CN114131035A - Silver powder preparation method and silver powder - Google Patents

Silver powder preparation method and silver powder Download PDF

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Publication number
CN114131035A
CN114131035A CN202111465463.1A CN202111465463A CN114131035A CN 114131035 A CN114131035 A CN 114131035A CN 202111465463 A CN202111465463 A CN 202111465463A CN 114131035 A CN114131035 A CN 114131035A
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China
Prior art keywords
silver
silver powder
reaction
preparing
organic solvent
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CN202111465463.1A
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Chinese (zh)
Inventor
范骁
陈珏
陈德
李文龙
龚洁
刘飞全
孙娅
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Changsha New Material Industry Research Institute Co Ltd
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Changsha New Material Industry Research Institute Co Ltd
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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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys

Abstract

The invention provides a method for preparing silver powder and the silver powder obtained by the method. The silver powder is prepared by the solvothermal method, the particle size of the silver powder can be well controlled under the conditions that a soluble silver source or an insoluble silver source is directly used and no other reactant is added in a specific solvent, the solvent can be recycled after reaction, the cost is saved, the post-treatment is simple, the reproducibility of the obtained silver powder is good, the problems in other preparation methods can be avoided, the obtained silver powder can be used as a function to be correspondingly used in electronic paste, and meanwhile, the silver powder has application prospects in the aspects of catalysis, biomedicine and the like.

