atomizing etc.), mechanical milling method can only be produced sheet or the plate-like silver powder of particle diameter＞20 μ m.The evaporation-condensation method can be produced the ball shape silver powder that particle diameter is 0.3～5 μ m.But this method yields poorly, the equipment cost height.Atomization generally can only production average grain diameter＞30 μ m silver powder.Have only the plasma atomization could produce the silver powder of particle diameter during greater than 200KW for (0.3～5 μ m) at power.The characteristics of physics method are that output is big, powder size is thick, equipment investment is big, cost is high, the powder recovery rate is low in a word.Mainly contain chemical vapour deposition technique and solution reduction method in chemical method, these methods all can be produced nano-scale silver powder.But the former cost height, efficient are low, and latter's advantage is more.The solution reduction method is present method with fastest developing speed, this method, not only can produce powder diameter for (10～200nm) nano level superfine silver powder, and can thicker (0.5～3 μ m) the micron order silver powder of production granularity, its production cost and equipment investment all are lower than the former.The research of chemical method focuses mostly in the reduction reaction characteristic aspect of the aqueous solution over past ten years, as solution concentration, reaction speed, pH value, reaction temperature, reducing agent add speed, whipped form, etc. with the relation of precipitation rate, growth process, silver powder particles shape, silver powder granularity and the specific surface of silver powder particles etc.In above-mentioned research process, a lot of patents of invention have been obtained.But at present in the technology of aqueous solution reduction preparation of silver powder, also exist a still unsolved difficult problem, it is long that the time is separated out in first reaction, be generally 1～2 hour, sometimes reach 4 hours, it two is after silver ion is reduced into silver-colored particle, assembles fast and grows up into micron particles, and this is very unfavorable for the preparation nano-scale silver powder.Its three are mother liquors with silver particles separate and cleaning and filtering is very difficult repeatedly.The thing followed be cause that the liquid handling amount is excessive, production efficiency is very low, real silver powder amount seldom, casting yield is low.When the preparation nano-scale silver powder, in order to control growing up of silver-colored particle, often adopt the silver ion solution of low molar concentration, this will further cause the treating capacity of mother liquor bigger, casting yield further reduces, production efficiency obviously descends, therefore be equipped with the technology of nano-silver powder with the solution reduction legal system, suitability for industrialized production all can not be dropped on a large scale in countries in the world at present.
Summary of the invention
Know-why of the present invention still belongs to the aqueous solution reducing process of silver ion, adopts the reduction reaction ion of microwave field in can activated water solution, quickens reduction reaction speed, reduces the characteristics of reaction temperature.Two electronics that the very fast acquisition of silver ion of divalence is provided by hydrazine, reduction becomes the silver atoms Ag of zeroth order.
The object of the present invention is to provide a kind of industrialized process for preparing of nano-scale silver powder, shorten the reaction time of solution reduction significantly; Employing prevents that with the method for interleaving agent silver-colored particle aggregation from growing up; Solved the problem that mother liquor separation and slip clean separation difficulty.
The present invention adopts microwave activation-aqueous solution reducing process to prepare average grain diameter≤50nm nano-scale silver powder technology.Its technology is: the salt AgNO that will contain silver ion earlier
3Water-soluble, use N
2H
4H
2The O hydrazine can provide the characteristics of electronics in the aqueous solution under the microwave field activation, apace with Ag
+ 2Ion is reduced into superfine silver-colored particle.Grow up in order to prevent that silver particles from assembling when separating out, at AgNO
3In the aqueous solution, add cheap interleaving agent PVA (polyvinyl alcohol).NO in the product
3 2-Acid ion is distilled water and cleans out.And deviate from residual water with alcohol, and adopt the method for the quick centrifugation of continous way that the waste liquid in the mother liquor is separated with sediment with cleaning fluid, low temperature drying can obtain nano level superfine silver powder in vacuum drying box at last.
The concrete processing step of preparation of the present invention is:
1, preparation AgNO
3The aqueous solution:
With solid AgNO
3Silver nitrate is pressed AgNO
3: H
2O=85: 1000 (quality) ratio joins in the distilled water, is heated to 60～80 ℃, and it is fully dissolved, and is prepared into AgNO
3The aqueous solution is standby;
2, preparation polyvinyl alcohol interleaving agent solution:
By (PVA) polyvinyl alcohol: HO
2=2: 100 (quality) ratio joins PVA in the distilled water, adds thermal agitation at 90-100 ℃, until dissolving fully, is prepared into PVA (interleaving agent) solution.
