CN115475953B - Preparation method of netlike nano silver - Google Patents
Preparation method of netlike nano silver Download PDFInfo
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- CN115475953B CN115475953B CN202211100615.2A CN202211100615A CN115475953B CN 115475953 B CN115475953 B CN 115475953B CN 202211100615 A CN202211100615 A CN 202211100615A CN 115475953 B CN115475953 B CN 115475953B
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- Prior art keywords
- netlike
- nano silver
- agno
- glycol
- silver
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 7
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- VMPITZXILSNTON-UHFFFAOYSA-N o-anisidine Chemical compound COC1=CC=CC=C1N VMPITZXILSNTON-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229940083025 silver preparation Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of netlike nano silver, which comprises the following steps: firstly, a certain concentration of AgNO is configured at a certain temperature 3 Glycol/water solution; next, agNO is introduced into 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution; after reacting for a period of time, centrifuging, washing and drying the product to obtain the netlike nano silver. The invention provides a method for preparing the netlike nano silver, which is simple and convenient to operate, good in stability, good in repeatability and high in yield, and is suitable for large-scale production of the netlike nano silver.
Description
Technical Field
The invention relates to the field of metallic silver preparation, in particular to a method for preparing a silver alloy by utilizing FeSO 4 Reduction of AgNO 3 The method for obtaining the netlike nano silver.
Background
The application field of nano silver is wide. The conductive coating is an important conductive medium of high-performance conductive coating, is a basic material of a flexible circuit board, a contact switch, a film switch and the like, and is also various high-end electrodes and electromagnetic compatible materials.
Application performance and shape of nano silverThe appearance structure is closely related. Therefore, the preparation method of the nano silver with different morphological structures is always a research hot spot. The silver nanoribbon coated with the polyamino anisole is prepared by using silver nitrate as a metal salt precursor, water as a solvent and the amino anisole as a reducing agent under the high-temperature hydrothermal condition by using the king dragon (CN 102009185B). Lai Yuekun (CN 109848439B) sequentially dissolving dopamine, copper sulfate and hydrogen peroxide in Tris buffer solution, mechanically stirring for a certain time, centrifuging to obtain polydopamine, finally dripping polydopamine solution into the mixed solution of silver nitrate and copper sulfate, and mechanically stirring and reacting for a certain time to obtain the silver nano-sheet. Zhao Xiaopeng (CN 101603186B) liquid diacid diester with AgNO 3 The oil/water interface formed by the aqueous solution is a soft membrane plate, the carbon fiber microelectrode is used as a cathode, and the chrysanthemum-like structure formed by the silver nanoribbon is prepared by a chemical electrodeposition method under the induction of the interface soft membrane plate.
FeSO 4 The solution contains ferrous ions, and can be used as a reducing agent to reduce silver ions into silver simple substance. Currently, feSO is adopted 4 The reduction system is also disclosed for obtaining nano silver with different morphological structures. Cai Xionghui (CN 103273082B) uses silver nitrate as silver source and FeSO 4 The flower-shaped spherical nano silver is obtained by taking a reducing agent, binary or more than binary organic acid, organic acid anhydride or organic acid salt as the reducing agent and reacting for a certain time at a certain temperature. Lu Ying (CN 105127448B) in the form of a prepared AgNO 3 Sequentially adding PVP and FeSO into the solution 4 Dilute H 2 SO 4 And obtaining the ultra-large area nano silver flake after the reaction of the solution. Chen Liqiao (CN 105268992B) is a two-dimensional silver flake which is obtained by direct reaction using a silver nitrate solution as an oxidizing solution and a ferrous sulfate and/or ascorbic acid solution containing an azide as a reducing solution. Cheng Zhipeng (CN 109014241B) using HF as structure directing agent, feSO 4 The silver hollow frame structure material is prepared by a reduction system.
Therefore, the nano silver with various shapes and structures can be prepared by adopting the prior art; however, the preparation method for the netlike nano silver is still relatively lacking in the prior art.
Disclosure of Invention
The invention aims at: providing a method for adopting FeSO 4 The method for preparing the reticular nano silver by the reduction system realizes the large-scale production of the reticular nano silver.
