CN101279370A - Method for obtaining monodispersed superfine silver powder from soft-agglomerated silver powder - Google Patents
Method for obtaining monodispersed superfine silver powder from soft-agglomerated silver powder Download PDFInfo
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- CN101279370A CN101279370A CNA2008100978057A CN200810097805A CN101279370A CN 101279370 A CN101279370 A CN 101279370A CN A2008100978057 A CNA2008100978057 A CN A2008100978057A CN 200810097805 A CN200810097805 A CN 200810097805A CN 101279370 A CN101279370 A CN 101279370A
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Abstract
A method for obtaining monodisperse ultra-fine silver powder from soft agglomerated silver powder relates to a preparation method of nano and sub-micron silver powder, which is especially applicable to the method for obtaining the monodisperse ultra-fine silver powder from the silver powder which is newly prepared and is in a soft agglomerated state. The method is characterized in that the soft agglomerated silver powder is washed and carried out the immersion pulping by adding water or the ultrasonic dispersion pulping, the vacuum drying is carried out after the materials are frozen, thus leading ice in the materials to be sublimated and further obtaining the monodisperse ultra-fine silver powder. The prepared silver powder is washed and then is carried out the immersion pulping by adding water or the ultrasonic dispersion pulping, the freezing and drying is further carried out under certain conditions, thus obtaining the nano and sub-micron ultra-fine silver powder with good dispersion, stable shape and controllable particle size. The method has short process flow, simple treatment process, good solid-liquid separation effect, high direct recovery ratio and stable process conditions, which is applicable to the industrial mass production of the monodisperse nano and sub-micron silver powder.
Description
Technical field
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder relates to the preparation method of a kind of nanometer and submicron silver powder, is specially adapted to obtain from the silver powder of freshly prepd soft-agglomerated state the method for monodisperse superfine silver powder.
Background technology
Super fine silver powder is owing to having favorable conductive characteristic and catalysis, processing characteristics, so have purposes widely in fields such as electronic information, electrician, catalysis.At present, the preparation method of super fine silver powder mainly contains physics method and chemical method.The physics method mainly contains gas evaporation coacervation, polishing and atomization etc.Prepared by physical method silver powder exists that equipment investment is big, energy consumption is high, productive rate is low and shortcoming such as cost height.Chemical reduction method is exactly with reducing agent the complex ion of silver ion or silver to be restored from the aqueous solution or organic system solution, forms the powder particle of silver.Chemical reduction method is the most general preparation method of present super fine silver powder, and industrial used super fine silver powder adopts this method preparation mostly.
But,,, will inevitably relate to the Separation of Solid and Liquid problem of powder adopting chemical reduction method to prepare in the process of super fine silver powder because super fine silver powder has characteristics such as particle diameter is little, polymolecularity.Especially for the superfine powder of＜1 μ m, adopt filter type can't realize substantially damming fully; Adopt centrifugal separation method, for the dispersion that contains high molecular surfactant, under the slow-speed of revolution (general＜as 3000rpm) can't to realize that Separation of Solid and Liquid is incomplete completely to superfine powder, cause direct yield low.And under high rotating speed, bigger centrifugal force can make the silver powder caking, destroys the pattern of silver powder, causes silver powder to collect and the secondary difficulties in dispersion, can't obtain the super fine silver powder of polymolecularity.And can't obtain the pressed powder of favorable dispersibility for high dispersive ground nanometer or super fine silver powder slurries.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides that a kind of technological process is simple, good effect of separating solid from liquid, productive rate height, function admirable, stable process conditions, is easy to suitability for industrialized production is obtained monodisperse superfine silver powder from soft-agglomerated silver powder method.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder, it is characterized in that with soft-agglomerated silver powder through washing, add water and soak pulp or ultrasonic dispersion pulp after, carry out freeze drying and make ice distillation in the material, obtain monodispersed super fine silver powder.
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder of the present invention is characterized in that adopting deionized water washing, adds water and soak pulp or ultrasonic dispersion pulp, and the solid content after the pulp in the pulp liquid is 50%-80%.
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder of the present invention is characterized in that describedly adding water to soak the pulp time being 60-120min.
A kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder of the present invention, the power that it is characterized in that described ultrasonic dispersion pulp is 360-600W, the time of ultrasonic dispersion is 5-10min.
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder of the present invention is characterized in that described refrigerating process temperature is freezing 3h-5h under-30～-50 ℃ of temperature; Vacuum drying make ice distillation in the material be under-10～40 ℃ of temperature, carry out vacuum drying ice in the material is sublimed up into contain with silver powder wet weight be under 110 ℃ of temperature＜0.1%.
