CN114799198A - High-dispersity nanogold powder and preparation method thereof - Google Patents
High-dispersity nanogold powder and preparation method thereof Download PDFInfo
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- CN114799198A CN114799198A CN202210390606.5A CN202210390606A CN114799198A CN 114799198 A CN114799198 A CN 114799198A CN 202210390606 A CN202210390606 A CN 202210390606A CN 114799198 A CN114799198 A CN 114799198A
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- gold powder
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 title description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 75
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000006722 reduction reaction Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- 238000009826 distribution Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 8
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical group CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 4
- 229940015043 glyoxal Drugs 0.000 claims description 4
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical group [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 3
- DLRJIFUOBPOJNS-UHFFFAOYSA-N phenetole Chemical compound CCOC1=CC=CC=C1 DLRJIFUOBPOJNS-UHFFFAOYSA-N 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 34
- 239000000919 ceramic Substances 0.000 description 8
- 239000010931 gold Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 238000010344 co-firing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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 provides a preparation method of high-dispersion nanoscale gold powder, which comprises the following steps: firstly, preparing a gold chloride solution; step two, preparing a reducing agent solution; thirdly, preparing gold powder through reduction reaction; fourthly, washing, wherein the average particle size distribution of the prepared nano-grade gold powder is 0.5-20 nm, and the apparent density is 4-6 g/cm 3 . The gold powder prepared by the method has no agglomeration phenomenon, the method is simple, the flow is short, and no waste liquid is generated in the preparation process.
Description
Technical Field
The invention relates to the technical field of gold powder preparation, in particular to a preparation method of high-dispersity nano gold powder in an organic system.
Background
Low temperature co-fired ceramic (LTCC) combines a multilayer ceramic element technology with a multilayer circuit pattern, and a modular integrated device or a three-dimensional ceramic-based multilayer circuit is manufactured by co-firing low temperature sintered ceramic and a metal inner conductor at the temperature of below 900 ℃. The technology is widely applied to the preparation of products such as multilayer ceramic capacitors and inductors, ceramic dielectric filters, optical communication substrates, ceramic antennas and the like, and has already gained important application in the military electronic fields such as aerospace, radar, communication and the like.
The conductive slurry is mainly used for manufacturing a precise circuit and plays a conductive role after being sintered. The gold paste has the advantages of excellent chemical property stability and conductivity, almost no electron migration in a severe environment, adaptability to a complex use environment and the like, and becomes one of the first raw materials for preparing high-reliability military electronic components in the aerospace and military fields. The gold powder is a key material for preparing the gold paste, and the quality of the performance of the gold powder directly determines the quality of the performance of the electronic element.
The existing method for preparing superfine gold powder (the particle size of the gold powder is less than 5 microns) is mainly prepared by reducing the gold powder with a reducing agent in an aqueous solution system, organic substances are required to be added as dispersing agents in the preparation process, and the gold powder is prevented from agglomeration, and the type and the adding proportion of the dispersing agents are difficult to accurately control, so that the gold powder prepared in the aqueous system has more or less agglomeration. The method for preparing the gold powder is to prepare the gold powder by reducing an organic system, the solvent is the dispersing agent, and the gold powder with high dispersibility can be prepared without adding other dispersing agents.
Disclosure of Invention
The invention aims to provide a preparation method of high-dispersion nanoscale gold powder, the prepared gold powder has no agglomeration phenomenon, the method is simple, the flow is short, and no waste liquid is generated in the preparation process.
In order to solve the technical problems, the invention provides a preparation method of high-dispersion nanoscale gold powder, which comprises the following steps:
firstly, preparing a gold chloride solution;
step two, preparing a reducing agent solution;
thirdly, preparing gold powder through reduction reaction;
and fourthly, washing.
The first step is specifically to dissolve gold chloride solid by using an organic solvent to prepare a gold chloride organic solution with the mass concentration of 10-50 g/L.
And the second step is to add a reducing agent into the organic solution of the gold chloride prepared in the first step, wherein the mass of the reducing agent is 3-5 times of that of the gold chloride.
The reducing agent is acetaldehyde, glyoxal or hydroquinone.
The organic solvent is butyl ether, anisole, phenetole, ethylene glycol or propylene glycol.
And the third step is further specifically heating the solution obtained in the second step for reflux reaction without stirring for 1-3 hours until the organic solution is colorless, stopping heating, and precipitating the gold powder obtained by reduction to the bottom of the solution.
And the fourth step is to pour out the solution obtained in the third step, precipitate gold powder at the bottom, wash the gold powder for 1 time by using ethanol, and dry the gold powder at 50-80 ℃ to obtain the high-dispersity nanoscale gold powder.