Description

Silver powder preparation method and silver powder
Technical Field
The invention relates to the technical field of silver powder preparation, in particular to a method for preparing silver powder by a solvothermal method and the silver powder prepared by the method.
Technical Field
Silver has high conductivity, antibacterial property and other special properties, is widely applied to the fields of catalytic materials, optical materials, biomedical treatment and the like at the present stage, and is widely applied to many fields of life and becomes an essential part of the life of people. Silver powder materials have attracted much attention in recent years due to their unique structure and excellent surface properties, and silver powder is often used as a conductive material, one of the main uses of which is for the preparation of flexible electronic products. Generally, it is dispersed in a suitable solvent, printed on a flexible substrate to construct electronic circuits, and made into flexible electronic products. Silver powder has a large specific surface area, a fast electron transfer capability, and a high density of active sites, and is also frequently used in electrochemical sensors to improve the performance of the electrochemical sensors. The silver powder has the characteristics of stable chemical property, relatively low cost and variable structural performance, so that the silver powder has variable application in electrochemical sensors.
At present, the preparation method of the silver powder mainly comprises a mechanical ball milling method, a chemical reduction method, a micro-emulsion method and an electrochemical method, and hydrothermal reaction is rarely reported. The existing high-temperature and high-pressure method for preparing silver powder mainly focuses on a hydrothermal method for preparing silver powder, and few reports are reported on the method for preparing silver powder by using a solvothermal method.
How to better regulate and control the growth process of the silver powder to obtain the silver powder with ideal morphology and uniform particle size distribution, and simultaneously avoid the defects of more impurities, high post-treatment difficulty, environmental pollution of organic solvents and the like of final products caused by adding reaction products and other substances, and is a technical problem to be solved in the field.
Disclosure of Invention
In view of the above, the invention provides a method for preparing silver powder, which adopts a solvothermal method to prepare the silver powder, can better control the particle size of the silver powder under the condition of directly using a soluble or insoluble silver source without adding any other additives and reducing agents, simplifies the post-treatment process, has good reproducibility of the obtained silver powder, can avoid the problems existing in other preparation methods, can be used as a function to be correspondingly used in electronic paste, and has potential application in the aspects of catalysis, biomedicine and the like.
One aspect of the present invention provides a method for preparing silver powder by a solvothermal method, comprising the steps of:
s1, dispersing a silver source in an organic solvent to obtain a silver-containing reaction stock solution;
s2, heating and reacting the reaction stock solution obtained in the step S1 to obtain a solid-liquid mixture;
and S3, separating the solid-liquid mixture to obtain the silver powder.
According to the method for preparing the silver powder by the solvothermal method, the silver source in the step S1 is one or a mixture of more of silver nitrate, silver fluoride, silver chlorate, silver oxalate, silver carbonate and the like.
According to the method for preparing the silver powder by the solvothermal method, the organic solvent in the step S1 is one or a mixture of more of ethylene glycol, isopropanol, n-propanol, tert-butanol and the like.
According to the method for preparing the silver powder by the solvothermal method, the mass ratio of the silver source to the organic solvent in the step S1 is (0.02-1): 1.
according to the method for preparing the silver powder by the solvothermal method, the silver source is silver nitrate, the organic solvent is isopropanol in the step S1, and the mass ratio of the added silver nitrate to the total substance of the added organic solvent in the step S1 is 0.05-0.8.
According to the method for preparing the silver powder by the solvothermal method, the heating reaction temperature is 120-220 ℃, and the reaction time is 5-15 h.
According to the method for preparing silver powder by the solvothermal method, in the step S3, the temperature control mode is that the solvothermal reaction kettle is placed in an oven with a certain temperature, the reaction temperature is controlled to be 150-200 ℃, and the reaction time is 6-10 h.
According to the method for preparing the silver powder by the solvothermal method, the silver particles obtained after the reaction are subjected to solid-liquid separation, and the organic solvent is collected and recycled.
According to another aspect of the invention, the silver powder is prepared by the method for preparing the silver powder by the solvothermal method.
In another aspect of the invention, the electronic paste comprises the silver powder.
Has the advantages that:
1. the preparation process adopts soluble or insoluble silver source, and has no selectivity to the silver source.
2. And no other auxiliary agent or reducing agent is added in the reaction process, the organic solvent is used as a solvent and also plays a role of a reducing agent, the process is simple, errors caused by other manual operations are reduced, and the obtained silver powder has fewer impurities, high purity and uniform structure.
3. The particle size of the prepared silver powder can be regulated and controlled by adjusting conditions such as reaction temperature, reaction time and the like, silver powder particles with different shapes can be obtained to meet different use requirements, and the reaction result reproducibility is good.
4. After the organic solvent after the reaction is recovered, the organic solvent can be continuously used through simple vacuum distillation recovery and purification, so that the cost is saved and the environmental pollution caused by the organic solvent is avoided.
Drawings
FIG. 1 is a picture of a silver nanoparticle powder product obtained in example 1;
FIG. 2 is a scanning electron microscope picture of the silver nanoparticles obtained in example 1;