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder of the present invention is characterized in that described soft-agglomerated silver powder is is raw material with the silver nitrate, in the dispersion of PVP, under alkali condition with the silver powder of glucose with silver ion reduction.
A kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder of the present invention is characterized in that described soft-agglomerated silver powder is is raw material with the silver nitrate, in the dispersion of PVA, under alkali condition with the silver powder of formaldehyde with silver ion reduction.
Method of the present invention can realize super fine silver powder Separation of Solid and Liquid and high direct yield efficiently, and processing procedure is simple.Carry out freeze drying again after adopting complete pulp, make nanometer or super fine silver powder under monodisperse status, realize the drying of original position, dry back powder shatter value and dispersed very good, the while can not destroyed original pattern of silver powder.Finally make good dispersion, pattern is good, particle diameter is controlled nanometer or submicron silver powder by " soft-agglomerated-pulp-freeze drying ", drying process is simple, is easy to realize the industrialization operation.
The specific embodiment
A kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder, it is characterized in that its process be with soft-agglomerated particle through the washing, soak pulp after, freezing 3h-5h under-30～-50 ℃ of temperature, under-10～40 ℃ of temperature, carry out vacuum drying again the ice in the material is distilled, obtain monodispersed super fine silver powder.
Embodiment 1
With the silver nitrate is raw material, in the dispersion of PVP, is silver powder with glucose with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 40～70nm.Soft-agglomerated particle natural subsidence speed is fast, effect of settling good.Soft-agglomerated particle being spent deionised water 4 times, add a spot of water then, is 50% admittedly contain weight, after immersion pulp 60min treats complete pulp, carries out freeze-drying in freeze drier.The pre-freeze temperature is-30 ℃, and the pre-freeze time is 5h, after pre-freeze is finished, carries out vacuum drying under-10～40 ℃ of temperature the ice in the material is distilled, and drying is as the criterion (110 ℃) with silver powder water capacity＜0.1%, obtains monodispersed super fine silver powder.
Embodiment 2
With the silver nitrate is raw material, in the dispersion of PVP, is silver powder with glucose with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 40～70nm.Soft-agglomerated particle natural subsidence speed is fast, effect of settling good.Soft-agglomerated particle is spent deionised water 4 times, adds a spot of water then, ultrasonic dispersion treatment 5min under the ultrasonic field of 600W, treat complete pulp after, in freeze drier, carry out freeze-drying.Cryogenic temperature is-50 ℃, and the time is 3h, carries out vacuum drying again and make ice lyophilization in the material with silver powder water capacity＜0.1% be as the criterion (110 ℃) under-10～40 ℃ of temperature.Obtain monodispersed super fine silver powder
Embodiment 3
With the silver nitrate is raw material, in the dispersion of PVA, is silver powder with formaldehyde with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 0.3～1.0 μ m.Soft-agglomerated particle natural subsidence speed is fast, effective.Soft-agglomerated particle is spent deionised water 4 times, add a spot of water then, ultrasonic dispersion treatment 10min under the ultrasonic field of 360W.After treating complete pulp, be 50%-80%, in freeze drier, carry out freeze-drying admittedly contain weight.The pre-freeze temperature is-50 ℃, and the pre-freeze time is 3h, after pre-freeze is finished, carries out vacuum drying and make ice distillation in the material under-10～40 ℃ of temperature, and is dry with silver powder water capacity＜0.1% be as the criterion (110 ℃).Obtain monodispersed super fine silver powder.
Embodiment 4
With the silver nitrate is raw material, in the dispersion of PVP, is silver powder with glucose with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 40～70nm.Soft-agglomerated particle natural subsidence speed is fast, effect of settling good.
Soft-agglomerated particle being spent deionised water 4 times, add a spot of water then, is 60% admittedly contain weight, soaks pulp 120min, treat complete pulp after, in freeze drier, carry out freeze-drying.The pre-freeze temperature is-30 ℃, and the pre-freeze time is 4h, after pre-freeze is finished, carries out vacuum drying 24h under-10～40 ℃ of gradient increased temperatures the ice in the material is distilled, and obtains monodispersed super fine silver powder.The nano-silver powder granularity is 40～70nm, and direct yield can reach more than 99.5%.
Embodiment 5
With the silver nitrate is raw material, in the dispersion of PVP, is silver powder with glucose with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 40～70nm.Soft-agglomerated particle natural subsidence speed is fast, effect of settling good.
