CN112935244A - Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry - Google Patents
Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry Download PDFInfo
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- CN112935244A CN112935244A CN202110108726.7A CN202110108726A CN112935244A CN 112935244 A CN112935244 A CN 112935244A CN 202110108726 A CN202110108726 A CN 202110108726A CN 112935244 A CN112935244 A CN 112935244A
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- silver nitrate
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- 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
- B22F1/17—Metallic particles coated with metal
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Abstract
The invention discloses a process for preparing silver-coated copper composite powder for photovoltaic use, which replaces pure silver slurry, comprises copper powder, mixed reducing solution, silver nitrate and ammonia water, and comprises the following steps: sensitizing copper powder to obtain sensitized copper powder; preparing a mixed reducing solution, and dispersing the sensitized copper powder into the mixed reducing solution to obtain a standby solution; mixing silver nitrate and ammonia water to obtain silver nitrate-ammonia water mixed solution; mixing the standby solution with a silver nitrate-ammonia water mixed solution, and treating to obtain the product. The invention greatly improves the safety and environmental protection in the operation process, and simultaneously, in the implementation process of the process flow, the raw material replacement efficiency is improved by using a silver ion rather than a metal silver mode, the waste of valuable raw materials in the process is greatly reduced, and the utilization rate of the raw materials is improved.
Description
Technical Field
The invention discloses a silver-coated copper composite powder process for photovoltaic use instead of pure silver slurry, and belongs to the technical field of photovoltaic processes.
Background
Pure silver paste is a conductive material which is used for dip coating and screen printing processes in the electronic industry at the earliest time, and the pure silver paste is required to be used as a preparation raw material of important accessories in the manufacturing of photovoltaic power generation equipment, however, the pure silver paste can generate toxic substances in the preparation process, and the multiple preparation processes are very easy to cause waste of silver materials, so that the improvement exists.
Disclosure of Invention
The technical problem to be solved by the present invention is to overcome the problems mentioned in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a process for preparing silver-coated copper composite powder for photovoltaic use instead of pure silver slurry comprises copper powder, mixed reducing liquid, silver nitrate and ammonia water, and comprises the following steps:
s1, sensitizing the copper powder to obtain sensitized copper powder;
s2, preparing a mixed reducing solution, and dispersing the sensitized copper powder into the mixed reducing solution to obtain a standby solution;
s3, mixing silver nitrate and ammonia water to obtain a silver nitrate-ammonia water mixed solution;
and S4, mixing the standby liquid with the silver nitrate-ammonia water mixed liquid, and treating to obtain the product.
Preferably, the step S1 includes:
s1.1, adding copper powder into dilute sulfuric acid, and removing copper oxide and impurities on the surface of the copper powder;
s1.2, cleaning the treated copper powder for 4-5 times by using ultrapure water, then adding the cleaned copper powder into stannous chloride solution with the concentration of 8-15g/L for sensitization, centrifugally stirring the mixture for 1-2 hours at normal temperature, and removing supernatant to obtain spare copper powder;
s1.3, washing the spare copper powder with ultrapure water for 4-6 times, and carrying out air drying at normal temperature to obtain the sensitized copper powder.
Preferably, the step S2 includes:
s2.1, mixing L-ascorbic acid with a dispersing agent to obtain a mixed reducing solution, wherein the using amount of the 1-ascorbic acid is 2.2 times of the molar weight of silver nitrate;
s2.2, the using amount of the dispersing agent is 10 times of the molar weight of silver nitrate;
and S2.3, dispersing the sensitized copper powder in the mixed reducing solution, and uniformly stirring to obtain a standby solution.
Preferably, the concentration of silver nitrate in the step S3 is 140g/L, and the concentration of ammonia water is 130g/L, respectively.
Preferably, the step S4 includes:
s4.1, mixing the standby solution and the silver nitrate-ammonia water mixed solution under stirring at the rotating speed of 10r/S-15r/S, wherein the temperature of a stirring kettle is 45-50 ℃, and the stirring reaction time is 35-40 minutes;
s4.2, standing and settling for 2.5-3 hours after stirring is finished, removing supernate and taking precipitate;
and S4.3, cleaning and drying to obtain the product.
