CN107598184A - A kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder - Google Patents
A kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder Download PDFInfo
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- CN107598184A CN107598184A CN201710713852.9A CN201710713852A CN107598184A CN 107598184 A CN107598184 A CN 107598184A CN 201710713852 A CN201710713852 A CN 201710713852A CN 107598184 A CN107598184 A CN 107598184A
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Abstract
The invention discloses a kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder.This method uses seed mediated growth method, passes through deposition of " nucleus-growth " the theoretical control silver nano-grain on silicon dioxide microsphere surface：Silver nitrate powder is dissolved in deionized water first, ammoniacal liquor is added until solution is changed into brown and become colorless again from colourless, obtain silver ammino solution, then silver ammino solution, silicon dioxide microsphere colloidal solution, glucose solution and CTAB solution are added in autoclave, autoclave is placed on 4~6h of reaction under 120 DEG C of environment, the thick solution of silver nano-grain parcel silicon dioxide microsphere is can obtain, finally can obtain silver nano-grain parcel silicon dioxide microsphere powder by centrifuging.In this way, obtained silver nano-grain parcel silicon dioxide microsphere is in regular spherical for profit.
Description
Technical field
The invention belongs to micro-nano spherical field of material preparation, is related to a kind of silver nano-grain parcel silicon dioxide microsphere powder
The preparation method at end.
Background technology
Because silver nano-grain has excellent electric conductivity and thermal conductivity, it is added to the shearing that conducting resinl can be improved in resin
The advantages that intensity, by one of conductive filler as conducting resinl.But silver nano-grain is easily reunited, it is difficult to stable to preserve；
Poor dispersion in resin, cause conductive adhesive performance unstable；And it is expensive, it is limited to a certain extent in conducting resinl
In application.
One layer of silver nano-grain is wrapped up on silicon dioxide microsphere surface, not give only silicon dioxide microsphere electric conductivity, and
And expanded volume fraction of the silver nano-grain in resin, solve silver nano-grain poor dispersion in resin and ask
Topic, can also be preserved for a long time.
The content of the invention
The present invention is in order to expand the application of silver nano-grain, there is provided a kind of silver nano-grain wraps up silicon dioxide microsphere
The preparation method of powder.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder, including following preparation process：First will
Silver nitrate powder is dissolved in deionized water, is added ammoniacal liquor until solution is changed into brown and become colorless again from colourless, is obtained silver-colored ammonia
Solution；Then silver ammino solution, silicon dioxide microsphere colloidal solution, glucose solution and CTAB solution are added in autoclave,
Autoclave is placed on 4~6h of reaction under 120 DEG C of environment, you can the thick solution of silver nano-grain parcel silicon dioxide microsphere is obtained,
Finally silver nano-grain parcel silicon dioxide microsphere powder is can obtain by centrifuging.
The preparation method of above-mentioned silver nano-grain parcel silicon dioxide microsphere powder, specifically includes following steps：
(1) take silver nitrate crystal to be dissolved in deionized water, be uniformly mixed with magnon, then ammoniacal liquor is added dropwise thereto,
Until solution is changed into brown and become colorless again from colourless, silver ammino solution is obtained；
(2) take glucose powder to be dissolved in deionized water, obtain glucose solution；
(3) CTAB powder is taken to be dissolved in deionized water, being heated to 40 DEG C is completely dissolved it, obtains CTAB solution；
(4) take silver ammino solution, silicon dioxide microsphere colloidal solution, glucose solution and CTAB solution to be added in autoclave, use magnetic
Oscillator takes out magnon after being uniformly mixed, then autoclave is placed on 4~6h of reaction under 120 DEG C of environment, you can obtains Yin Na
Rice grain wraps up the thick solution of silicon dioxide microsphere, finally can obtain silver nano-grain parcel silica by centrifuging
Microsphere powder.
The preparation method of silver ammino solution in the step (1)：Magnon stirring in silver nitrate solution is kept, thereto
Ammoniacal liquor is added dropwise, until solution is changed into brown and become colorless again from colourless.
The silicon dioxide microsphere particle diameter of silicon dioxide microsphere colloidal solution in the step (4) is 400~460nm.