FIG. 3 is a graph of the spectrum of silver nanoparticles obtained in example 1.
Detailed Description
In some embodiments of the present invention, the method for preparing silver powder by solvothermal method comprises the steps of:
s1, dispersing a silver source in an organic solvent to obtain a silver-containing reaction stock solution;
s2, heating and reacting the reaction stock solution obtained in the step S1 to obtain a solid-liquid mixture;
and S3, separating the solid-liquid mixture to obtain the silver powder.
It has been unexpectedly found that silver powder can be obtained by a hot solvent reaction by merely dispersing a silver source in an organic solvent without adding other reaction substances such as a dispersant, a reducing agent, etc. That is, the reaction liquid in the step S1 may contain only the silver source and the solvent.
In some embodiments, the silver source in step S1 may be selected from one or more of silver nitrate, silver fluoride, silver chlorate, silver oxalate, silver carbonate, and the like.
In some embodiments, the organic solvent in step S1 is a mixture of one or more of ethylene glycol, isopropanol, n-propanol, tert-butanol, and the like.
In some embodiments, the mass ratio of the silver source to the organic solvent in step S1 is 0.02 to 1.
In one embodiment, the silver source in step S1 is silver nitrate, the organic solvent is isopropanol, and the ratio of the amount of silver ion-containing substance added to the silver nitrate to the amount of organic solvent added in step S1 is 0.05-0.8.
In one embodiment, when the silver source is silver nitrate and the organic solvent is isopropanol, the product obtained by the reaction has a better product form than the combination of other parts of silver source and organic solvent, and is more suitable for industrial production and application.
In some embodiments, in the step S2, the heating reaction temperature is 120-220 ℃, and the reaction time is 5-15 h.
Those skilled in the art will appreciate that the vessel for heating the reaction may be varied as long as the corresponding reaction environment is provided. In some embodiments, the reaction vessel is a reaction kettle, reaction tank, or other type of reaction equipment. The heating means may also be varied, and in some embodiments, the heating means is electrical heating, infrared heating, oil bath heating, oven heating, or the like.
In some embodiments, in the step S3, the temperature control manner is to place the solvothermal reaction kettle in an oven with a certain temperature, control the reaction temperature at 150-.
In some embodiments, the silver powder prepared has an average particle size of 60 to 180 nm. The silver powder can be used in the electronic paste as a functional element. In other embodiments, silver powder may be used in catalysis, biomedicine, and the like.
In some embodiments, the silver powder is prepared to have a burnout value of 0.1% to 0.2%.
In some embodiments, in step S3, the silver particles obtained after the reaction are subjected to solid-liquid separation, and the organic solvent is collected and recycled.
In some embodiments, the method of collecting organic solvent for recycling comprises distillation.
In some embodiments, the distilled organic solvent may be used in the solvothermal preparation of silver powder. In some embodiments, the recovered solvent is used in its entirety during the solvothermal preparation of the silver powder. In other embodiments, the recovered solvent is added to the reaction solution as part of the organic solvent.
In step S3, the solid-liquid separation mode may be flexibly selected as long as the solid-liquid separation can be achieved. In some embodiments, the separation method is one or more of filtration, sedimentation, or centrifugation, among others.
In some embodiments, in step S3, the solid-liquid separation further comprises washing and drying steps, and the washing is aimed at removing some impurities in the silver powder, and the washing step is within the scope of the present invention as long as the washing step can achieve the function. The method of the invention does not use components such as a dispersing agent, a reducing agent and the like, and the composition of the product is more single. Preferably, in some embodiments, the surface impurities are removed by washing with deionized water and/or ethanol 3-5 times. And drying after washing to obtain the silver powder, wherein the drying method comprises at least one of vacuum drying, freeze drying, natural drying, heating drying and forced air drying.
The silver powder is prepared by the preparation method, and the burning loss value of the silver powder is 0.1-0.2%. In some embodiments of the present invention, the silver powder has a particle size of 60 to 180 nm.
The invention also provides an electronic paste, which comprises the silver powder.
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Step 1, dissolving 2.55g of silver oxalate in 50g of isopropanol, fully stirring and standing, and precipitating the silver oxalate at the bottom;
step 2, transferring the obtained solution and the precipitate into a reaction kettle, placing the reaction kettle into an oven, setting the temperature of the oven to be 150 ℃, and preserving heat for 6 hours;
and 3, obtaining a solid-liquid mixture after the reaction is finished, performing suction filtration, recovering reaction isopropanol, washing with deionized water for 5 times, then washing with ethanol for 3 times, removing surface impurities, and drying in a 60 ℃ blast oven for 100min to obtain the silver powder.
Example 2
Step 1, dissolving 2.55g of silver nitrate into 50g of isopropanol, and fully stirring and dispersing to obtain a clarified silver nitrate solution;
step 2, transferring the obtained clear solution into a reaction kettle, placing the reaction kettle into an oven, setting the temperature of the oven to be 150 ℃, and preserving heat for 6 hours;
and 3, obtaining a solid-liquid mixture after the reaction is finished, performing suction filtration, recovering reaction isopropanol, washing with deionized water for 5 times, then washing with ethanol for 3 times, removing surface impurities, and drying in a 60 ℃ blast oven for 100min to obtain the silver powder.
Example 3
Step 1, dissolving 3.5g of silver nitrate in 50g of isopropanol, and fully stirring and dispersing to obtain a clarified silver nitrate solution;
step 2, transferring the obtained clear solution into a reaction kettle, placing the reaction kettle into an oven, setting the temperature of the oven to be 150 ℃, and preserving heat for 6 hours;
