[go: up one dir, main page]

CN112705726A - Preparation method of shape-controllable nano silver powder - Google Patents

Preparation method of shape-controllable nano silver powder Download PDF

Info

Publication number
CN112705726A
CN112705726A CN202011498607.9A CN202011498607A CN112705726A CN 112705726 A CN112705726 A CN 112705726A CN 202011498607 A CN202011498607 A CN 202011498607A CN 112705726 A CN112705726 A CN 112705726A
Authority
CN
China
Prior art keywords
nano
silver powder
silver
preparation
nano silver
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011498607.9A
Other languages
Chinese (zh)
Inventor
林志丹
曹琳
张鹏
李卫
王启伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinan University
Original Assignee
Jinan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jinan University filed Critical Jinan University
Priority to CN202011498607.9A priority Critical patent/CN112705726A/en
Publication of CN112705726A publication Critical patent/CN112705726A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

本发明涉及纳米银制备技术领域,具体公开了一种形貌可控的纳米银粉的制备方法。所述的制备方法包含如下步骤:将硝酸银和聚乙烯吡咯烷酮溶解在乙二醇中,然后加入聚乙二醇;反应结束后即得纳米银粉。本发明提供了一种全新的纳米银粉的制备方法,该方法可以快速制备得到形貌可控的纳米银粉;成功克服了以硝酸银为原料、以聚乙烯吡咯烷酮为稳定剂、以乙二醇为还原剂制备纳米银,无法制备形貌可控的纳米银的技术缺陷。采用本发明所述的方法,可以快速制备得到粒径分布范围较窄、粒径均匀的纳米银粉。

Figure 202011498607

The invention relates to the technical field of nano-silver preparation, and specifically discloses a preparation method of nano-silver powder with controllable morphology. The preparation method comprises the following steps: dissolving silver nitrate and polyvinylpyrrolidone in ethylene glycol, then adding polyethylene glycol; and obtaining nano silver powder after the reaction is completed. The invention provides a brand-new preparation method of nano-silver powder, which can quickly prepare nano-silver powder with controllable morphology; successfully overcomes the problem of using silver nitrate as raw material, polyvinylpyrrolidone as stabilizer and ethylene glycol as The technical defect of preparing nano-silver with reducing agent is the inability to prepare nano-silver with controllable morphology. By adopting the method of the present invention, nano-silver powder with narrow particle size distribution range and uniform particle size can be quickly prepared.