The technical scheme of the invention is as follows: a preparation method of netlike nano silver comprises the following specific steps:
(1) At a certain temperature, a certain concentration of AgNO is configured 3 Glycol/water solution;
(2) To AgNO 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution;
(3) After reacting for a period of time, centrifuging, washing and drying the product to obtain the netlike nano silver.
In the step (1), the certain temperature is 0-10 ℃.
In the step (1), agNO with certain concentration 3 The volume ratio of the glycol/water is 1/9~3/7, and the glycol/water solution is 0.0005-0.001 mol/L.
In the step (2), agNO in the mixed solution 3 、HF、FeSO 4 The mass ratio of (2) is 1: (0.5-1): (0.7 to 1.2).
In the step (3), the reaction time is 10-30 minutes.
The principle of the invention is as follows: in the reaction system of the present invention, feSO 4 As AgNO 3 The reducing agent realizes the smooth proceeding of the reducing process; HF and Ag + Coordination complexing, regulating and controlling the dynamic process of the reaction; the glycol reduces the ion migration rate in the solution, regulates the reaction rate to a certain extent, and can be adsorbed on the surface of the formed silver crystal nucleus to influence the growth habit of silver. FeSO in the whole reaction system 4 And the synchronous and accurate control of the reaction concentration of ethylene glycol and HF and the reaction temperature realizes the dynamic and thermodynamic stable growth of the reticular nano silver.
Compared with the prior art, the invention has the beneficial effects that: the prior art has realized the scale production of silver nanobelts, silver nanosheets, spherical nano silver and the like, but is difficult to obtain the netlike nano silver, and the netlike nano silver can be prepared on a large scale by adopting the technology of the invention, the process is simple, and the product yield is high.
Drawings
Fig. 1 is a scanning electron microscope picture of the network nano silver of example 1.
Fig. 2 is a scanning electron microscope picture of the network nano silver of example 2.
Fig. 3 scanning electron microscope pictures of the network nano silver of example 3.
Detailed Description
The following examples are presented to further illustrate the technical aspects of the present invention, but are not to be construed as limiting the technical aspects.
Example 1: the netlike nano silver is prepared according to the following steps
(1) At the temperature of 0 ℃, a certain concentration of AgNO is prepared 3 Glycol/water solution; the AgNO with certain concentration 3 The volume ratio of the glycol to the water is 1/9, and the glycol/water solution is 0.0005-0.001 mol/L;
(2) To AgNO 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution; agNO in the mixed solution 3 、HF、FeSO 4 The mass ratio of (2) is 1:0.5:0.7;
(3) After reacting for 10 minutes, centrifuging, washing and drying the product to obtain the netlike nano silver.
Example 2: the netlike nano silver is prepared according to the following steps
(1) At a temperature of 5 ℃, a certain concentration of AgNO is prepared 3 Glycol/water solution; the AgNO with certain concentration 3 Ethylene glycol/water solution is 0.00075 mol/L, wherein the volume ratio of ethylene glycol/water is 1/7;
(2) To AgNO 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution; agNO in the mixed solution 3 、HF、FeSO 4 The mass ratio of (2) is 1: 0.75-1: 0.95;
(3) After reacting for 20 minutes, centrifuging, washing and drying the product to obtain the netlike nano silver.
Example 3: the netlike nano silver is prepared according to the following steps
(1) At the temperature of 10 ℃, a certain concentration of AgNO is prepared 3 Glycol/water solution; the AgNO with certain concentration 3 The volume ratio of the glycol to the water is 3/7;
(2) To AgNO 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution; agNO in the mixed solution 3 、HF、FeSO 4 The mass ratio of (2) is 1:1:1.2;
(3) After 30 minutes of reaction, the resultant is centrifuged, washed and dried to obtain the netlike nano silver.
Claims (2)
1. A preparation method of netlike nano silver is characterized by comprising the following specific steps:
(1) At a certain temperature, a certain concentration of AgNO is configured 3 Glycol/water solution; the certain temperature is 0-10 ℃; the AgNO with certain concentration 3 The volume ratio of the glycol to the water is 1/9~3/7, and the glycol/water solution is 0.0005-0.001 mol/L;
(2) To AgNO 3 Adding a certain amount of HF structure directing agent and FeSO into glycol/water solution 4 A reducing agent to form a mixed solution; agNO in the mixed solution 3 、HF、FeSO 4 The mass ratio of (2) is 1: (0.5-1): (0.7-1.2);
(3) After reacting for a period of time, centrifuging, washing and drying the product to obtain the netlike nano silver.
