CN109773210A - A kind of preparation method of the flower shape micro-silver powder with elongated big petal - Google Patents
A kind of preparation method of the flower shape micro-silver powder with elongated big petal Download PDFInfo
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- CN109773210A CN109773210A CN201910166569.8A CN201910166569A CN109773210A CN 109773210 A CN109773210 A CN 109773210A CN 201910166569 A CN201910166569 A CN 201910166569A CN 109773210 A CN109773210 A CN 109773210A
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- silver powder
- preparation
- flower shape
- silver
- shape micro
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 36
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 32
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 16
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 16
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000003643 water by type Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- 241000555268 Dendroides Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of flower shape micro-silver powder with elongated big petal.Preparation method is the following steps are included: now match silver nitrate aqueous solution, aqueous ascorbic acid is promptly added in the silver nitrate aqueous solution of certain stirring rate, it is reacted 5~10 minutes at 20~30 DEG C, silver powder is washed with a large amount of deionized waters immediately later, obtains the flower shape micro-silver powder with elongated big petal after dry.The method does not need additionally to add that the substances such as surfactant, preparation process are simple and easy, and obtained morphologies are uniform, with high purity, conversion ratio is big, are suitble to actual production.
Description
Technical field
The invention belongs to metallic synthesis technical fields, in particular to the flower shape micro-silver powder of elongated big petal
Preparation method.
Background technique
Silver powder can be widely applied to conductive rubber, conductive adhesive, conductive coating etc., be related to electronic equipment, catalysis,
The various fields such as antibacterial, electromagnetic shielding.Currently, being mainly to pass through ball-milling method or chemical synthesis preparation using wider silver powder
Sheet, spherical and near-spherical silver powder, as a kind of small particle flake silver powder of Chinese patent preparation method (CN108405859A), point
Dissipate the good preparation method (CN105345023A) of super fine silver powder etc. of property.In addition, also polygon about being prepared with chemical synthesis
Shape silver powder (CN1401452A), rodlike silver powder (CN1059211765A), dendroid silver powder (CN101811196A,
CN101353814A report).Recently, Chinese patent (CN106424752A, CN101579746A) is disclosed with flower shape
The silver powder of microstructure is applied in electrically conductive ink, can promote the electric conductivity of electrically conductive ink.But it is needed in patent CN106424752A
The first reducing agent solution, the second reducing agent solution, surfactant solution are used, is needed in patent CN101579746A to can
Acid or alcohol are added in soluble silver salt and reducing agent, therefore preparation process is all more complicated.In addition, the flower shape knot of the silver powder of preparation
Petal is all smaller on structure.
Summary of the invention
For above situation, the present invention provides simple flower shape micro-silver powder of the preparation with elongated big petal of one kind
Method.The method does not need addition surfactant etc. substances, easy to operate, and silver powder obtained purity is high, yield are big, fit
Close actual production.
Technical scheme is as follows:
A kind of preparation method of flower shape micro-silver powder with elongated big petal provided by the invention, it is characterized in that:
Silver nitrate is dissolved in the water, silver nitrate aqueous solution is obtained；By reducing agent dissolution of ascorbic acid Yu Shuizhong, resisted
The aqueous solution of bad hematic acid；Aqueous ascorbic acid is promptly added in the silver nitrate aqueous solution of certain stirring rate, 20~
30 DEG C are reacted 5~10 minutes, are washed silver powder with a large amount of deionized waters immediately later, are obtained the flower with elongated big petal after dry
Piece shape micro-silver powder.
The concentration of the silver nitrate aqueous solution is 0.9~1.1mol/L；
The concentration of the aqueous ascorbic acid is 0.9~1.1mol/L；
The silver nitrate and ascorbic acid mass ratio are 1: 1.0~1.1；
The mixing speed is 100~500 revs/min.
Detailed description of the invention
Fig. 1 is the stereoscan photograph for the flower shape micro-silver powder with elongated big petal that the embodiment of the present invention 1 synthesizes
Fig. 2 is the stereoscan photograph for the flower shape micro-silver powder with elongated big petal that the embodiment of the present invention 2 synthesizes
Specific embodiment
Embodiment 1
Silver nitrate is dissolved in the water, the silver nitrate aqueous solution of 0.9mol/L is obtained.By reducing agent dissolution of ascorbic acid in
In water, the aqueous ascorbic acid of 0.9mol/L is obtained.9.6mL aqueous ascorbic acid, which is promptly added to stirring rate, is
In 100 revs/min of 10mL silver nitrate aqueous solution, 20 DEG C are reacted 10 minutes, wash silver powder with a large amount of deionized waters immediately later, are done
The flower shape micro-silver powder with elongated big petal is obtained after dry.
Embodiment 2
Silver nitrate is dissolved in the water, the silver nitrate aqueous solution of 1.1mol/L is obtained.By reducing agent dissolution of ascorbic acid in
In water, the aqueous ascorbic acid of 1.1mol/L is obtained.106mL aqueous ascorbic acid, which is promptly added to stirring rate, is
In 500 revs/min of 100mL silver nitrate aqueous solution, 30 DEG C are reacted 5 minutes, wash silver powder with a large amount of deionized waters immediately later, are done
The flower shape micro-silver powder with elongated big petal is obtained after dry.