Figure 202011498607

Description

Preparation method of shape-controllable nano silver powder
Technical Field
The invention relates to the technical field of nano silver preparation, in particular to a preparation method of nano silver powder with controllable morphology.
Background
The 21 st century is an era of rapid development of electronic information manufacturing industry, electronic products such as smart phones, tablet computers, electronic books and wearable watches are ubiquitous, and the life style of human beings is thoroughly changed. With the development of high-tech industries, research and development of new related materials have attracted much attention from governments and research institutions throughout the world.
The micro-nano material has the characteristics of high surface activity, large surface area and the like, so that the micro-nano material becomes a 'pet' in the research field of related new materials, and particularly, the micro-nano structure material with optical and electric characteristics, such as micro-nano noble metal gold and silver, becomes a very active topic in the research field. Among them, the silver nanoparticles have advantages of excellent conductivity, oxidation resistance, low-temperature sintering property, stable chemical properties, easy processing, etc., and thus are widely used in the production of electronic tags (fidd), solar cell electrodes, membrane switches, flexible printed circuit boards, Organic Light Emitting Diodes (OLEDs), transparent conductive films, etc.
The application of the nano silver powder mainly takes conductive paste or electronic paste as a carrier, the nano silver powder is used as a conductive phase to be filled in a conductive compound to prepare conductive silver paste, conductive silver ink and the like, and then electronic printing means such as screen printing, impression printing, ink-jet printing and the like are used for producing electronic products and components thereof. That is to say, the silver nanopowder as the conductive filler is the basis of the conductive ink material, and plays an important role in the conductive silver paste and the conductive silver ink. In recent years, the investment of various countries on preparing high-performance nano silver powder is huge, and silver powder manufacturers such as DuPont, Sumitomo and Tianzhong Japan occupy most of the global market due to the advanced production process. However, the starting of China is relatively late, and a small gap exists between high-end silver powder products and abroad, so that the development of the nano silver powder which has excellent product quality and can be applied to actual products has very important theoretical and practical significance.
The liquid phase reduction method has become one of the most main methods for preparing the micro-nano silver powder because of the advantages of simple production equipment, convenient operation, low price of raw materials and the like. However, the existing liquid phase reduction method is difficult to realize high-efficiency production with controllable size and controllable shape, and the service performance and application value of the nano silver powder are seriously influenced. Therefore, the rapid and controllable preparation of the nano silver powder with uniform size and single appearance is a technical problem in the field of silver powder production at present.
The closest prior art (schwann (er.) bracelet, et al research on the synthesis of stable nano-silver sol by ethylene glycol method [ J ] chemical world, 2009,5:257 + 259) discloses a method for preparing nano-silver sol by using silver nitrate as a raw material, polyvinylpyrrolidone as a stabilizer and ethylene glycol as a reducing agent; although the method can realize the rapid preparation of the nano silver, the prepared nano silver has a random shape; the method is uncontrollable and impossible for preparing nano silver with specific shape and size.
Disclosure of Invention
In order to solve the technical problems that in the prior art, silver nitrate is used as a raw material, polyvinylpyrrolidone is used as a stabilizer, and glycol is used as a reducing agent to prepare nano silver, the shape of the nano silver is not controllable, and the nano silver with consistent shape cannot be prepared; the invention provides a preparation method of nanometer silver powder with controllable morphology.
The technical problem to be solved by the invention is realized by the following technical scheme:
