[go: up one dir, main page]

CN110860699A - Method for preparing silver nanowires at low cost and application thereof - Google Patents

Method for preparing silver nanowires at low cost and application thereof Download PDF

Info

Publication number
CN110860699A
CN110860699A CN201911161258.9A CN201911161258A CN110860699A CN 110860699 A CN110860699 A CN 110860699A CN 201911161258 A CN201911161258 A CN 201911161258A CN 110860699 A CN110860699 A CN 110860699A
Authority
CN
China
Prior art keywords
mother liquor
silver nanowires
silver
reaction
low cost
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.)
Withdrawn
Application number
CN201911161258.9A
Other languages
Chinese (zh)
Inventor
王杰
徐少晨
徐志
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to CN201911161258.9A priority Critical patent/CN110860699A/en
Publication of CN110860699A publication Critical patent/CN110860699A/en
Withdrawn legal-status Critical Current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
    • B22F1/0547Nanofibres or nanotubes
    • 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
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • 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

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

Abstract

A preparation method of low-cost silver nanowires comprises the following steps of, firstly, collecting dark green mother liquor after preparing silver nanowires by a polyol method, adding water absorbent particles into the dark green mother liquor, and then fully stirring the mixture to ensure that the water in the reaction mother liquor is fully absorbed; step two, after the absorption in the step one is finished, filtering reaction mother liquor, heating to a certain temperature, and then directly adding a proper amount of silver source and surfactant into the reaction mother liquor; and thirdly, transferring the mixed solution in the second step into a hydrothermal reaction kettle, and reacting for a period of time at a proper temperature to realize the preparation of the low-cost silver nanowire.