The rotating speed of centrifugation in the step (4) is 6000r/min, and centrifugation time is 5 minutes.
The beneficial effect that the present invention is reached：The inventive method can prepare silver nano-grain parcel silicon dioxide microsphere powder
End, and the shape of the silver nano-grain parcel silicon dioxide microsphere prepared is in regular spherical.
Brief description of the drawings
Fig. 1 is the preparation flow figure that silver nano-grain wraps up silicon dioxide microsphere powder.
Embodiment
The present invention is described further with reference to specific embodiment and accompanying drawing.Following examples are only used for clearer
Ground illustrates technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1
(1) take 0.27g silver nitrate crystals to be dissolved in 50mL deionized waters, be uniformly mixed with magnon, then thereto
Ammoniacal liquor is added dropwise, until solution is changed into brown and become colorless again from colourless, obtains silver ammino solution；
(2) take 2.7g glucose powder to be dissolved in 40mL deionized waters, obtain glucose solution；
(3) 1g CTAB powder is taken to be dissolved in 40mL deionized waters, being heated to 40 DEG C is completely dissolved it, and it is molten to obtain CTAB
Liquid；
(4) 2.5mL silver ammino solutions are taken, silicon dioxide microsphere colloidal solution, the 2.5mL glucose solutions that 5mL particle diameters are 400nm
It is added to 3mL CTAB solution in autoclave, magnon is taken out after being uniformly mixed with magnon, then autoclave is placed on
4h is reacted under 120 DEG C of environment, you can the thick solution of silver nano-grain parcel silicon dioxide microsphere is obtained, finally by centrifuging
It can obtain silver nano-grain parcel silicon dioxide microsphere powder.
Its pattern is determined using SEM (SEM) to obtain：Silver nano-grain is wrapped in silicon dioxide microsphere surface,
And in regular spherical.
Embodiment 2
(1) take 0.27g silver nitrate crystals to be dissolved in 50mL deionized waters, be uniformly mixed with magnon, then thereto
Ammoniacal liquor is added dropwise, until solution is changed into brown and become colorless again from colourless, obtains silver ammino solution；
(2) take 2.7g glucose powder to be dissolved in 40mL deionized waters, obtain glucose solution；
(3) 1g CTAB powder is taken to be dissolved in 40mL deionized waters, being heated to 40 DEG C is completely dissolved it, and it is molten to obtain CTAB
Liquid；
(4) 2.5mL silver ammino solutions are taken, silicon dioxide microsphere colloidal solution, the 2.5mL glucose solutions that 5mL particle diameters are 460nm
It is added to 3mL CTAB solution in autoclave, magnon is taken out after being uniformly mixed with magnon, then autoclave is placed on
6h is reacted under 120 DEG C of environment, you can the thick solution of silver nano-grain parcel silicon dioxide microsphere is obtained, finally by centrifuging
It can obtain silver nano-grain parcel silicon dioxide microsphere powder.
Its pattern is determined using SEM (SEM) to obtain：Silver nano-grain is wrapped in silicon dioxide microsphere surface,
And in regular spherical.
Embodiments of the present invention are explained in detail above, but the present invention is not limited to above-mentioned embodiment,
In one of ordinary skill in the art's possessed knowledge, it can also be made on the premise of present inventive concept is not departed from each
Kind change.
Claims (4)
1. a kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder, comprises the following steps：First by silver nitrate
Powder is dissolved in deionized water, is added ammoniacal liquor until solution is changed into brown and become colorless again from colourless, is obtained silver ammino solution；So
Silver ammino solution, silicon dioxide microsphere colloidal solution, glucose solution and CTAB solution are added in autoclave afterwards, autoclave
It is placed on 4~6h of reaction under 120 DEG C of environment, you can obtain the thick solution of silver nano-grain parcel silicon dioxide microsphere, finally pass through
Centrifuge and can obtain silver nano-grain parcel silicon dioxide microsphere powder.