Soft-agglomerated particle being spent deionised water 4 times, add a spot of water then, is 50% admittedly contain weight, ultrasonic dispersion treatment 5min under the ultrasonic field of 600W, treat complete pulp after, in freeze drier, carry out freeze-drying.The pre-freeze temperature is-30 ℃, and the pre-freeze time is 4h, after pre-freeze is finished, carries out vacuum drying 24h under-10～40 ℃ of gradient increased temperatures the ice in the material is distilled, and obtains monodispersed super fine silver powder.The nano-silver powder granularity is 40～70nm, and direct yield can reach more than 99.5%.
Embodiment 6
With the silver nitrate is raw material, in the dispersion of PVA, is silver powder with formaldehyde with silver ion reduction under alkali condition.This silver powder is soft-agglomerated particle, and the primary particle granularity is 0.3～1.0 μ m.Soft-agglomerated particle natural subsidence speed is fast, effective.Soft-agglomerated particle being spent deionised water 4 times, add a spot of water then, is 80% admittedly contain weight, ultrasonic dispersion treatment 10min under the ultrasonic field of 600W.After treating complete pulp, in freeze drier, carry out freeze-drying.The pre-freeze temperature is-30 ℃, and the pre-freeze time is 4h, after pre-freeze is finished, carries out vacuum drying 24h under-10～40 ℃ of gradients rise the ice in the material is distilled, and obtains monodispersed super fine silver powder.The super fine silver powder granularity is 0.3～1.0 μ m, and direct yield can reach more than 99.5%.
Claims (7)
1. method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder, it is characterized in that with soft-agglomerated silver powder through washing, add water and soak pulp or ultrasonic dispersion pulp after, carry out freezing final vacuum drying the ice in the material is distilled, obtain monodispersed super fine silver powder.
2. a kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder according to claim 1, it is characterized in that it being to adopt the deionized water washing, add water and soak after pulp or the ultrasonic dispersion pulp, the liquid-solid weight that contains of pulp is 50%-80% after the pulp.
3. a kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder according to claim 1 is characterized in that describedly adding water to soak the pulp time being 60-120min.
4. a kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder according to claim 1, the power that it is characterized in that described ultrasonic dispersion pulp is 360-600W, the time of ultrasonic dispersion is 5-10min.
5. a kind of method of obtaining monodisperse superfine silver powder from soft-agglomerated silver powder according to claim 1 is characterized in that described refrigerating process temperature is freezing 3h-5h under-30～-50 ℃ of temperature; Vacuum drying make ice distillation in the material be under-10～40 ℃ of temperature, carry out vacuum drying ice in the material is sublimed up into contain with silver powder wet weight be under 110 ℃ of temperature＜0.1%.
6. a kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder according to claim 1, it is characterized in that described soft-agglomerated silver powder is is raw material with the silver nitrate, in the dispersion of PVP, under alkali condition with the silver powder of glucose with silver ion reduction.
7. a kind of method of from soft-agglomerated silver powder, obtaining monodisperse superfine silver powder according to claim 1, it is characterized in that described soft-agglomerated silver powder is is raw material with the silver nitrate, in the dispersion of PVA, under alkali condition with the silver powder of formaldehyde with silver ion reduction.
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| CNA2008100978057A CN101279370A (en) | 2008-05-15 | 2008-05-15 | Method for obtaining monodispersed superfine silver powder from soft-agglomerated silver powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104080561A (en) * | 2012-02-02 | 2014-10-01 | 户田工业株式会社 | Silver microparticles, method for producing same, and electronic device, conductive film, and conductive paste containing said silver microparticles |
| CN105345023A (en) * | 2015-10-30 | 2016-02-24 | 溧阳市立方贵金属材料有限公司 | Preparing method for superfine silver powder good in dispersity |
| CN105579533A (en) * | 2013-08-16 | 2016-05-11 | 汉高知识产权控股有限责任公司 | Submicron silver particle ink compositions, process and applications |
-
2008
- 2008-05-15 CN CNA2008100978057A patent/CN101279370A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104080561A (en) * | 2012-02-02 | 2014-10-01 | 户田工业株式会社 | Silver microparticles, method for producing same, and electronic device, conductive film, and conductive paste containing said silver microparticles |
| CN105579533A (en) * | 2013-08-16 | 2016-05-11 | 汉高知识产权控股有限责任公司 | Submicron silver particle ink compositions, process and applications |
| US10301496B2 (en) | 2013-08-16 | 2019-05-28 | Henkel IP & Holding GmbH | Submicron silver particle ink compositions, process and applications |
| CN105345023A (en) * | 2015-10-30 | 2016-02-24 | 溧阳市立方贵金属材料有限公司 | Preparing method for superfine silver powder good in dispersity |
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Open date: 20081008 |