a preparation method of nanometer silver powder with controllable morphology comprises the following steps:
dissolving silver nitrate and polyvinylpyrrolidone in ethylene glycol, and then adding polyethylene glycol; and (3) reacting for 15-30 min at 130-160 ℃, and obtaining the nano silver powder after the reaction is finished.
The inventor finds that the nano silver is prepared by taking silver nitrate as a raw material, polyvinylpyrrolidone as a stabilizing agent and glycol as a reducing agent, although the nano silver can be quickly prepared; the prepared nano silver is irregular in shape, and the prepared nano silver has various shapes such as particles, blocks and rods; the preparation of the material cannot be controlled to obtain single granular, blocky or rod-shaped materials; namely, the method cannot control the shape of the nano silver. However, with the method, how to realize controllable morphology and produce nano silver with single morphology is a great technical problem in the field.
In order to solve the problem, the inventor finds out that: polyethylene glycol is added in the process of preparing the nano silver by using silver nitrate as a raw material, polyvinylpyrrolidone as a stabilizer and ethylene glycol as a reducing agent, and all the prepared nano silver is granular without the appearance of blocky and rodlike nano silver. Therefore, the single shape can be successfully prepared by adding the polyethylene glycol in the process of preparing the nano-silver by using the silver nitrate as the raw material, the polyvinylpyrrolidone as the stabilizer and the ethylene glycol as the reducing agent, and the technical problem that the shape of the nano-silver cannot be controlled in the prior art is solved.
Preferably, the using amount ratio of the silver nitrate to the polyvinylpyrrolidone to the ethylene glycol is 1g: 1-2 g: 150-300 mL.
Most preferably, the ratio of the amounts of silver nitrate, polyvinylpyrrolidone and ethylene glycol is 1g:1.5g:200 mL.
Preferably, the volume ratio of the ethylene glycol to the polyethylene glycol is 1-2: 1-2.
Most preferably, the volume ratio of ethylene glycol to polyethylene glycol is 2: 1.
Preferably, the reaction conditions are at 140 ℃ for 20 min.
Preferably, the reaction is carried out while stirring.
Preferably, the preparation method of the morphology-controllable nano silver powder specifically comprises the following steps:
dissolving silver nitrate and polyvinylpyrrolidone in ethylene glycol, and reacting for 5-10 min at 130-160 ℃; adding polyethylene glycol containing octyl phenol polyoxyethylene ether-10, and continuously reacting for 10-20 min at 130-160 ℃; and obtaining the nano silver powder after the reaction is finished.
Further research by the inventor shows that under the above method conditions, the nano silver powder with a single granular morphology can be prepared; however, the prepared silver powder still has the defect of wide particle size distribution range, which causes uneven particle size. However, on the basis of the method, how to prepare the nano silver powder with narrow particle size distribution range and uniform particle size is another technical problem in the front of technicians.
In order to solve the problem, the inventors further conducted a large number of experiments and found that: in the preparation steps, silver nitrate and polyvinylpyrrolidone are dissolved in ethylene glycol to react for 5-10 min, then polyethylene glycol containing octyl phenol polyoxyethylene ether-10 is added, and the reaction is continued for 10-20 min at 130-160 ℃. And adding polyethylene glycol containing octyl phenol polyoxyethylene ether-10 after reacting for a period of time, so that the prepared nano silver particles have narrow particle size distribution range and uniform particle size. The method successfully overcomes the defect of uneven particle size caused by wider particle size distribution range of the particles.
Preferably, the dosage ratio of the octyl phenol polyoxyethylene ether-10 to the polyethylene glycol is 1g: 100-200 mL.
Preferably, the polyethylene glycol is polyethylene glycol 400.
Preferably, the molecular weight of the polyvinylpyrrolidone is 25000-60000.
Has the advantages that: the invention provides a brand-new preparation method of nano silver powder, which can quickly prepare the nano silver powder with controllable morphology; the technical defect that the shape-controllable nano silver can not be prepared by using silver nitrate as a raw material, polyvinylpyrrolidone as a stabilizer and ethylene glycol as a reducing agent is overcome successfully. By adopting the method, the nano silver powder with narrow particle size distribution range and uniform particle size can be quickly prepared.