2. the preparation method of silver nano-grain parcel silicon dioxide microsphere powder according to claim 1, it is characterised in that
Specifically include following steps：
(1) take silver nitrate crystal to be dissolved in deionized water, be uniformly mixed with magnon, then ammoniacal liquor is added dropwise thereto,
Until solution is changed into brown and become colorless again from colourless, silver ammino solution is obtained；
(2) take glucose powder to be dissolved in deionized water, obtain glucose solution；
(3) powder is taken to be dissolved in deionized water, being heated to 40 DEG C is completely dissolved it, obtains CTAB solution；
(4) take silver ammino solution, silicon dioxide microsphere colloidal solution, glucose solution and CTAB solution to be added in autoclave, use magnetic
Oscillator takes out magnon after being uniformly mixed, then autoclave is placed on 4~6h of reaction under 120 DEG C of environment, you can obtains Yin Na
Rice grain wraps up the thick solution of silicon dioxide microsphere, finally can obtain silver nano-grain parcel silica by centrifuging
Microsphere powder.
3. the preparation method of silver nano-grain parcel silicon dioxide microsphere powder according to claim 1 or 2, its feature exist
In：The silicon dioxide microsphere particle diameter of described silicon dioxide microsphere colloidal solution is 400~460nm.
4. the preparation method of silver nano-grain parcel silicon dioxide microsphere powder according to claim 2, it is characterised in that：
The rotating speed of centrifugation in the step (4) is 6000r/min, and centrifugation time is 5 minutes.
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Citations (8)
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| KR20130075566A (en) * | 2011-12-27 | 2013-07-05 | 서울대학교산학협력단 | Fabrication method of highly conductive silica/polyaniline core/shell nano particle and application to the pseudo capacitor via solution process |
| CN103223488A (en) * | 2013-05-08 | 2013-07-31 | 宁波大学 | Preparation method for silver-coated silicon dioxide composite microsphere particles |
| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
| CN104439276A (en) * | 2014-11-30 | 2015-03-25 | 湖南科技大学 | Method for fast preparing hollow porous silicon dioxide/silver nanoparticle composite and product |
| CN104550941A (en) * | 2014-11-26 | 2015-04-29 | 东华大学 | Preparation method of silica @ noble metal nano-composite microspheres |
| CN105290394A (en) * | 2015-11-03 | 2016-02-03 | 宁波大学 | Silver-mesoporous silica-silver sandwich core shell nanometer material and preparation and application thereof |
| CN105561988A (en) * | 2014-10-16 | 2016-05-11 | 西安艾菲尔德复合材料科技有限公司 | Synthesizing method for silicon dioxide-silver nano-composite microspheres |
| CN105562714A (en) * | 2016-02-03 | 2016-05-11 | 宁波大学 | Nanometer material for SERS (Surface-Enhanced Raman Scattering) detection and preparing method of nanometer material |
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2017
- 2017-08-18 CN CN201710713852.9A patent/CN107598184A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130075566A (en) * | 2011-12-27 | 2013-07-05 | 서울대학교산학협력단 | Fabrication method of highly conductive silica/polyaniline core/shell nano particle and application to the pseudo capacitor via solution process |
| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
| CN103223488A (en) * | 2013-05-08 | 2013-07-31 | 宁波大学 | Preparation method for silver-coated silicon dioxide composite microsphere particles |
| CN105561988A (en) * | 2014-10-16 | 2016-05-11 | 西安艾菲尔德复合材料科技有限公司 | Synthesizing method for silicon dioxide-silver nano-composite microspheres |
| CN104550941A (en) * | 2014-11-26 | 2015-04-29 | 东华大学 | Preparation method of silica @ noble metal nano-composite microspheres |
| CN104439276A (en) * | 2014-11-30 | 2015-03-25 | 湖南科技大学 | Method for fast preparing hollow porous silicon dioxide/silver nanoparticle composite and product |
| CN105290394A (en) * | 2015-11-03 | 2016-02-03 | 宁波大学 | Silver-mesoporous silica-silver sandwich core shell nanometer material and preparation and application thereof |
| CN105562714A (en) * | 2016-02-03 | 2016-05-11 | 宁波大学 | Nanometer material for SERS (Surface-Enhanced Raman Scattering) detection and preparing method of nanometer material |
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Application publication date: 20180119 |