Preferably, the dilute sulfuric acid concentration in step S1.1 is 8% by weight.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, copper powder, mixed reducing liquid, silver nitrate, ammonia water and other raw materials are respectively treated and sequentially mixed to obtain the silver-coated copper composite powder, the operation process is simple and easy to operate, heavy metal toxic impurities generated in the reaction process of copper, silver and other metal substances are avoided, the safety and the environmental protection performance of the invention in the operation process are greatly improved, and meanwhile, in the implementation process of the process flow, the raw material replacement efficiency is improved by using a silver ion rather than a metal silver mode, the waste of precious raw materials in the process is greatly reduced, and the utilization rate of the raw materials is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A process for preparing silver-coated copper composite powder for photovoltaic use instead of pure silver slurry comprises copper powder, mixed reducing liquid, silver nitrate and ammonia water, and comprises the following steps:
s1, sensitizing the copper powder to obtain sensitized copper powder;
wherein the step S1 includes:
s1.1, adding copper powder into dilute sulfuric acid with the weight percentage concentration of 8% to remove copper oxide and impurities on the surface of the copper powder, wherein the design enables the oxidized impurities and the attached other impurities of the copper powder in the air to be subjected to reaction extraction in the processing process of the copper powder, and the oxidized impurities and the attached other impurities are separated from the copper powder to reduce the impurities of raw materials;
s1.2, cleaning the treated copper powder for 4-5 times by using ultrapure water, then adding the cleaned copper powder into stannous chloride solution with the concentration of 8-15g/L for sensitization, centrifugally stirring the mixture for 1-2 hours at normal temperature, and removing supernatant to obtain standby copper powder, wherein the design is used for removing solution impurities in the copper powder and reducing the negative influence of the extracted solution on other materials in the subsequent processing process;
s1.3, cleaning the spare copper powder for 4-6 times by using ultrapure water, and carrying out normal-temperature air drying to obtain the sensitized copper powder.
Example 2
S2, preparing a mixed reducing solution, and dispersing the sensitized copper powder into the mixed reducing solution to obtain a standby solution;
wherein the step S2 includes:
s2.1, mixing L-ascorbic acid and a dispersing agent to obtain a mixed reducing solution, wherein the using amount of the 1-ascorbic acid is 2.2 times of the molar weight of silver nitrate, and the design is used for dispersing the silver nitrate so that the silver nitrate can fully react with other materials in the subsequent processing process;
s2.2, the using amount of the dispersing agent is 10 times of the molar weight of silver nitrate;
s2.3, dispersing the sensitized copper powder in the mixed reducing liquid, and uniformly stirring to obtain a standby liquid.
Example 3
S3, mixing silver nitrate and ammonia water to obtain a silver nitrate-ammonia water mixed solution, wherein the silver nitrate concentration is 140g/L, and the ammonia water concentration is 130g/L, respectively.
Example 4
S4, mixing the standby liquid with a silver nitrate-ammonia water mixed liquid, and treating to obtain a product;
wherein the step S4 includes:
s4.1, mixing the standby liquid and the silver nitrate-ammonia water mixed liquid under stirring at the rotating speed of 10r/S-15r/S, wherein the temperature of a stirring kettle is 45-50 ℃, and the stirring reaction time is 35-40 minutes, and the design is used for combining copper powder in the standby liquid with silver ions so that the silver ions can be coated on the surfaces of the copper powder, and a silver-coated copper composite powder body can be obtained smoothly;
s4.2, standing and settling for 2.5-3 hours after stirring, removing supernatant and taking precipitate, wherein the design is used for removing liquid components in the product to obtain a final product;
and S4.3, cleaning and drying to obtain the product.
Specifically, the copper powder, the mixed reducing solution, the silver nitrate, the ammonia water and other raw materials are respectively treated and sequentially mixed to obtain the silver-coated copper composite powder, the operation process is simple and easy to operate, heavy metal toxic impurities generated in the reaction process of copper, silver and other metal substances are avoided, the safety and the environmental friendliness in the operation process of the invention are greatly improved, meanwhile, in the implementation process of the process flow of the invention, the raw material replacement efficiency is improved by using a silver ion rather than a metal silver mode, the waste of precious raw materials in the process is greatly reduced, and the utilization rate of the raw materials is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The process for preparing the silver-coated copper composite powder for photovoltaic use instead of pure silver slurry is characterized by comprising copper powder, mixed reducing solution, silver nitrate and ammonia water, and comprises the following steps:
s1, sensitizing the copper powder to obtain sensitized copper powder;
s2, preparing a mixed reducing solution, and dispersing the sensitized copper powder into the mixed reducing solution to obtain a standby solution;
s3, mixing silver nitrate and ammonia water to obtain a silver nitrate-ammonia water mixed solution;
and S4, mixing the standby liquid with the silver nitrate-ammonia water mixed liquid, and treating to obtain the product.