Drawings
FIG. 1 is an SEM photograph of the nano silver powder prepared in example 1.
FIG. 2 is an SEM image of the nano silver powder prepared in example 2.
Fig. 3 is an SEM image of the nano silver powder prepared in comparative example 1.
Fig. 4 is an SEM image of the nano silver powder prepared in comparative example 2.
Fig. 5 is an SEM image of the nano silver powder prepared in comparative example 3.
Detailed Description
The present invention will be further explained with reference to the following specific examples and drawings, but the examples are not intended to limit the present invention in any manner.
EXAMPLE 1 preparation of Nano silver powder
(1) Dissolving 0.1g of silver nitrate and 0.15g of polyvinylpyrrolidone (molecular weight of 58000) in 20ml of ethylene glycol, adding 10ml of polyethylene glycol 400, and fully mixing and stirring to obtain a mixed solution;
(2) reacting the mixed solution at 140 ℃ for 20min at the magnetic stirring speed of 200 r/min;
(3) diluting with anhydrous ethanol 5 times after reaction, and centrifuging at 8000r/min for 20 min; and (3) after the solution is layered, sucking out the supernatant by using an injector, washing and purifying the precipitate solution by using absolute ethyl alcohol again, and repeating the process for 3 times to obtain the nano silver powder.
EXAMPLE 2 preparation of Nano silver powder
(1) Dissolving 0.1g of silver nitrate and 0.15g of polyvinylpyrrolidone (molecular weight of 58000) in 20ml of ethylene glycol, and reacting at 140 ℃ and a magnetic stirring rate of 200r/min for 5 min; then adding 10ml of polyethylene glycol 400 containing 0.1g of octyl phenol polyoxyethylene ether-10, and fully mixing and stirring to obtain a mixed solution;
(2) reacting the mixed solution at 140 ℃ for 15min at the magnetic stirring speed of 200 r/min;
(3) diluting with anhydrous ethanol 5 times after reaction, and centrifuging at 8000r/min for 20 min; and (3) after the solution is layered, sucking out the supernatant by using an injector, washing and purifying the precipitate solution by using absolute ethyl alcohol again, and repeating the process for 3 times to obtain the nano silver powder.
Example 2 differs from example 1 in that silver nitrate and polyvinylpyrrolidone are dissolved in ethylene glycol in the preparation step and reacted for a certain period of time, and then polyethylene glycol containing octylphenol polyoxyethylene ether-10 is added.
Comparative example 1 preparation of Nano silver powder
(1) Dissolving 0.1g of silver nitrate and 0.15g of polyvinylpyrrolidone (molecular weight of 58000) in 20ml of ethylene glycol, then adding 10ml of ethylene glycol, and fully mixing and stirring to obtain a mixed solution;
(2) reacting the mixed solution at 140 ℃ for 20min at the magnetic stirring speed of 200 r/min;
(3) diluting with anhydrous ethanol 5 times after reaction, and centrifuging at 8000r/min for 20 min; and (3) after the solution is layered, sucking out the supernatant by using an injector, washing and purifying the precipitate solution by using absolute ethyl alcohol again, and repeating the process for 3 times to obtain the nano silver powder.
The difference between the comparative example 1 and the example 1 is that no reducing agent polyethylene glycol is added in the preparation process, and all the reducing agent ethylene glycol is used as the reducing agent.
Comparative example 2 preparation of Nano silver powder
(1) Dissolving 0.1g of silver nitrate and 0.15g of polyvinylpyrrolidone (molecular weight of 58000) in 20ml of ethylene glycol, and reacting at 140 ℃ and a magnetic stirring rate of 200r/min for 5 min; then adding 10ml of polyethylene glycol 400, and fully mixing and stirring to obtain a mixed solution;
(2) reacting the mixed solution at 140 ℃ for 15min at the magnetic stirring speed of 200 r/min;
(3) diluting with anhydrous ethanol 5 times after reaction, and centrifuging at 8000r/min for 20 min; and (3) after the solution is layered, sucking out the supernatant by using an injector, washing and purifying the precipitate solution by using absolute ethyl alcohol again, and repeating the process for 3 times to obtain the nano silver powder.
Comparative example 2 differs from example 2 in that the polyethylene glycol added stepwise does not contain octylphenol polyoxyethylene ether-10.