The prepared gold powder is sphere-like powder, the average particle size distribution is 0.5-20 nm, and the apparent density is 4-6 g/cm 3 The powder dispersibility is high.
The gold paste for the LTCC device prepared by using the nanoscale gold powder has good printing performance and good co-firing matching with a green ceramic tape. The slurry is sintered to obtain a compact gold thin film which has low resistance, good conductivity and high fine wire resolution.
The invention has the advantages of
(1) In the gold powder preparation process, the reduction is carried out in an organic system, a dispersing agent is not required to be added in the reduction process, the pH value of the solution is not required to be adjusted, the nano-scale gold powder can be obtained by directly heating and refluxing, the gold powder is free of agglomeration, the method is simple, the flow is short, and the gold powder can be rapidly prepared in a large amount.
(2) The organic solvent used in the preparation process of the gold powder can be distilled and purified and can be repeatedly used, and no waste liquid is generated in the preparation process.
(3) The gold powder prepared by the method is settled to the bottom of the flask, the gold powder is easy to clean, the upper solution is poured out, and the lower part of the gold powder can be dried only by cleaning with ethanol once. The gold powder can not be adhered in the drying process.
Detailed Description
The invention provides a preparation method of high-dispersion nanoscale gold powder, which comprises the following steps:
firstly, preparing a gold chloride solution;
step two, preparing a reducing agent solution;
thirdly, preparing gold powder through reduction reaction;
and fourthly, washing.
The first step is specifically to dissolve gold chloride solid by using an organic solvent to prepare a gold chloride organic solution with the mass concentration of 10-50 g/L.
And the second step is to add a reducing agent into the organic solution of the gold chloride prepared in the first step, wherein the mass of the reducing agent is 3-5 times of that of the gold chloride.
The reducing agent is acetaldehyde, glyoxal or hydroquinone.
The organic solvent is butyl ether, anisole, phenetole, ethylene glycol or propylene glycol.
And the third step is further specifically heating the solution obtained in the second step for reflux reaction without stirring for 1-3 hours until the organic solution is colorless, stopping heating, and precipitating the gold powder obtained by reduction to the bottom of the solution.
And the fourth step is to pour out the solution obtained in the third step, precipitate gold powder at the bottom, wash the gold powder for 1 time by using ethanol, and dry the gold powder at 50-80 ℃ to obtain the high-dispersity nanoscale gold powder.
The prepared gold powder is sphere-like powder, the average particle size distribution is 0.5-20 nm, and the apparent density is 4-6 g/cm 3 The powder dispersibility is high.
The gold paste for the LTCC device prepared by using the nanoscale gold powder has good printing performance and good co-firing matching with a green ceramic tape. The slurry is sintered to obtain a compact gold thin film which has low resistance, good conductivity and high fine wire resolution.
The following embodiments are described in detail to solve the technical problems by applying technical means to the present invention, and the implementation process of achieving the technical effects can be fully understood and implemented.
Example 1
Dissolving gold chloride solid in anisole to prepare a gold chloride organic solution with the mass concentration of 10 g/L; adding an organic reducing agent, namely glyoxal, of which the mass is 3 times that of gold chloride, into an organic solution of the gold chloride; heating the solution for reflux reaction without stirring for 1.5 hours, stopping heating, and standing for half an hour until brown nanoscale gold powder is precipitated at the bottom of the solution; pouring out most of organic solution, washing gold powder at the bottom with ethanol for 1 time, and drying at 50 deg.C to obtain product with average particle diameter of 10nm and apparent density of 5.8g/cm 3 The gold powder of (1).
Example 2
Dissolving a gold chloride solid in butyl ether to prepare a gold chloride organic solution with the mass concentration of 25 g/L; adding an organic reducing agent acetaldehyde with the mass 4 times of the mass of the gold chloride into an organic solution of the gold chloride; heating the solution for reflux reaction without stirring for 2.5 hours, stopping heating, and standing for half an hour until brown nanoscale gold powder is precipitated at the bottom of the solution; pouring out most of organic solution, washing gold powder at the bottom with ethanol for 1 time, and drying at 60 deg.C to obtain product with average particle diameter of 5nm and apparent density of 4.3g/cm 3 The gold powder of (1).
Example 3
Dissolving a gold chloride solid in ethylene glycol to prepare a gold chloride organic solution with the mass concentration of 50 g/L; adding an organic reducing agent hydroquinone with the mass 5 times of the mass of the gold chloride into an organic solution of the gold chloride; heating the solution for reflux reaction without stirring, reacting for 3 hours, stopping heating, and standing for half an hour until brown nanoscale gold powder is precipitated at the bottom of the solution; most of the organic solution was poured firstPouring out gold powder at the bottom, washing with ethanol for 1 time, oven drying at 80 deg.C to obtain powder with average particle diameter of 20nm and apparent density of 5.6g/cm 3 The gold powder of (1).