and 3, obtaining a solid-liquid mixture after the reaction is finished, performing suction filtration, recovering reaction isopropanol, washing with deionized water for 5 times, then washing with ethanol for 3 times, removing surface impurities, and drying in a 60 ℃ blast oven for 100min to obtain the silver powder.
Example 4
Step 1, dissolving 2.55g of silver oxalate in 50g of tert-butyl alcohol, fully stirring and standing, and precipitating the silver oxalate at the bottom;
step 2, transferring the obtained solution and the precipitate into a reaction kettle, setting the temperature of an oven to be 180 ℃, and preserving heat for 8 hours;
and 3, obtaining a solid-liquid mixture after the reaction is finished, performing suction filtration, recovering reaction isopropanol, washing with deionized water for 5 times, then washing with ethanol for 3 times, removing surface impurities, and drying in a 60 ℃ blast oven for 100min to obtain the silver powder.
Comparative example 1
Step 1, dissolving 2.55g of silver nitrate in 50g of water, and fully stirring and dispersing to obtain a clarified silver nitrate solution;
step 2, transferring the obtained clear solution into a reaction kettle, placing the reaction kettle into an oven, setting the temperature of the oven to be 150 ℃, and preserving heat for 6 hours;
and 3, after the reaction is finished, the reaction solution is still a clear and transparent solution, and no solid is generated.
Comparative example 2
Step 1, dissolving 3.5g of silver nitrate in 50g of water, and fully stirring and dispersing to obtain a clarified silver nitrate solution;
step 2, transferring the obtained clear solution into a reaction kettle, setting the temperature of an oven to be 180 ℃, and preserving heat for 10 hours;
and 3, after the reaction is finished, the reaction solution is still a clear and transparent solution, and no solid is generated.
Those skilled in the art will readily appreciate that the above-described preferred embodiments may be freely combined, superimposed, without conflict.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for preparing silver powder by a solvothermal method is characterized by comprising the following steps:
s1, dispersing a silver source in an organic solvent to obtain a silver-containing reaction stock solution;
s2, heating and reacting the reaction stock solution obtained in the step S1 to obtain a solid-liquid mixture;
and S3, separating the solid-liquid mixture to obtain the silver powder.
2. The method for preparing silver powder according to claim 1, wherein the silver source in step S1 is one or more selected from silver nitrate, silver fluoride, silver chlorate, silver oxalate, and silver carbonate.
3. The method for preparing silver powder according to claim 1, wherein the organic solvent in step S1 is a mixture of one or more of ethylene glycol, isopropanol, n-propanol, tert-butanol, etc.
4. The method for producing silver powder according to claim 1, wherein the mass ratio of the silver source to the organic solvent in step S1 is (0.02-1): 1.
5. the method for preparing silver powder according to claim 1, wherein the silver source in step S1 is silver nitrate, the organic solvent is isopropyl alcohol, and the silver ion-containing substance is added in an amount of 0.05 to 0.8 by mass based on the total substance of the organic solvents added in step S1.
6. The method for preparing silver powder by the solvothermal method as claimed in claim 1, wherein the heating reaction temperature is 120 ℃ and 220 ℃ and the reaction time is 5-15 h.
7. The method for preparing silver powder according to claim 1, wherein in step S3, the temperature is controlled by placing the solvothermal reaction kettle in an oven at a certain temperature, wherein the reaction temperature is controlled at 150 ℃ and 200 ℃ and the reaction time is 6-10 h.
8. The method for preparing silver powder according to claim 1, wherein the silver particles obtained after the reaction are subjected to solid-liquid separation, and the organic solvent is collected and recycled.
9. A silver powder, characterized in that the silver powder is produced by the solvothermal method for producing a silver powder according to any one of claims 1 to 8.
10. An electronic paste, characterized in that it comprises the silver powder according to claim 9.
CN202111465463.1A 2021-11-30 2021-11-30 Silver powder preparation method and silver powder Pending CN114131035A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4539041A (en) * 1982-12-21 1985-09-03 Universite Paris Vii Process for the reduction of metallic compounds by polyols, and metallic powders obtained by this process
US20040025635A1 (en) * 2001-04-02 2004-02-12 Kurihara Lynn K. Processing of nanocrystalline metallic powders and coatings using the polyol process
JP2005146386A (en) * 2003-11-18 2005-06-09 Mitsui Mining & Smelting Co Ltd Method of producing metal powder slurry, and nickel powder slurry obtained by the production method
CN1768152A (en) * 2003-01-31 2006-05-03 拉尔夫·W·布鲁斯 Microwave assisted continuous synthesis of manocrystalline powders and coatings using the polyol process
JP2017057488A (en) * 2015-09-18 2017-03-23 株式会社応用ナノ粒子研究所 Manufacturing method of nano silver particle and nano silver particle
CN110014168A (en) * 2019-05-23 2019-07-16 深圳先进技术研究院 A kind of nano-Ag particles and preparation method thereof
CN111168083A (en) * 2020-02-24 2020-05-19 深圳先进技术研究院 Preparation method of nano silver powder

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4539041A (en) * 1982-12-21 1985-09-03 Universite Paris Vii Process for the reduction of metallic compounds by polyols, and metallic powders obtained by this process
US20040025635A1 (en) * 2001-04-02 2004-02-12 Kurihara Lynn K. Processing of nanocrystalline metallic powders and coatings using the polyol process
CN1768152A (en) * 2003-01-31 2006-05-03 拉尔夫·W·布鲁斯 Microwave assisted continuous synthesis of manocrystalline powders and coatings using the polyol process
JP2005146386A (en) * 2003-11-18 2005-06-09 Mitsui Mining & Smelting Co Ltd Method of producing metal powder slurry, and nickel powder slurry obtained by the production method
JP2017057488A (en) * 2015-09-18 2017-03-23 株式会社応用ナノ粒子研究所 Manufacturing method of nano silver particle and nano silver particle
CN110014168A (en) * 2019-05-23 2019-07-16 深圳先进技术研究院 A kind of nano-Ag particles and preparation method thereof
CN111168083A (en) * 2020-02-24 2020-05-19 深圳先进技术研究院 Preparation method of nano silver powder

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