3, preparation (binary liquid mixture of silver nitrate-PVA):
At above-mentioned AgNO
3In the aqueous solution, press PVA (polyvinyl alcohol) solution: AgNO
3Solution=1: 2 (mass ratio) adds (PVA) polyvinyl alcohol water solution, is heated to 55～65 ℃ of stirrings, is prepared into (the binary liquid mixture of silver nitrate-PVA).
4, preparation silver nitrate-hydrazine-PVA ternary mixed solution:
Press N
2H
4H
2O (hydrazine): AgNO
3(silver nitrate)=1: 1.7 mass ratio is with N
2H
4H
2O solution slowly pour into (in the binary liquid mixture of silver nitrate-PVA), carry out brute force simultaneously and stir, be prepared into silver nitrate-hydrazine-PVA ternary mixed solution.
5, microwave activation-aqueous solution reduction:
The ternary mixed solution is sent into activation-reduction in the microwave field of 2450MHZ frequency, heating using microwave 1～2 minute, solution begins heat release, a large amount of foams occur, occurs a large amount of silver bright color Nano Silver powder particles simultaneously, and reduction reaction was finished rapidly in 1～2 minute.
6, high speed centrifugation separates nano-silver powder:
When need precipitating with the no AgCl of HCl check, can discard in mother liquor.With Sharples centrifuge mother liquor is separated with silver powder, will contain small portion of residual NO
3 2-The nano-silver powder slip of root or powder agglomates take out and change cleaning over to.
7, stirring and washing sediment repeatedly:
With distilled water stirring and washing silver powder slip or powder agglomates repeatedly, with NO
4 2-Radical ion washes, and does not have NO in sediment
3 2-Till the radical ion; Sharples centrifuge can inject muddy liquid continuously under non-stop-machine situation.Silver-colored particle separates automatically with waste liquid in centrifuge, and waste liquid can automatically be discharged, so just can be with nano-Ag particles and a large amount of waste liquid centrifugations, thus can finish the work of cleaning repeatedly efficiently.
8, dehydration adds dispersant:
To not contain NO
3 2-The nano-silver powder slip or the powder agglomates of nitrate ion, by quality than silver powder: alcohol=add alcohol at 1: 5, utilize the dehydration of alcohol further the residual water in the silver powder to be removed.Meanwhile add particle dispersants (SD), addition is 0.1 ‰ of an alcohol (quality), and stirs 25～35 minutes, through centrifugation, reclaim and remove alcohol.
9, vacuum drying, reclaim residual alcohol:
With the silver powder slip that removes behind the alcohol, 30Pa, by 45～65 minutes/Kg oven dry, further reclaims residual alcohol by 65～80 ℃ in a vacuum.Cool off the back discharging, can obtain the superfine nano silver powder of average grain diameter≤50nm.，
10, Performance Detection:
Can detect nanoscale Ag mealiness, mainly carry out XRD, SEM, tem analysis and BET specific surface and measure.
11, carry out vacuum packaging.
The invention has the advantages that:
(1), provides the new technology of a kind of average grain diameter of the large-scale production of serialization apace nano level superfine from production technology less than the argent powder of 50nm.
(2), device therefor is simple, operation is short, realize that easily serialization controls automatically, has improved the automatization level that China's silver powder is produced greatly.