2. The silver-clad copper composite powder process for photovoltaic use, instead of pure silver paste, according to claim 1, wherein the step S1 includes:
s1.1, adding copper powder into dilute sulfuric acid, and removing copper oxide and impurities on the surface of the copper powder;
s1.2, cleaning the treated copper powder for 4-5 times by using ultrapure water, then adding the cleaned copper powder into stannous chloride solution with the concentration of 8-15g/L for sensitization, centrifugally stirring the mixture for 1-2 hours at normal temperature, and removing supernatant to obtain spare copper powder;
s1.3, washing the spare copper powder with ultrapure water for 4-6 times, and carrying out air drying at normal temperature to obtain the sensitized copper powder.
3. The silver-clad copper composite powder process for photovoltaic use, instead of pure silver paste, according to claim 1, wherein the step S2 includes:
s2.1, mixing L-ascorbic acid with a dispersing agent to obtain a mixed reducing solution, wherein the using amount of the 1-ascorbic acid is 2.2 times of the molar weight of silver nitrate;
s2.2, the using amount of the dispersing agent is 10 times of the molar weight of silver nitrate;
and S2.3, dispersing the sensitized copper powder in the mixed reducing solution, and uniformly stirring to obtain a standby solution.
4. The process of claim 1, wherein the silver nitrate concentration in the step S3 is 140g/L, and the ammonia water concentration is 110-130 g/L.
5. The silver-clad copper composite powder process for photovoltaic use, instead of pure silver paste, according to claim 1, wherein the step S4 includes:
s4.1, mixing the standby solution and the silver nitrate-ammonia water mixed solution under stirring at the rotating speed of 10r/S-15r/S, wherein the temperature of a stirring kettle is 45-50 ℃, and the stirring reaction time is 35-40 minutes;
s4.2, standing and settling for 2.5-3 hours after stirring is finished, removing supernate and taking precipitate;
and S4.3, cleaning and drying to obtain the product.
6. The process of claim 2, wherein the dilute sulfuric acid in step S1.1 is 8 wt% in the silver-coated copper composite powder for photovoltaic use instead of pure silver paste.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110108726.7A CN112935244A (en) | 2021-01-27 | 2021-01-27 | Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110108726.7A CN112935244A (en) | 2021-01-27 | 2021-01-27 | Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry |
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| CN112935244A true CN112935244A (en) | 2021-06-11 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004052044A (en) * | 2002-07-19 | 2004-02-19 | Mitsui Mining & Smelting Co Ltd | Silver-coated copper powder and its manufacturing method |
| CN1876282A (en) * | 2006-07-07 | 2006-12-13 | 清华大学 | Chemical method for silver coating on copper powder surface |
| CN102328076A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver coated copper powder for electronic slurry |
| CN102554222A (en) * | 2012-03-15 | 2012-07-11 | 上海交通大学 | Preparation method of silver-coated copper composite powders |
| CN102950282A (en) * | 2012-10-15 | 2013-03-06 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver-copper coating powder |
| CN105149575A (en) * | 2015-10-23 | 2015-12-16 | 乐山新天源太阳能科技有限公司 | Preparation method of silver coated copper powder |
| JP2017025380A (en) * | 2015-07-23 | 2017-02-02 | 三井金属鉱業株式会社 | Silver-coated copper powder and method for producing the same |
| CN111360246A (en) * | 2020-04-24 | 2020-07-03 | 刘勤华 | Silver-coated copper powder with high coating rate and excellent quality and preparation method thereof |
-
2021
- 2021-01-27 CN CN202110108726.7A patent/CN112935244A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004052044A (en) * | 2002-07-19 | 2004-02-19 | Mitsui Mining & Smelting Co Ltd | Silver-coated copper powder and its manufacturing method |
| CN1876282A (en) * | 2006-07-07 | 2006-12-13 | 清华大学 | Chemical method for silver coating on copper powder surface |
| CN102328076A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver coated copper powder for electronic slurry |
| CN102554222A (en) * | 2012-03-15 | 2012-07-11 | 上海交通大学 | Preparation method of silver-coated copper composite powders |
| CN102950282A (en) * | 2012-10-15 | 2013-03-06 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver-copper coating powder |
| JP2017025380A (en) * | 2015-07-23 | 2017-02-02 | 三井金属鉱業株式会社 | Silver-coated copper powder and method for producing the same |
| CN105149575A (en) * | 2015-10-23 | 2015-12-16 | 乐山新天源太阳能科技有限公司 | Preparation method of silver coated copper powder |
| CN111360246A (en) * | 2020-04-24 | 2020-07-03 | 刘勤华 | Silver-coated copper powder with high coating rate and excellent quality and preparation method thereof |
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Application publication date: 20210611 |
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