Comparative example 3 preparation of Nano silver powder
(1) Dissolving 0.1g of silver nitrate and 0.15g of polyvinylpyrrolidone (molecular weight of 58000) in 20ml of ethylene glycol, and reacting at 140 ℃ and a magnetic stirring rate of 200r/min for 5 min; then adding 10ml of polyethylene glycol 400 containing 0.1g of sodium dodecyl benzene sulfonate, and fully mixing and stirring to obtain a mixed solution;
(2) reacting the mixed solution at 140 ℃ for 15min at the magnetic stirring speed of 200 r/min;
(3) diluting with anhydrous ethanol 5 times after reaction, and centrifuging at 8000r/min for 20 min; and (3) after the solution is layered, sucking out the supernatant by using an injector, washing and purifying the precipitate solution by using absolute ethyl alcohol again, and repeating the process for 3 times to obtain the nano silver powder.
Comparative example 3 is different from example 2 in that silver nitrate and polyvinylpyrrolidone are dissolved in ethylene glycol to react for a certain period of time in the preparation step, and then polyethylene glycol containing sodium dodecylbenzenesulfonate is added. And example 2 was the addition of polyethylene glycol containing octylphenol polyoxyethylene ether-10.
Scanning SEM images of the nano silver powder prepared in the examples 1-2 and the comparative examples 1-3 by using an ULTRA 55FESEM type field emission scanning electron microscope produced by Germany Zeiss company; observing the morphology and the particle size range of the nano silver powder through an SEM picture; the results are shown in Table 1 and FIGS. 1 to 5.
TABLE 1 statistical results of morphology and particle size range of nano silver powder
Morphology of Range of particle size
Example 1 All in granular form 30~170nm
Example 2 All in granular form 30~50nm
Comparative example 1 Stick, block and granule -
Comparative example 2 All in granular form 40~140nm
Comparative example 3 All in granular form 40~120nm
As can be seen from table 1 and attached fig. 1 to 5, all the shapes of the nano silver particles prepared in example 1 are granular; the nano silver particles prepared in the comparative example 1 have irregular shapes including rods, blocks and particles. The preparation method is characterized in that polyethylene glycol is added in the process of preparing nano silver by taking silver nitrate as a raw material, polyvinylpyrrolidone as a stabilizer and ethylene glycol as a reducing agent, and all the prepared nano silver is granular without the appearance of blocky and rodlike nano silver; the method can successfully prepare the nano silver with single appearance, overcomes the technical problem that the appearance of the nano silver cannot be controlled in the prior art, and successfully realizes the appearance control.
As can be seen from the table 1 and the attached drawings 1-5, although the granular nano silver powder can be prepared in the embodiment 1, the shape can be controlled; however, the prepared nano silver powder particles have the particle size range of 30-170 nm, wide particle size range and uneven particle size. In the embodiment 2, on the basis of the embodiment 1, silver nitrate and polyvinylpyrrolidone are dissolved in ethylene glycol and are reacted for a period of time, then polyethylene glycol containing octyl phenol polyoxyethylene ether-10 is added for reaction, the particle size range of the silver nanoparticles can be successfully controlled within 30-50 nm by adopting the method, the particle size range of the silver nanoparticles is greatly reduced, and the silver nanoparticles obtained by adopting the technical method have narrow particle size range and uniform size; the method successfully solves the defect of uneven particle size caused by wider particle size distribution range of the particles.
As can be seen from Table 1 and accompanying FIGS. 1-5, comparative examples 2 and 3 have no significant improvement in particle size range over example 1; the silver nitrate and the polyvinylpyrrolidone are dissolved in the ethylene glycol to react for a period of time, and then the polyethylene glycol containing the octyl phenol polyoxyethylene ether-10 is added to obtain the nano silver particles with narrow particle size range and uniform size; the polyethylene glycol does not contain octyl phenol polyoxyethylene ether-10 or contains other dispersing agents, and the nano silver particles with narrow particle size range and uniform size cannot be prepared.