2. The method for preparing the netlike nano-silver according to claim 1, wherein the method comprises the following steps: in the step (3), the reaction time is 10-30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211100615.2A CN115475953B (en) | 2022-09-09 | 2022-09-09 | Preparation method of netlike nano silver |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211100615.2A CN115475953B (en) | 2022-09-09 | 2022-09-09 | Preparation method of netlike nano silver |
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| Publication Number | Publication Date |
|---|---|
| CN115475953A CN115475953A (en) | 2022-12-16 |
| CN115475953B true CN115475953B (en) | 2024-01-26 |
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| CN202211100615.2A Active CN115475953B (en) | 2022-09-09 | 2022-09-09 | Preparation method of netlike nano silver |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030044276A (en) * | 2001-11-29 | 2003-06-09 | 한국지질자원연구원 | Preparation of flake-type fine silver powders |
| CN102672199A (en) * | 2012-06-01 | 2012-09-19 | 中国科学院理化技术研究所 | Preparation method of silver particle with sheet-strip integrated structural shape |
| CN104607655A (en) * | 2015-03-06 | 2015-05-13 | 苏州大学 | Silver nanowire preparation method |
| KR101527522B1 (en) * | 2014-01-16 | 2015-06-18 | 주식회사 효성 | Manufacturing method of silver nano ring and thereof silver nano ring |
| CN106424755A (en) * | 2016-11-08 | 2017-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Silver microwire, preparation and application |
| CN109014241A (en) * | 2018-08-29 | 2018-12-18 | 淮阴师范学院 | A method of preparing silver-colored micron hollow frame structural material |
| CN114381169A (en) * | 2020-10-19 | 2022-04-22 | 湖南工业大学 | High-conductivity nano-silver conductive ink and preparation method thereof |
| CN114974646A (en) * | 2022-06-21 | 2022-08-30 | 北京信息科技大学 | Preparation method of reticular nano silver and reticular nano silver |
| CN115852680A (en) * | 2022-11-07 | 2023-03-28 | 浙江理工大学 | Preparation method and application of hot-press reinforced multifunctional nano-silver fabric without adhesive |
-
2022
- 2022-09-09 CN CN202211100615.2A patent/CN115475953B/en active Active
Patent Citations (9)
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|---|---|---|---|---|
| KR20030044276A (en) * | 2001-11-29 | 2003-06-09 | 한국지질자원연구원 | Preparation of flake-type fine silver powders |
| CN102672199A (en) * | 2012-06-01 | 2012-09-19 | 中国科学院理化技术研究所 | Preparation method of silver particle with sheet-strip integrated structural shape |
| KR101527522B1 (en) * | 2014-01-16 | 2015-06-18 | 주식회사 효성 | Manufacturing method of silver nano ring and thereof silver nano ring |
| CN104607655A (en) * | 2015-03-06 | 2015-05-13 | 苏州大学 | Silver nanowire preparation method |
| CN106424755A (en) * | 2016-11-08 | 2017-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Silver microwire, preparation and application |
| CN109014241A (en) * | 2018-08-29 | 2018-12-18 | 淮阴师范学院 | A method of preparing silver-colored micron hollow frame structural material |
| CN114381169A (en) * | 2020-10-19 | 2022-04-22 | 湖南工业大学 | High-conductivity nano-silver conductive ink and preparation method thereof |
| CN114974646A (en) * | 2022-06-21 | 2022-08-30 | 北京信息科技大学 | Preparation method of reticular nano silver and reticular nano silver |
| CN115852680A (en) * | 2022-11-07 | 2023-03-28 | 浙江理工大学 | Preparation method and application of hot-press reinforced multifunctional nano-silver fabric without adhesive |
Non-Patent Citations (1)
| Title |
|---|
| 不同溶剂体系生成纳米银形貌研究;陈艳艳;陈广学;崔艳艳;陈奇峰;邰晶磊;杨宇;;包装工程(21);全文 * |
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| CN115475953A (en) | 2022-12-16 |
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