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of high-dispersion nanoscale gold powder is characterized by comprising the following steps:
firstly, preparing a gold chloride solution;
step two, preparing a reducing agent solution;
thirdly, preparing gold powder through reduction reaction;
the fourth step, washing,
the average particle size distribution of the prepared nano-grade gold powder is 0.5-20 nm, and the apparent density is 4-6 g/cm 3 。
2. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: the first step is specifically to dissolve gold chloride solid by using an organic solvent to prepare a gold chloride organic solution with the mass concentration of 10-50 g/L.
3. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: and the second step is to add a reducing agent into the organic solution of the gold chloride prepared in the first step, wherein the mass of the reducing agent is 3-5 times of that of the gold chloride.
4. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: the reducing agent is acetaldehyde, glyoxal or hydroquinone.
5. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: the organic solvent is butyl ether, anisole, phenetole, ethylene glycol or propylene glycol.
6. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: and the third step is further specifically heating the solution obtained in the second step for reflux reaction without stirring for 1-3 hours until the organic solution is colorless, stopping heating, and precipitating the gold powder obtained by reduction to the bottom of the solution.
7. The method for preparing highly dispersed nanoscale gold powder according to claim 1, wherein: and the fourth step is to pour out the solution obtained in the third step, precipitate gold powder at the bottom, wash the gold powder for 1 time by using ethanol, and dry the gold powder at 50-80 ℃ to obtain the high-dispersity nanoscale gold powder.
8. Nanoscale gold powder produced by the production method according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210390606.5A CN114799198A (en) | 2022-04-14 | 2022-04-14 | High-dispersity nanogold powder and preparation method thereof |
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| CN202210390606.5A CN114799198A (en) | 2022-04-14 | 2022-04-14 | High-dispersity nanogold powder and preparation method thereof |
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| CN114799198A true CN114799198A (en) | 2022-07-29 |
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|---|---|---|---|
| CN202210390606.5A Pending CN114799198A (en) | 2022-04-14 | 2022-04-14 | High-dispersity nanogold powder and preparation method thereof |
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| Country | Link |
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| CN (1) | CN114799198A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116079065A (en) * | 2023-04-07 | 2023-05-09 | 山东有研国晶辉新材料有限公司 | Liquid-phase carbon removal method for gold chloride solution |
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| CN104985191A (en) * | 2015-07-08 | 2015-10-21 | Tcl集团股份有限公司 | Silver nano cube with monodispersity and preparation method and conductive ink thereof |
| CN105817645A (en) * | 2016-05-13 | 2016-08-03 | 溧阳市立方贵金属材料有限公司 | Ultra-pure silver powder preparation method capable of controlling particle size |
| CN108941609A (en) * | 2018-09-10 | 2018-12-07 | 河南金渠银通金属材料有限公司 | Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof |
| CN109622985A (en) * | 2018-12-11 | 2019-04-16 | 有研亿金新材料有限公司 | A kind of preparation method of high decentrality submicron grade bronze |
| WO2020222542A1 (en) * | 2019-05-02 | 2020-11-05 | 파워팩 주식회사 | Oxidation stability-improved silver nano powder prepared by wet process and method for preparing same |
| CN113399679A (en) * | 2021-05-08 | 2021-09-17 | 东方电气集团科学技术研究院有限公司 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
-
2022
- 2022-04-14 CN CN202210390606.5A patent/CN114799198A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090029148A1 (en) * | 2005-09-22 | 2009-01-29 | Nippon Shokubai Co., Ltd. | Metal Nanoparticle, Metal Nanoparticle Colloid, Method for Storing Metal Nanoparticle Colloid, and Metal Coating Film |
| CN104985191A (en) * | 2015-07-08 | 2015-10-21 | Tcl集团股份有限公司 | Silver nano cube with monodispersity and preparation method and conductive ink thereof |
| CN105817645A (en) * | 2016-05-13 | 2016-08-03 | 溧阳市立方贵金属材料有限公司 | Ultra-pure silver powder preparation method capable of controlling particle size |
| CN108941609A (en) * | 2018-09-10 | 2018-12-07 | 河南金渠银通金属材料有限公司 | Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof |
| CN109622985A (en) * | 2018-12-11 | 2019-04-16 | 有研亿金新材料有限公司 | A kind of preparation method of high decentrality submicron grade bronze |
| WO2020222542A1 (en) * | 2019-05-02 | 2020-11-05 | 파워팩 주식회사 | Oxidation stability-improved silver nano powder prepared by wet process and method for preparing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116079065A (en) * | 2023-04-07 | 2023-05-09 | 山东有研国晶辉新材料有限公司 | Liquid-phase carbon removal method for gold chloride solution |
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