Description

Method for preparing silver nanowires at low cost and application thereof
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to a preparation method and application of silver nanowires.
Background
The silver nanowire is a typical one-dimensional noble metal nanowire which has excellent optical, electrical, flexibility and thermal properties, and is a noble metal nano material mainly researched at present with the copper nanowire and the gold nanowire. Compared with copper nanowires, silver nanowires have good stability, are not easily oxidized by air, and are beneficial to wide application; compared with gold nanowires, gold nanowires are not prepared on a large scale as silver nanowires or copper nanowires at present because the preparation process of gold nanowires is complex and the yield is always low. Therefore, silver nanowires are a novel functional material most likely to be practical in noble metal nanowires.
At present, the application research of silver nanowires mainly focuses on the field of optoelectronics, such as the preparation of transparent conductive electrodes; the field of intelligent wearable equipment, such as electronic skin, ultrasensitive physiological detectors and the like; the electric heating field, such as heating film, defogging film, etc. and fuel cell catalyst.
The preparation method of silver nano-wire mainly includes hydrothermal method, microwave auxiliary method, ultraviolet reduction method, hard template method and electrochemical deposition method, among them, the polyol method proposed by professor of summer boy of university of california rational engineering is a method which is currently very widely applied, this method mainly uses polyol (such as ethylene glycol, glycerol, etc.) as solvent, through adding metal salt (such as silver nitrate), depending on the reducibility of polyol to reduce it into elementary substance nano-particles, the precipitation process of these nano-particles will produce super-symmetrical cubic structure unit cells, these unit cells as the seeds of growing nano-wire are dispersed in the solution, then by the action of surfactant, and further grow along a certain specific direction, thus get oriented growth nano-material, for example, polyvinylpyrrolidone is often added as surfactant in the above-mentioned reaction, the silver nanoparticle has a selective passivation effect, has a strong coating effect on the { 100 } crystal face group of the silver nanoparticle, and has a weak coating effect on the { 111 } crystal face group, so that the silver nanoparticle added with polyvinylpyrrolidone can continue to grow along the { 111 } crystal face group.
In the above method, the general process flow is as described above, but the inventor found a serious problem in using the method, that is, after the reaction is finished, the silver nanowires are washed from the mother liquor by centrifugation and then the mother liquor is directly poured out. In the process, the reaction mother liquor is greatly wasted, meanwhile, the poured reaction mother liquor also contains a large amount of available substances, and if the method is used for scale production, the pressure on subsequent wastewater treatment is also high, and the requirement of current recyclable development is not met.
Therefore, the invention aims to solve the problems, realize the emission reduction of the mother solution in the preparation process of the silver nanowires and reduce the cost for preparing the silver nanowires, and particularly provides the patent application of the invention.
Prior art documents:
patent documents:
1、CN102328095A;
2、CN103201061A;
3、CN103203467A;
4、US2009196788A1;
study literature:
1、On the polyol synthesis of silver nanostructures: glycolaldehyde as areducing agent,《Nano Lett》;
2、Crystalline silver nanowires by soft solution processing,《Nano Lett》;
3、Large-Scale Synthesis of Uniform Silver Nanowires Through a Soft, Self-Seeding,《Adv. Mater》;
4、Large-scale synthesis and characterization of very long silvernanowires via successive multistep growth,《Cryst. Growth Des》。
disclosure of Invention
The invention aims to provide a low-cost preparation method of silver nanowires, which can be used for preparing the silver nanowires and reducing the preparation cost of the silver nanowires on one hand by realizing the repeated recycling of reaction mother liquor; on the other hand, the method fully utilizes useful substances in the mother liquor, reduces the amount of waste liquor, lightens the subsequent production pressure, is a green production mode, and in a word, the production method provided by the invention can achieve the effect of achieving multiple purposes and has good practical value.
In order to make the technical solution of the present invention apparent to those skilled in the art, the technical solution of the present invention will now be described in detail as follows.
A preparation method of low-cost silver nanowires comprises the following steps:
firstly, collecting dark green mother liquor after preparing silver nanowires by a polyol method, adding water absorbent particles into the dark green mother liquor, and fully stirring the mixture to ensure that the water absorbent particles fully absorb water in reaction mother liquor;
step two, after the absorption in the step one is finished, filtering reaction mother liquor, heating to a certain temperature, and then directly adding a proper amount of silver source and surfactant into the reaction mother liquor;
and thirdly, transferring the mixed solution in the second step into a hydrothermal reaction kettle, and reacting for a period of time at a proper temperature to realize the preparation of the low-cost silver nanowire.
Further, the dark green mother liquor in the first step of the present invention refers to a mother liquor obtained after silver nanowires are separated out by using deionized water or ethanol in the preparation of polyol.
Further, the adsorbent particles according to the first aspect of the present invention refer to a polymeric water absorbent or a molecular sieve water absorbent.
Furthermore, the certain temperature in the second step of the invention is 40-60 ℃, which can reduce the viscosity of the polyol and is beneficial to the dissolution of the silver salt and the surfactant.
Furthermore, the silver source in the second step of the invention is one of nitrate and silver acetate; the surfactant is polyvinylpyrrolidone; wherein the adding mass ratio of the silver salt to the surfactant is 1: 2-3.
Furthermore, the hydrothermal reaction temperature in the third step of the invention is 120-150 ℃, and the reaction time is 12-24 h.
After the reaction is finished, the reaction kettle is opened after the reaction kettle is naturally cooled to room temperature, the reaction solution is earthy yellow, and after washing and centrifugal analysis, it can be seen that the previous reaction mother liquor is used as a raw material to continue the reaction, and the silver nanowires can be successfully prepared only by adding a proper amount of silver source and surfactant, so that the reaction cost can be obviously reduced compared with the method of directly using a new solvent.
The silver nanowire prepared by the method can be used for preparing conductive ink, and has good conductive performance.
Compared with the prior art, the invention has the following beneficial technical effects:
1) the mother liquor of the previous reaction is used as a reaction raw material to continue the reaction, so that the preparation of the low-cost silver nanowire is successfully realized, the dual effects of reducing the cost and discharging less waste are achieved, and the effect of achieving multiple purposes is achieved;
2) in the subsequent preparation process, only a silver source and a surfactant need to be added, and other substances do not need to be additionally added, so that the full utilization of useful substances in the reaction mother liquor is realized;
3) the product is analyzed, and the yield of the silver nanowire obtained by using the mother liquor reaction can reach more than 60 percent through calculation.
Drawings
FIG. 1 is an SEM photograph of low-cost silver nanowires prepared according to the present invention;
fig. 2 SEM photograph of low cost silver nanowires prepared by the present invention.
Detailed Description
In order to further fully illustrate the technical solutions of the present invention, the preferred embodiments of the present invention will now be described in detail with reference to the specific embodiments, but it should be noted that the description is only for further illustrating the features and advantages of the present invention, and is not intended to limit the claims of the present invention.
A preparation method of low-cost silver nanowires comprises the following steps:
firstly, collecting dark green mother liquor after preparing silver nanowires by a polyol method, adding water absorbent particles into the dark green mother liquor, and fully stirring the mixture to ensure that the water absorbent particles fully absorb water in reaction mother liquor;
step two, after the absorption in the step one is finished, filtering reaction mother liquor, heating to a certain temperature, and then directly adding a proper amount of silver source and surfactant into the reaction mother liquor;
and thirdly, transferring the mixed solution in the second step into a hydrothermal reaction kettle, and reacting for a period of time at a proper temperature to realize the preparation of the low-cost silver nanowire.
Example 1
Measuring 40mL of reaction mother liquor, adding a proper amount of high-molecular water absorbent into the reaction mother liquor, and repeatedly filtering for 3 times; and then heating the mixture to 40 ℃, adding 0.5g of silver nitrate and 1.0g of polyvinylpyrrolidone into the mixture, stirring the mixture to dissolve the silver nitrate and the polyvinylpyrrolidone, transferring the mixture into a 50mL reaction kettle, sealing the reaction kettle, placing the reaction kettle in a 120 ℃ oven to react for 20 hours, taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, and then washing and separating the reaction kettle to obtain the low-cost silver nanowire.
Example 2
Measuring 40mL of reaction mother liquor, adding a proper amount of molecular sieve water absorbent into the reaction mother liquor, and repeatedly filtering for 3 times; and then heating the mixture to 40 ℃, adding 0.5g of silver nitrate and 1.0g of polyvinylpyrrolidone into the mixture, stirring the mixture to dissolve the silver nitrate and the polyvinylpyrrolidone, transferring the mixture into a 50mL reaction kettle, sealing the reaction kettle, placing the reaction kettle in a 120 ℃ oven to react for 20 hours, taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, and then washing and separating the reaction kettle to obtain the low-cost silver nanowire.
Example 3
Measuring 40mL of reaction mother liquor, adding a proper amount of molecular sieve water absorbent into the reaction mother liquor, and repeatedly filtering for 3 times; and then heating the mixture to 40 ℃, adding 0.6g of silver nitrate and 1.5g of polyvinylpyrrolidone into the mixture, stirring the mixture to dissolve the silver nitrate and the polyvinylpyrrolidone, transferring the mixture into a 50mL reaction kettle, sealing the reaction kettle, placing the reaction kettle in a 130 ℃ oven to react for 22 hours, taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, and then washing and separating the reaction kettle to obtain the low-cost silver nanowire.
Example 4
Measuring 40mL of reaction mother liquor, adding a proper amount of molecular sieve water absorbent into the reaction mother liquor, and repeatedly filtering for 3 times; and then heating the mixture to 50 ℃, adding 0.6g of silver nitrate and 1.5g of polyvinylpyrrolidone into the mixture, stirring the mixture to dissolve the silver nitrate and the polyvinylpyrrolidone, transferring the mixture into a 50mL reaction kettle, sealing the reaction kettle, placing the reaction kettle in a drying oven at 140 ℃ for reacting for 19 hours, taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, and then washing and separating the reaction kettle to obtain the low-cost silver nanowire.
Example 5
Weighing 80mL of reaction mother liquor, adding a proper amount of molecular sieve water absorbent into the reaction mother liquor, and repeatedly filtering for 3 times; and then heating the silver nanowire to 45 ℃, adding 1.0g of silver nitrate and 2.0g of polyvinylpyrrolidone into the silver nanowire, stirring and dissolving the silver nanowire, transferring the silver nanowire into a 100mL reaction kettle, sealing the reaction kettle, placing the reaction kettle in a 120 ℃ oven for reaction for 24 hours, taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, and then washing and separating the reaction kettle to obtain the low-cost silver nanowire.
The above description is only an embodiment of the present invention, and the scope of the present invention is not limited thereto, and any technical solutions that fall within the spirit of the present invention should be included in the scope of the present invention.