Claims (10)

1.一种形貌可控的纳米银粉的制备方法,其特征在于,包含如下步骤:1. a preparation method of shape-controllable nano-silver powder, is characterized in that, comprises the steps: 将硝酸银和聚乙烯吡咯烷酮溶解在乙二醇中,然后加入聚乙二醇;反应后即得纳米银粉。The silver nitrate and polyvinylpyrrolidone are dissolved in ethylene glycol, and then polyethylene glycol is added; after the reaction, nano silver powder is obtained. 2.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,硝酸银、聚乙烯吡咯烷酮以及乙二醇的用量比为1g:1~2g:150~300mL。2 . The method for preparing nano-silver powder with controllable morphology according to claim 1 , wherein the dosage ratio of silver nitrate, polyvinylpyrrolidone and ethylene glycol is 1g:1~2g:150~300mL. 3 . 3.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,硝酸银、聚乙烯吡咯烷酮以及乙二醇的用量比为1g:1.5g:200mL。3. The preparation method of shape-controllable nano-silver powder according to claim 1, wherein the dosage ratio of silver nitrate, polyvinylpyrrolidone and ethylene glycol is 1g:1.5g:200mL. 4.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,乙二醇与聚乙二醇的体积比为1~2:1~2;最优选地,乙二醇与聚乙二醇的体积比为2:1。4. The method for preparing nano-silver powder with controllable morphology according to claim 1, wherein the volume ratio of ethylene glycol to polyethylene glycol is 1-2:1-2; most preferably, ethylene glycol The volume ratio of alcohol to polyethylene glycol was 2:1. 5.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,所述反应的条件为在130~160℃下反应15~30min。5 . The method for preparing nano-silver powder with controllable morphology according to claim 1 , wherein the reaction condition is to react at 130-160° C. for 15-30 min. 6 . 6.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,所述反应的条件为在140℃下反应20min。6 . The method for preparing nano-silver powder with controllable morphology according to claim 1 , wherein the reaction condition is to react at 140° C. for 20 min. 7 . 7.根据权利要求1所述的形貌可控的纳米银粉的制备方法,其特征在于,具体包含如下步骤:7. the preparation method of shape-controllable nano-silver powder according to claim 1, is characterized in that, specifically comprises the following steps: 将硝酸银和聚乙烯吡咯烷酮溶解在乙二醇中,在130~160℃下反应5~10min;接着加入含有辛基苯酚聚氧乙烯醚-10的聚乙二醇,继续在130~160℃下反应10~20min;反应结束后即得纳米银粉。Dissolve silver nitrate and polyvinylpyrrolidone in ethylene glycol, react at 130-160°C for 5-10min; then add polyethylene glycol containing octylphenol polyoxyethylene ether-10, continue at 130-160°C The reaction is carried out for 10-20 minutes; after the reaction is completed, the nano-silver powder is obtained. 8.根据权利要求7所述的形貌可控的纳米银粉的制备方法,其特征在于,辛基苯酚聚氧乙烯醚-10与聚乙二醇的用量比为1g:100~200mL。8 . The method for preparing nano-silver powder with controllable morphology according to claim 7 , wherein the dosage ratio of octylphenol ethoxylate-10 and polyethylene glycol is 1 g: 100-200 mL. 9 . 9.根据权利要求1~8任一项所述的形貌可控的纳米银粉的制备方法,其特征在于,所述的聚乙二醇为聚乙二醇400。9 . The method for preparing nano-silver powder with controllable morphology according to claim 1 , wherein the polyethylene glycol is polyethylene glycol 400. 10 . 10.根据权利要求1~8任一项所述的形貌可控的纳米银粉的制备方法,其特征在于,所述的聚乙烯吡咯烷酮的分子量为25000~60000。10 . The method for preparing nano-silver powder with controllable morphology according to claim 1 , wherein the molecular weight of the polyvinylpyrrolidone is 25,000-60,000. 11 .
CN202011498607.9A 2020-12-17 2020-12-17 Preparation method of shape-controllable nano silver powder Pending CN112705726A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011498607.9A CN112705726A (en) 2020-12-17 2020-12-17 Preparation method of shape-controllable nano silver powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011498607.9A CN112705726A (en) 2020-12-17 2020-12-17 Preparation method of shape-controllable nano silver powder

