CN102248177B - Laser-induced method for preparing spherical silver powder - Google Patents
Laser-induced method for preparing spherical silver powder Download PDFInfo
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- CN102248177B CN102248177B CN 201110214850 CN201110214850A CN102248177B CN 102248177 B CN102248177 B CN 102248177B CN 201110214850 CN201110214850 CN 201110214850 CN 201110214850 A CN201110214850 A CN 201110214850A CN 102248177 B CN102248177 B CN 102248177B
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Abstract
The invention discloses a laser-induced method for preparing spherical silver powder. The spherical silver powder is obtained from a water solution of silver nitrate by using an oxidation-reduction reaction; and at the initial phase of the reaction, a silver crystal nucleus is generated by the oxidation-reduction reaction and obtains energy for quick vibration and dispersion by using laser radiation, thereby the growth of the silver crystal nucleus is controlled and spherical silver powder particles are obtained. The morphology of the spherical silver powder is adjusted by adjusting the wavelength and the power of laser. The diameters of the spherical silver powder particles are increased by prolonging the reaction time and the time for irradiating the reactant by laser. According to the invention, the spherical silver powder is prepared by adopting a laser-induced method; in the oxidation-reduction reaction process, a proper reaction system is established and controlled by adopting the laser to irradiate the reactant; and the silver crystal nucleus is induced to generate the morphology transition, thereby the spherical silver powder is obtained. The prepared silver powder material has the characteristics of high degree of sphericity, favorable dispersion, uniformity in granularity, high tap density, excellent conducting performance, and the like and can meet the large-scale industrial requirement.
Description
Technical field
The present invention relates to chemical field, relate in particular to photochemistry, particularly preparation is as the method for the ball-type silver powder of electrocondution slurry, and concrete is a kind of induced with laser ball-type silver powder preparation method.
Background technology
Super fine silver powder has very stable physicochemical characteristics; Have very excellent performance aspect numerous in electricity, optics and catalysis etc., be widely used in electric slurry industry, medical and many fields such as anti-biotic material, electromagnetic shielding, ceramic material, environment-friendly materials and coating at present.The preparation method of super fine silver powder has a variety of, like chemical reduction method, electrochemical deposition method, electrolysis, sputtering method, vibratory milling method, sol-gal process etc.In the prior art, chemical reduction method is the method that the most general being used for prepares super fine silver powder.The key problem in technology of producing super fine silver powder is when producing in batches, to control its size, size distribution and pattern.And wherein the electrocondution slurry modulated of ball-type silver powder has to roll and starches not roll banding; Printing is prone to off-grid; Shrinkage factor is minimum, and characteristics such as sintered membrane densification are widely used in high-end electric slurry market; Be the splendid raw material of solar cell, PDP shielding silver paste and high conductivity thick film ink, also can be used for the powder metallurgy industry.Chemical method prepares the technology of ball-type silver powder; Like patent: CN1387968 " preparation method of superfine spherical silver powder ", CN101214555 " a kind of preparation method of spherical nano-silver powder ", but all there are deficiency in its technology and performance; Restrict its industrialization, also limited its application simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of induced with laser ball-type silver powder preparation method, there is technical problem not enough, that restrict its industrialization and application in the performance that described this induced with laser ball-type silver powder preparation method will solve the method for preparing ball-type silver powder in the prior art and ball-type silver powder.
This induced with laser ball-type silver powder preparation method of the present invention; Comprise a process of utilizing redox reaction from the aqueous solution of silver nitrate, to obtain ball-type silver powder, wherein, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder; Utilize laser radiation silver nucleus; Crystal face is activated, thereby the silver-colored nucleus growth in the control course of reaction obtains the ball-type silver powder particles.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, the Wavelength of Laser scope of irradiation reactant is between 100～600 nanometers.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder,, regulate the pattern of ball-type silver powder through regulating the Wavelength of Laser and the power of irradiation reactant.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder,, increase the diameter of ball-type silver powder particles through prolonging the time of reaction time and laser radiation reactant.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, adopt ascorbic acid, hydrazine hydrate, glucose or the sodium hypophosphite aqueous solution etc. as reducing agent.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, pH value of reactants is between 3 to 9, and reaction temperature is between 10 to 90 degree.
Further, the total impurities content in the aqueous solution of described silver nitrate is lower than 10 ppm.