Claims (8)

1. A preparation method of low-cost silver nanowires is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
firstly, collecting dark green mother liquor after preparing silver nanowires by a polyol method, adding water absorbent particles into the dark green mother liquor, and fully stirring the mixture to ensure that the water absorbent particles fully absorb water in reaction mother liquor;
step two, after the absorption in the step one is finished, filtering reaction mother liquor, heating to a certain temperature, and then directly adding a proper amount of silver source and surfactant into the reaction mother liquor;
and thirdly, transferring the mixed solution in the second step into a hydrothermal reaction kettle, and reacting for a period of time at a proper temperature to realize the preparation of the low-cost silver nanowire.
2. The method of claim 1 for preparing low cost silver nanowires, wherein: the dark green mother liquor in the first step is mother liquor obtained after silver nanowires are separated by using deionized water or ethanol in the preparation of polyhydric alcohol.
3. The method of claim 1 for preparing low cost silver nanowires, wherein: the adsorbent particles in the first step are referred to as a polymeric water absorbent or a molecular sieve water absorbent.
4. The method of claim 1 for preparing low cost silver nanowires, wherein: the certain temperature in the second step is 40-60 ℃.
5. The method of claim 1 for preparing low cost silver nanowires, wherein: the silver source in the second step is one of nitrate and silver acetate; the surfactant is polyvinylpyrrolidone; wherein the adding mass ratio of the silver salt to the surfactant is 1: 2-3.
6. The method of claim 1 for preparing low cost silver nanowires, wherein: the hydrothermal reaction temperature in the third step is 120-150 ℃, and the reaction time is 12-24 h.
7. Low cost silver nanowires prepared according to the method of any one of claims 1-6.
8. Use of low-cost silver nanowires according to claim 7, characterized in that it is used in the field of conductive inks.
CN201911161258.9A 2019-11-24 2019-11-24 Method for preparing silver nanowires at low cost and application thereof Withdrawn CN110860699A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911161258.9A CN110860699A (en) 2019-11-24 2019-11-24 Method for preparing silver nanowires at low cost and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911161258.9A CN110860699A (en) 2019-11-24 2019-11-24 Method for preparing silver nanowires at low cost and application thereof