(3), microwave activation reduction and continuous high-speed centrifugation technique saved the reduction and the sedimentation time of nano-silver powder widely, enhances productivity about 200～250 times
(4), the nano level superfine argent powder produced is spherical in shape,
Description of drawings
Fig. 1 is preparation technology's flow chart of the present invention.Wherein 1 is by AgNO
3: H
2O=85: 1000 (quality) ratio prepares AgNO
3The aqueous solution is with AgNO
3Join powerful stirring the in the distilled water.And heat 60-80 ℃; Be prepared into AgNO
3The aqueous solution is standby.The 2nd, by (PVA): HO
2=2: 100 (quality) ratio joins PVA in the distilled water, adds thermal agitation at 90-100 ℃, is prepared into the PVA interleaving agent solution of 2% (quality) concentration.The 3rd, be prepared into that (binary liquid mixture of silver nitrate-PVA) is pressed PVA interleaving agent solution: AgNO
3Solution=1: 2 (mass ratio) joins AgNO with PVA solution
3In the solution, be prepared into (the binary liquid mixture of silver nitrate-PVA).The 4th, preparation silver nitrate-hydrazine-PVA ternary mixed solution is pressed N
2H
4H
2O: AgNO
3=1: 1.7 mass ratios are with N
2H
4H
2O solution slowly pour into (in the binary liquid mixture of silver nitrate-PVA), carry out brute force simultaneously and stir, be prepared into silver nitrate-hydrazine-PVA ternary mixed solution.The 5th, activation-reduction in the microwave field of 2450MHZ frequency is sent into the ternary mixed solution in the reduction of the microwave activation-aqueous solution, heating using microwave 1～2 minute, and a large amount of silvery white Nano Silver powder particle of appearance in the solution, reduction reaction is finished.The 6th, with Sharples centrifuge silvery white silver powder is separated with mother liquor.The 7th, with distilled water stirring and washing, centrifugation repeatedly, with residual nitric acid root NO
3 2-Ion washes.The 8th, dehydration of alcohol adds particle dispersants (SD), and with silver powder and the quick centrifugation of alcohol.The 9th, vacuum drying further obtains the nano level metal silver powder after recovered alcohol, the oven dry.The 10th, the nano-silver powder Performance Detection is mainly carried out XRD, SEM, tem analysis and BET specific surface and is measured.The 11st, carry out vacuum packaging.
The specific embodiment
Embodiment 1: during preparation 1kg nanometer Ag powder, should follow these steps to finish.
1, takes by weighing 1.57kg AgNO
3Powder is pressed AgNO
3: H
2O=85: 1000 mass ratios join in the 18.53Kg distilled water, are heated to 80 ℃, and it is fully dissolved, and are prepared into 20.1Kg AgNO
3The aqueous solution;
2, press PVA: H
2O=2: 100 (mass ratioes), 0.197Kg PVA is joined in the 9.85Kg distilled water, until dissolving fully, promptly be prepared into 10.05Kg PVA interleaving agent solution for standby in 100 ℃ of heating, stirring.
3, the preparation (binary liquid mixture of silver nitrate-PVA).
At above-mentioned 20.1Kg AgNO
3In the aqueous solution, press PVA solution: AgNO
3Solution=1: 2 (mass ratio) adds the PVA aqueous solution of 10.05Kg, is prepared into the 30.15Kg (binary liquid mixture of silver nitrate-PVA).
4, preparation silver nitrate-hydrazine-PVA ternary mixed solution
Press N
2H
4H
2O: AgNO
3=1: 1.7 mass ratios are with 0.93Kg N
2H
4H
2O solution slowly pour into 30.15Kg (in the binary liquid mixture of silver nitrate-PVA), carry out brute force simultaneously and stir, be prepared into 31.08Kg silver nitrate-hydrazine-PVA ternary mixed solution.
5, microwave activation-aqueous solution reduction
The ternary mixed solution is distributed into canister (1.5Kg/ jar) sends into activation-reduction in the microwave field of 2450MHZ frequency, heating using microwave 2 minutes, solution begins heat release, a large amount of foams occur, occur a large amount of silvery white Nano Silver powder particles simultaneously, reduction reaction was finished rapidly in 2 minutes.
6, high speed centrifugation separates nano-silver powder
With Sharples centrifuge silvery white silver powder is separated with mother liquor; , mother liquor needs the check with HCl, and no AgCl can discard when precipitating, and will contain small amount of N O
3 2-Nano-silver powder slip or powder agglomates take out and change over to cleaning
7, stirring and washing sediment repeatedly
With distilled water stirring and washing silver powder slip or powder agglomates repeatedly, with NO
3 2-Ion washes, and does not have NO in sediment
3 2-Till the radical ion; In cleaning process repeatedly with Sharples centrifuge with nano-Ag particles and a large amount of cleaning fluid centrifugations, cleaning fluid is discharged fast.
8, dehydration of alcohol adds activator
To not contain NO
3 2-The nano-silver powder slip or the powder agglomates of ion, press silver powder: alcohol=1: 5 (mass ratio) adds alcohol 5kg, utilizes the dehydration of alcohol further the residual water in the silver powder to be removed.Meanwhile adding particle dispersants SD (by 0.1 ‰ adding of adding alcohol quality) is 0.5g, and stirs 35 minutes, through centrifugation, reclaim and remove alcohol.