Operation principle of the present invention is: in initial reaction stage, silver ion reduction is assembled the silver-colored nucleus of formation.After nucleus absorbs laser, fast vibration and dispersion, crystal face is activated, thereby controls silver-colored nucleus growth, obtains ball-type silver powder.Whole process can be divided into induces and two stages of growth response.If the Wavelength of Laser that silver-colored nucleus absorbs is different with power, then the degree that is activated of crystal face is different, causes silver-colored preferential growth to be orientated difference, finally can obtain the silver powder of different-shape.According to photoinduction mechanism, photon energy must could cause silver-colored nucleus activation above a certain critical value in the reaction reduction process, and promptly laser wavelength of incidence must being only effectively less than critical wavelength.Therefore, after the selected suitable reaction system, laser plays a decisive role to the orientation of growth of silver-colored nucleus.Through regulating Wavelength of Laser and power, can obtain highly purified ball-type silver powder, the size of particle be can control through adjusting the reaction time, thereby particle diameter and all controlled ball-type silver powder of pattern obtained.
The present invention and prior art are compared, and its effect is actively with tangible.The present invention adopts the induced with laser method to prepare ball-type silver powder; Be different from the free growing mechanism of galactic nucleus in the general redox reaction; In oxidation-reduction process, at first adopt the laser radiation reactant, set up and control suitable reaction system, induce initial stage silver nucleus activation; Thereby in subsequent reactions, cause the chain type explosive reaction, thereby obtain a large amount of ball-type silver powder as seed.Solved the deficiency that the performance of the method for preparing ball-type silver powder in the prior art and ball-type silver powder exists, the particle diameter of ball-type silver powder and pattern all can be controlled.The ball-type silver powder of the present invention preparation has technology with equipment is simple, production stable, be fit to the advantage of large-scale production, but also the raw material with energy-saving and environmental protection, employing are prone to acquisition, the one feeding amount is big, output is high, cost is low and process equipment does not have advantages such as specific (special) requirements.Technology belongs to international advanced, leading domestic.Characteristics such as the silver powder material of preparation has sphericity height, good dispersion, epigranular is controlled, tap density is high, electric conductivity is superior can satisfy the large-scale industry requirement.
Description of drawings
Fig. 1 is the process chart of induced with laser ball-type silver powder preparation method of the present invention.
Fig. 2 is the ball-type silver powder scanning electron microscope sem figure that the present invention prepares.
The specific embodiment
Embodiment 1
Induced with laser ball-type silver powder preparation method of the present invention; Comprise a process of utilizing redox reaction from the aqueous solution of silver nitrate, to obtain ball-type silver powder, wherein, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder; Utilize laser radiation silver nucleus; Crystal face is activated, thereby the silver-colored nucleus growth in the control course of reaction obtains the ball-type silver powder particles.
As depicted in figs. 1 and 2, in one embodiment of the invention, the 20g silver nitrate is dissolved in 0.5 liter of deionized water; Be mixed with oxidation liquid, the 20g sodium hypophosphite is dissolved in 1 liter of deionized water, be mixed with reducing solution; The reducing solution for preparing is poured in the reduction reactor, utilized magnetic stirring apparatus to stir, and to utilize wavelength be the laser radiation reactant of 532 nanometers; Simultaneously oxidation liquid is injected reducing solution with the speed of 500 milliliters of per minutes; Stir 20 minutes to the entire reaction completion, take out product then, through spending deionised water to washing electrical conductivity of water after the centrifuge centrifugation less than 50 u s/cm; Again gained silver powder product is placed in the vacuum drying chamber, under 40 ℃ of conditions, silver powder is dried to Powdered.
Concrete, in course of reaction, the aqueous solution that in reactant, adds ammonia is regulated pH value, and it specifically reacts formula and is:
NaH
2PO
2＋4AgNO
3＋6NH
3·H
2O=4Ag↓+(NH
4)
3PO
4+NaNO
3+3NH
4NO
3+4H
2O
The concentration of the aqueous solution of ammonia is 26%, and the adding volume is 100ml.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, the Wavelength of Laser scope of irradiation reactant is between 100～600 nanometers.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder,, regulate the pattern of ball-type silver powder through regulating the Wavelength of Laser and the power of irradiation reactant.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder,, increase the diameter of ball-type silver powder particles through prolonging the time of reaction time and laser radiation reactant.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, adopt ascorbic acid, hydrazine hydrate, glucose or the sodium hypophosphite aqueous solution etc. as reducing agent.
Further, in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder, pH value of reactants is between 3 to 9, and reaction temperature is between 10 to 90 degree.
Further, the total impurities content in the aqueous solution of described silver nitrate is lower than 10 ppm.