Publications (1)

Publication Number Publication Date
CN110860699A true CN110860699A (en) 2020-03-06

Family

ID=69655914

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911161258.9A Withdrawn CN110860699A (en) 2019-11-24 2019-11-24 Method for preparing silver nanowires at low cost and application thereof

Country Status (1)

Country Link
CN (1) CN110860699A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024125168A1 (en) * 2022-12-13 2024-06-20 中国石油天然气股份有限公司 Method for preparing iridium nanocrystal

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104785794A (en) * 2015-05-12 2015-07-22 重庆文理学院 Making method for silver nanowire even in length-diameter ratio
CN105873700A (en) * 2013-12-31 2016-08-17 罗地亚经营管理公司 Processes for making silver nanostructures
CN105934297A (en) * 2014-01-20 2016-09-07 公立大学法人滋贺县立大学 Silver nanowire production method
CN110270693A (en) * 2019-07-12 2019-09-24 刘松青 A kind of silver nanowires continuous producing method that solvent recovery cycle utilizes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105873700A (en) * 2013-12-31 2016-08-17 罗地亚经营管理公司 Processes for making silver nanostructures
CN105934297A (en) * 2014-01-20 2016-09-07 公立大学法人滋贺县立大学 Silver nanowire production method
CN104785794A (en) * 2015-05-12 2015-07-22 重庆文理学院 Making method for silver nanowire even in length-diameter ratio
CN110270693A (en) * 2019-07-12 2019-09-24 刘松青 A kind of silver nanowires continuous producing method that solvent recovery cycle utilizes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024125168A1 (en) * 2022-12-13 2024-06-20 中国石油天然气股份有限公司 Method for preparing iridium nanocrystal

Similar Documents

Publication Publication Date Title
CN100515952C (en) A kind of preparation method of copper sulfide hollow sphere
CN108892130A (en) The green synthesis method of graphene quantum dot is prepared using starch
CN103754837B (en) Utilize porous bismuth oxide for the method for Template preparation bismuth-containing nano-hollow ball
CN104785266B (en) A kind of preparation method of nano-cobaltic-cobaltous oxide/graphene composite material
CN101372330A (en) A method of coating carbon nanotubes with metal-doped zinc oxide nanoparticles
CN105478795B (en) A kind of method that silver nano-grain is prepared using sugarcane extract
Qi et al. One-dimensional CuS microstructures prepared by a PVP-assisted microwave hydrothermal method
CN106398397A (en) Method for preparing monodisperse graphene based nano silver composite
CN103111307A (en) Preparation method of graphene supported nickel/platinum core-shell nano compound
CN103042230A (en) Preparation method for micron spherical silver powder for electronic paste
CN107413354A (en) A kind of preparation method for the cupric oxide nano composite for loading silver
CN107555470A (en) A kind of method of two-step method synthesis zinc cadmium sulphur solid-solution material
CN104625082B (en) Nanometer nickel powder preparation method
CN114029499A (en) A kind of preparation method of ultra-long nano silver wire material
CN101613121A (en) A kind of preparation method of ellipsoidal zinc oxide
CN106540711A (en) A kind of method that green prepares Ag-ZnO grapheme foam nickel material
CN105562711B (en) A kind of preparation method of nano silver wire
CN101161338B (en) Graphite oxide loaded with Cu2O microparticles and its preparation method
CN110860699A (en) Method for preparing silver nanowires at low cost and application thereof
CN104986802A (en) Platy nanometer material and preparation method thereof
CN106540716A (en) A kind of preparation method and application of nano material CuS/Ni
CN100560503C (en) Preparation method of hollow multi-level copper oxide nanomaterial
CN107297510A (en) Method for preparing nano-scale silver particle powder by reducing silver salt intermediate in grading manner
CN108994315A (en) Method for preparing silver nanowire material by using carrageenan as template and reducing agent
CN105036092B (en) Preparation method of spherical silver selenide particles

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
WW01 Invention patent application withdrawn after publication

Application publication date: 20200306

WW01 Invention patent application withdrawn after publication