9, vacuum drying, recovered alcohol
With the silver powder slip that removes behind the alcohol, in vacuum drying box 30Pa, 65 ℃, by 65 minutes/Kg oven dry, further recovered alcohol, cooling back discharging promptly obtains the nano-level sphere silver powder of 1kg average grain diameter≤50nm.
10, Performance Detection
To nanoscale Ag silver powder Performance Detection, mainly carry out XRD, SEM, tem analysis and BET specific surface and measure
11, vacuum packaging
Embodiment 2: during preparation 500g nanometer Ag powder, should follow these steps to finish
1, takes by weighing 0.785kg AgNO
3Powder is with AgNO
3Press AgNO
3: H
2O=85: 1000 mass ratios join in the 9.265Kg distilled water, are heated to 60 ℃, and powerful the stirring is prepared into 10.05Kg AgNO
3The aqueous solution;
2, preparation PVA solution is pressed PVA: H
2O=2: 100 (mass ratioes) take by weighing 0.099Kg PVA powder and 4.925Kg distilled water, until dissolving fully, promptly are prepared into 5.024Kg PVA interleaving agent solution for standby in 90 ℃ of heating, stirring.
3, the preparation (binary liquid mixture of silver nitrate-PVA)
Above-mentioned 1,2 two kind of solution are amounted to 15.074Kg and is mixed and made into binary liquid mixture, and (3) are identical among concrete operations and the embodiment 1.
4, preparation silver nitrate-hydrazine-PVA ternary mixed solution
Basic identical with (4) among the embodiment 1.Do not exist together is with 0.465kg N
2H
4H
2That O solution is slowly poured into is above-mentioned (in the binary liquid mixture of silver nitrate-PVA).
5, microwave activation-aqueous solution reduction
Basic identical with (5) among the embodiment 1.Just heating using microwave is 1 minute,
6,7,8 and embodiment 1 in 6,7,8 technologies basic identical.The mixing time that just adds alcohol and particle dispersants SD in 8 is 25 minutes.
9, vacuum drying, recovered alcohol
With the silver powder slip that removes behind the alcohol, in vacuum drying box 30Pa, 80 ℃, by 45 minutes/Kg oven dry, further recovered alcohol, cooling back discharging can obtain the nano-level sphere silver powder of 0.5kg average grain diameter≤50nm.
10,11 with embodiment 1 in 10,11, identical, Performance Detection, vacuum packaging.
Claims (1)
1, a kind of industrialized process for preparing of nano-scale silver powder, concrete processing step is:
A. prepare four kinds of aqueous solution:
Preparation AgNO
3The aqueous solution: with solid AgNO
3Silver nitrate is pressed AgNO
3: H
2O=85: 1000 mass ratios join in the distilled water, are heated to 60～80 ℃, the powerful stirring, and fully dissolving is prepared into AgNO
3The aqueous solution;
Preparation polyvinyl alcohol interleaving agent solution: press polyvinyl alcohol: H
2O=2: 100 mass ratioes, pva powder is joined in the distilled water, be stirred and heated to 90-100 ℃, promptly be prepared into polyvinyl alcohol interleaving agent solution;
Preparation silver nitrate-polyvinyl alcohol binary liquid mixture: at above-mentioned AgNO
3In the aqueous solution, press poly-vinyl alcohol solution: AgNO
3Solution=mass ratio mixed two kinds of solution in 1: 2, was prepared into silver nitrate-polyvinyl alcohol binary liquid mixture;
Preparation silver nitrate-hydrazine-polyvinyl alcohol ternary mixed solution: press N
2H
4H
2O: AgNO
3=1: 1.7 mass ratios are with N
2H
4H
2O solution slowly pours in silver nitrate-polyvinyl alcohol binary liquid mixture, carry out being prepared into silver nitrate-hydrazine-polyvinyl alcohol ternary mixed solution after brute force stirs;
B. microwave activation-aqueous solution reduction:
The ternary mixed solution is sent to carries out microwave activation-aqueous solution reduction in the microwave field of 2450MHZ frequency, heating using microwave 1～2 minute, a large amount of Nano Silver powder particles are separated out in solution and foam, and reduction reaction was finished in 1～2 minute;
C. high speed centrifugation separates nano-silver powder:
Mother liquor and silver powder sediment are isolated and excluded waste liquid fast with Sharples centrifuge, mother liquor and cleaning fluid are constantly discharged rapid subsidence nano particle, eliminating waste liquid under the effect of high speed centrifugation power;