Publications (1)

Publication Number Publication Date
CN112705726A true CN112705726A (en) 2021-04-27

Family

ID=75544378

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011498607.9A Pending CN112705726A (en) 2020-12-17 2020-12-17 Preparation method of shape-controllable nano silver powder

Country Status (1)

Country Link
CN (1) CN112705726A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117921016A (en) * 2023-04-03 2024-04-26 北京机科国创轻量化科学研究院有限公司 A method for preparing nano-scale ultrafine silver powder of photovoltaic silver paste

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070275259A1 (en) * 2006-05-25 2007-11-29 Samsung Electro-Mechanics Co., Ltd. Method of producing metal nanoparticles and metal nanoparticles produced thereby
US20090023007A1 (en) * 2004-02-10 2009-01-22 Mitsui Mining & Smelting Co., Ltd. Highly crystalline silver powder and method for producing the same
CN102205422A (en) * 2011-01-17 2011-10-05 深圳市圣龙特电子有限公司 Nano copper powder for electronic paste and preparation process
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste
US20180200801A1 (en) * 2016-05-18 2018-07-19 Shenzhen Guohua Optoelectronics Co., Ltd. Preparation Method for the Nano-silver Particles
CN111168083A (en) * 2020-02-24 2020-05-19 深圳先进技术研究院 A kind of preparation method of nano silver powder
CN111992738A (en) * 2020-09-19 2020-11-27 西安瑞特三维科技有限公司 Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090023007A1 (en) * 2004-02-10 2009-01-22 Mitsui Mining & Smelting Co., Ltd. Highly crystalline silver powder and method for producing the same
US20070275259A1 (en) * 2006-05-25 2007-11-29 Samsung Electro-Mechanics Co., Ltd. Method of producing metal nanoparticles and metal nanoparticles produced thereby
CN102205422A (en) * 2011-01-17 2011-10-05 深圳市圣龙特电子有限公司 Nano copper powder for electronic paste and preparation process
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste
US20180200801A1 (en) * 2016-05-18 2018-07-19 Shenzhen Guohua Optoelectronics Co., Ltd. Preparation Method for the Nano-silver Particles
CN111168083A (en) * 2020-02-24 2020-05-19 深圳先进技术研究院 A kind of preparation method of nano silver powder
CN111992738A (en) * 2020-09-19 2020-11-27 西安瑞特三维科技有限公司 Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LIN CAO等: "The Preparation of Ag Nanoparticle and Ink Used for Inkjet Printing of Paper Based Conductive Patterns", 《MATERIALS》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117921016A (en) * 2023-04-03 2024-04-26 北京机科国创轻量化科学研究院有限公司 A method for preparing nano-scale ultrafine silver powder of photovoltaic silver paste

Similar Documents

Publication Publication Date Title
CN103658675B (en) Copper nanowire and preparation method thereof
CN110355380B (en) Preparation method of hexagonal flaky micron-crystal silver powder
CN101880493B (en) Method for preparing nano copper conductive ink
CN101077529B (en) A kind of preparation method of nanometer copper powder and copper paste
CN104096850B (en) The method that silver ammonia complex prepares superfine spherical silver powder is reduced with para-aminophenol
CN104263082A (en) Graphene organic silver conductive printing ink and preparation method thereof
CN102493265B (en) Method for preparing metal nano particle and cellulose fiber composite material
CN114029499B (en) Preparation method of ultralong nano silver wire material
CN107716944B (en) The method that chemical method prepares nano-grade silver powder
CN111922358B (en) Method for synthesizing nano silver with controllable morphology by reduction at normal temperature
CN103008679A (en) Method for preparing nano-silver particle and nano-silver wire mixed conductive ink
CN104815990A (en) Method for preparing nanometer sliver colloid with liquid phase reduction method
TW202302774A (en) Nano-metal 3D printing ink and application thereof
CN104845449A (en) Preparation and application of RFID antenna-based inkjet conductive ink
CN103042230A (en) Preparation method for micron spherical silver powder for electronic paste
CN114054769B (en) Silver micro powder and preparation method and application thereof
CN106077704A (en) A kind of ultra-long silver nanowire and its preparation method and application
CN112705726A (en) Preparation method of shape-controllable nano silver powder
CN106366769A (en) Anti-oxidative nano-copper conductive ink, and preparation method and printing application
CN106564937A (en) Preparation method of antimony-doped nanometer tin oxide (ATO) powder
CN113649558B (en) Nano silver wire and preparation method thereof
CN105788756B (en) A kind of transparent metal conducting film and preparation method thereof
CN109822106A (en) A kind of preparation method and applications of flake silver powder
CN102118918A (en) Flexible transparent electronic circuit and preparation method thereof
CN111001820B (en) Nano silver wire and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20210427