The operation principle of present embodiment is: in initial reaction stage, silver ion is assembled the silver-colored nucleus of formation.After nucleus absorbs laser, fast vibration and dispersion, crystal face is activated, thereby controls silver-colored nucleus growth, obtains ball-type silver powder.Whole process can be divided into induces and two stages of growth response.If the Wavelength of Laser that silver-colored nucleus absorbs is different with power, then the degree that is activated of crystal face is different, causes silver-colored preferential growth to be orientated difference, finally can obtain the silver powder of different-shape.According to photoinduction mechanism, photon energy must could cause silver-colored nucleus activation above a certain critical value in the reaction reduction process, and promptly laser wavelength of incidence must being only effectively less than critical wavelength.Therefore, after the selected suitable reaction system, laser plays a decisive role to the orientation of growth of silver-colored nucleus.Through regulating Wavelength of Laser and power, can obtain highly purified ball-type silver powder, the size of particle be can control through adjusting the reaction time, thereby particle diameter and all controlled ball-type silver powder of pattern obtained.
Claims (3)
1. an induced with laser ball-type silver powder preparation method comprises a process of utilizing redox reaction from the aqueous solution of silver nitrate, to obtain ball-type silver powder, it is characterized in that: in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder; Utilize laser radiation silver nucleus; The crystal face of activation silver nucleus, thus the silver-colored nucleus growth in the control course of reaction obtains the ball-type silver powder particles; The Wavelength of Laser scope is between 100～600 nanometers; Through regulating the Wavelength of Laser and the power of the silver-colored nucleus of irradiation, regulate the pattern of ball-type silver powder particles, through prolonging the time of reaction time and laser radiation reactant; Increase the diameter of ball-type silver powder particles, adopt ascorbic acid, hydrazine hydrate, glucose or the sodium hypophosphite aqueous solution as reducing agent.
2. induced with laser ball-type silver powder preparation method as claimed in claim 1; It is characterized in that: in the described redox reaction process that from the aqueous solution of silver nitrate, obtains ball-type silver powder; PH value of reactants is between 3 to 9, and reaction temperature is between 10 to 90 degree.
3. induced with laser ball-type silver powder preparation method as claimed in claim 1, it is characterized in that: the impurity content in the aqueous solution of described silver nitrate is lower than 10 ppm.
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| CN104525964B (en) * | 2014-12-21 | 2017-02-22 | 北京工业大学 | Preparing method for regular spherical silver nanometer particles |
| CN105436517B (en) * | 2015-12-24 | 2017-05-17 | 苏州思美特表面材料科技有限公司 | Method for preparing metal powder by utilizing nano crystal seed induction |
| CN105642913B (en) * | 2016-03-25 | 2017-09-22 | 北京理工大学 | A kind of method that laser-induced material reproducibility prepares polymorphic gold nano structure |
| CN106563812B (en) * | 2016-10-26 | 2018-04-24 | 东南大学 | A kind of method of light triggering synthesizing superfine nano silver wire in aqueous solution |
| JP7001061B2 (en) * | 2016-11-02 | 2022-01-19 | コニカミノルタ株式会社 | Manufacturing method of additive manufacturing |
| CN106908434A (en) * | 2017-03-20 | 2017-06-30 | 上海镭立激光科技有限公司 | Using the device of ultraviolet Raman spectrometer real-time control spherical silver powder preparation process |
| CN107976384B (en) * | 2017-10-20 | 2019-07-09 | 浙江大学 | One-wavelength laser induces incandescence nano-scale carbon soot calipers and method |
| CN113118453B (en) * | 2019-12-30 | 2022-11-29 | Tcl科技集团股份有限公司 | Silver nano particle, preparation method thereof and photoinduction device |
| CN113640270A (en) * | 2021-06-17 | 2021-11-12 | 北京工业大学 | Method for preparing superlattice SERS substrate based on laser tuning plasma resonance |
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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 |
| CN1857833A (en) * | 2006-05-30 | 2006-11-08 | 华东理工大学 | Preparing process of silver powder for printing slurry of electrode in solar cell |
| CN101497135B (en) * | 2009-03-12 | 2010-09-22 | 宁波大学 | Method for preparing spherical silver nano granule |
| CN101716685B (en) * | 2009-12-14 | 2011-08-24 | 昆明理工大学 | Method for preparing spherical superfine silver powder by using chemical reduction method |
| CN102069193B (en) * | 2011-01-17 | 2012-07-04 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
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Effective date of registration: 20130409 Address after: 215000 Suzhou Industrial Park, Jiangsu, China Road, No. 1, No. Patentee after: Suzhou Inreal Optoelectronic Material Technology Co., Ltd. Address before: 201203 Edison road Shanghai, Pudong New Area Zhangjiang hi tech Park No. 328 1 floor Patentee before: Shanghai Longxiang New Material Technology Co.,Ltd. |