Claims (5)
1. a kind of preparation method of the flower shape micro-silver powder with elongated big petal, it is characterized in that:
Silver nitrate is dissolved in the water, silver nitrate aqueous solution is obtained；
By reducing agent dissolution of ascorbic acid Yu Shuizhong, aqueous ascorbic acid is obtained；
Aqueous ascorbic acid is promptly added in the silver nitrate aqueous solution of certain stirring rate, 20~30 DEG C of reactions 5~
10 minutes, silver powder is washed with a large amount of deionized waters immediately later, the flower shape micron silver with elongated big petal is obtained after dry
Powder.
2. a kind of preparation method of flower shape micro-silver powder with elongated big petal described in claim 1, it is characterised in that
The concentration of the silver nitrate aqueous solution is 0.9~1.1mol/L.
3. a kind of preparation method of flower shape micro-silver powder with elongated big petal described in claim 1, it is characterised in that
The concentration of the aqueous ascorbic acid is 0.9~1.1mol/L.
4. a kind of preparation method of flower shape micro-silver powder with elongated big petal described in claim 1, it is characterised in that
The silver nitrate and ascorbic acid mass ratio are 1: 1.0~1.1.
5. a kind of preparation method of flower shape micro-silver powder with elongated big petal described in claim 1, it is characterised in that
The mixing speed is 100~500 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910166569.8A CN109773210A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of the flower shape micro-silver powder with elongated big petal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910166569.8A CN109773210A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of the flower shape micro-silver powder with elongated big petal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109773210A true CN109773210A (en) | 2019-05-21 |
Family
ID=66487425
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910166569.8A Pending CN109773210A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of the flower shape micro-silver powder with elongated big petal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109773210A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110181073A (en) * | 2019-06-21 | 2019-08-30 | 天津大学 | A kind of synthetic method preparing branch shape silver blacker-than-black material |
| CN113245555A (en) * | 2021-05-06 | 2021-08-13 | 潍坊道正新材料科技有限公司 | Petal-shaped conductive silver powder and preparation method thereof |
| CN115055692A (en) * | 2022-07-06 | 2022-09-16 | 江西理工大学南昌校区 | Synthesis method of electronic-grade micro-nano dendritic silver particles for aerosol spraying process |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005146387A (en) * | 2003-11-18 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | Dendrite-shaped fine silver powder, and its production method |
| CN101579746A (en) * | 2008-05-13 | 2009-11-18 | 中国科学院理化技术研究所 | Preparation method of micron-sized superfine silver powder with shapes of pine cones, flowers or trees |
| CN102221543A (en) * | 2011-06-01 | 2011-10-19 | 中国科学院合肥物质科学研究院 | Method for preparing surface enhanced Raman scattering active substrate with three-dimensional silver micro-nano structure |
| CN103386482A (en) * | 2012-05-09 | 2013-11-13 | 五邑大学 | Three-dimensional flower-type metal silver particles and preparation method thereof |
| CN103551589A (en) * | 2013-10-30 | 2014-02-05 | 江苏理工学院 | Method for synthesizing flower-like silver microparticles |
| CN106424752A (en) * | 2016-09-29 | 2017-02-22 | 清华大学深圳研究生院 | Silver powder with flower-shaped microstructure and preparation method thereof and electric conducting ink |
| CN109382524A (en) * | 2018-11-19 | 2019-02-26 | 吉林大学 | A kind of method that one-step method prepares the long controllable flower-shaped silver particles of branch |
-
2019
- 2019-03-01 CN CN201910166569.8A patent/CN109773210A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005146387A (en) * | 2003-11-18 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | Dendrite-shaped fine silver powder, and its production method |
| CN101579746A (en) * | 2008-05-13 | 2009-11-18 | 中国科学院理化技术研究所 | Preparation method of micron-sized superfine silver powder with shapes of pine cones, flowers or trees |
| CN102221543A (en) * | 2011-06-01 | 2011-10-19 | 中国科学院合肥物质科学研究院 | Method for preparing surface enhanced Raman scattering active substrate with three-dimensional silver micro-nano structure |
| CN103386482A (en) * | 2012-05-09 | 2013-11-13 | 五邑大学 | Three-dimensional flower-type metal silver particles and preparation method thereof |
| CN103551589A (en) * | 2013-10-30 | 2014-02-05 | 江苏理工学院 | Method for synthesizing flower-like silver microparticles |
| CN106424752A (en) * | 2016-09-29 | 2017-02-22 | 清华大学深圳研究生院 | Silver powder with flower-shaped microstructure and preparation method thereof and electric conducting ink |
| CN109382524A (en) * | 2018-11-19 | 2019-02-26 | 吉林大学 | A kind of method that one-step method prepares the long controllable flower-shaped silver particles of branch |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110181073A (en) * | 2019-06-21 | 2019-08-30 | 天津大学 | A kind of synthetic method preparing branch shape silver blacker-than-black material |
| CN113245555A (en) * | 2021-05-06 | 2021-08-13 | 潍坊道正新材料科技有限公司 | Petal-shaped conductive silver powder and preparation method thereof |
| CN115055692A (en) * | 2022-07-06 | 2022-09-16 | 江西理工大学南昌校区 | Synthesis method of electronic-grade micro-nano dendritic silver particles for aerosol spraying process |
| CN115055692B (en) * | 2022-07-06 | 2023-09-26 | 江西理工大学南昌校区 | Synthesis method of electronic-grade micro-nano dendritic silver particles for aerosol spraying process |
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Application publication date: 20190521 |