D, stirring and washing sediment repeatedly:
Use the nitrate anion NO in the distilled water stirring and washing sediment repeatedly
3 2-Ion, and continuous quick centrifugal eliminating cleaning fluid do not have NO in cleaning fluid
3 2-Behind the root, stop washing;
E. dehydration of alcohol adds dispersant:
Slip or powder agglomates and industrial alcohol with the d processing, by quality than silver powder: industrial alcohol=1: 5 adds industrial alcohol, utilize the dehydration of alcohol further the residual water in the nano-silver powder to be removed, meanwhile for preventing that the nano-silver powder particle agglomeration from adding micro-particle dispersants SD, addition is by 0.1 ‰ addings that add alcohol quality, above-mentioned slip stirred after 25～35 minutes, separates with Sharples centrifuge alcohol is separated and recovery;
F. vacuum drying, recovered alcohol
Using vacuum drying box, is 30Pa in vacuum, 65～80 ℃, by 45～65 minutes/Kg oven dry, and further reclaim residual alcohol, and cool off the back discharging, promptly obtain the superfine nano silver powder of grain shape almost spherical, average grain diameter≤50nm;
G. nanoscale Ag powder should carry out XRD, SEM, tem analysis and BET project mensuration, and carries out vacuum packaging.
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Cited By (2)
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| CN102179528A (en) * | 2011-04-14 | 2011-09-14 | 北京科技大学 | Preparation method of deposited, ventilated and reduced nanometer-level silver powder |
| CN102120265B (en) * | 2010-01-07 | 2013-04-10 | 中国科学院化学研究所 | Preparation method of colloid of mono-dispersed silver nano particles and nano silver powder and conductive ink thereof |
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| JP4284283B2 (en) * | 2005-02-02 | 2009-06-24 | Ｄｏｗａエレクトロニクス株式会社 | Silver particle powder manufacturing method |
| CN101200553B (en) * | 2006-12-14 | 2011-02-16 | 中国科学院理化技术研究所 | Silver particles/polyvinyl alcohol composite film as well as preparation method and uses thereof |
| CN101249566B (en) * | 2008-03-31 | 2010-06-02 | 中国科学院物理研究所 | Preparation method of monodisperse silver nano |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN103480858B (en) * | 2013-09-10 | 2015-05-06 | 徐志兵 | Silver nano particle preparation method using visible light to reduce silver ions |
| CN108480647B (en) * | 2018-01-23 | 2022-01-18 | 珠海纳金科技有限公司 | Recycling method of nano-silver particle waste liquid |
| CN111348793B (en) * | 2018-12-24 | 2022-01-07 | 荆门市格林美新材料有限公司 | Treatment method of hydrazine hydrate liquid-phase reduction silver powder waste liquid |
| CN110449598A (en) * | 2019-09-06 | 2019-11-15 | 辽宁星空新能源发展有限公司 | A kind of method that rapid precipitation prepares two-dimensional metallic silver simple substance nanometer sheet |
| CN113695583A (en) * | 2021-08-09 | 2021-11-26 | 浙江海虹控股集团有限公司 | Method and system for continuously preparing superfine silver powder under assistance of microwaves |
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2004
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120265B (en) * | 2010-01-07 | 2013-04-10 | 中国科学院化学研究所 | Preparation method of colloid of mono-dispersed silver nano particles and nano silver powder and conductive ink thereof |
| CN102179528A (en) * | 2011-04-14 | 2011-09-14 | 北京科技大学 | Preparation method of deposited, ventilated and reduced nanometer-level silver powder |
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| CN1569369A (en) | 2005-01-26 |
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Assignee: Guangzhou Ruxing Technology Development Co., Ltd. Assignor: University of Science and Technology Beijing Contract fulfillment period: 2006.6.1 to 2011.5.31 contract change Contract record no.: 2008320000114 Denomination of invention: Industrialized preparation technology of nm-class silver powder Granted publication date: 20060111 License type: Exclusive license Record date: 2008.8.28 |
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