CN103059492A - Preparation method for silver (Ag)/polymethyl methacrylate (PMMA) nanocomposite material with high Ag content - Google Patents
Preparation method for silver (Ag)/polymethyl methacrylate (PMMA) nanocomposite material with high Ag content Download PDFInfo
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- CN103059492A CN103059492A CN2012105880808A CN201210588080A CN103059492A CN 103059492 A CN103059492 A CN 103059492A CN 2012105880808 A CN2012105880808 A CN 2012105880808A CN 201210588080 A CN201210588080 A CN 201210588080A CN 103059492 A CN103059492 A CN 103059492A
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Abstract
The invention relates to a preparation method for a silver (Ag)/polymethyl methacrylate (PMMA) nanocomposite material with high Ag content, controllable grain size and content of nanosilver and uniformly distributed nanosilve. The method comprises the following steps: (1) pouring nanosliver seed solution into a high-temperature dimethyl formamide (DMF)/PMMA/polyvinyl pyrrolidone (PVP) mixed system and reacting at high temperature to prepare Ag/PMMA nanocomposite sol; and (2) coating the Ag/PMMA nanocomposite sol on a base plate, performing vacuum drying at low temperature and removing the DMF to obtain the Ag/PMMA nanocomposite material. The preparation method has the following advantages: (1) the high-content nanosilver is uniformly dispersed into the PMMA matrix and the grain size and the content are controllable; (2) the reducing rate of silver ions is improved and the nanosliver with uniform grain size is generated; (3) vacuum drying is performed at low temperature, so aggregation and growth of the nanosilver are prevented in the drying process; and (4) the PMMA with high molecular weight is selected as a raw materials, so the prepared composite material has high performance.
Description
Technical field
The present invention relates at the synthetic metal nanoparticle of polymkeric substance environment situ, be used for the preparation method of the Ag/PMMA nano composite material of the controlled and high Ag content that is evenly distributed in polymer based nanocomposites field, particularly a kind of nanometer silver particle diameter and content.
Background technology
Character nontoxic, sterilization that nanometer silver not only has, have the good Nonlinear Third-Order Optical Properties, thermal property and the electromagnetic property that are different from the respective masses material, so that nano silver composite material not only has high thermal conductivity, high conductivity, also have higher surfactivity and catalytic performance, therefore the research of nano silver composite material has caused widely concern in recent years, and nanometer silver-polymer matrix composite also will become the important materials of using future in the fields such as photoelectricity, catalysis and biological chemistry.Aspect the Ag/PMMA nano composite material, because it has the excellent performance such as the non-linear absorption of optics, the electroconductibility of electricity, biomedical sterilization, in optics, electricity, and the aspect such as biomedical all has a wide range of applications.
Will be with the Ag/PMMA nanocomposite applications in electricity and photoelectricity field, gordian technique is to realize filling, the control of particle diameter and the even distribution of particle of high-content nanometer silver in PMMA.Yet the high surface of nanometer silver can cause the nanometer silver of high-content to be reunited in PMMA, so that distribution and particle diameter are uncontrollable, can't produce a desired effect.Being combined with of in-situ synthesis and pyroreaction condition can solve above-mentioned difficulties, and (1) the pyroreaction condition that it is advantageous that can improve Ag greatly
+Rate of reduction, a large amount of nano-Ag particles generate rapidly, simultaneously with small particle size distribution in the PMMA system, thereby can embody best and keep the peculiar property of nanometer silver; (2) nanometer silver and PMMA mix with other form of molecular level, nearly all remain on when nanometer silver is reduced on the position of oneself, have simultaneously the complexing action of dispersion agent PVP and nanometer silver, make the dispersion of nanometer silver highly even; (3) doping content is easily controlled, and the content of nanometer silver of doping is simply determined by the Silver Nitrate amount that adds.Therefore at high temperature adopt in-situ synthesis to make the preparation of the Ag/PMMA nano composite material of high silver content become possibility.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method of simple and feasible is provided, prepares high silver content Ag/PMMA nano composite material, to satisfy the Ag/PMMA nano composite material in the application in electricity and photoelectricity field.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of the Ag/PMMA nano composite material of high Ag content provided by the invention, a kind of with N, dinethylformamide (DMF) is solvent and reductive agent, Silver Nitrate is the Ag source, polymethylmethacrylate (PMMA) is polymeric matrix, Polyvinylpyrolidone (PVP) (PVP) is dispersion agent, adopts the method that may further comprise the steps:
(1) preparation of the nano combined colloidal sol of high Ag content Ag/PMMA:
To dissolve AgNO
3DMF solution join by a certain percentage in the DMF/PMMA/PVP mixed system, obtained the nano combined colloidal sol of described Ag/PMMA in 3 ~ 30 minutes through pyroreaction, the mass ratio of contained nanometer silver and PMMA is 1:(10 ~ 2.5 in the colloidal sol);
(2) preparation of high Ag content Ag/PMMA nano composite material:
The nano combined colloidal sol of Ag/PMMA is coated on the substrate, places freeze drying box low-temperature vacuum drying desolventizing DMF, obtain described Ag/PMMA nano composite material;
Through above-mentioned steps, realize the Ag/PMMA Nano-composite materials that nanometer silver particle diameter and content are controlled and be evenly distributed.
In step (1), can AgNO will have been dissolved
3DMF solution join in the DMF/PMMA/PVP mixed system by the volume ratio of 1:5.
Described PMMA is high molecular PMMA, and its molecular-weight average can be 250,000 ~ 350,000.
Described Ag
+Concentration in DMF can be controlled at 2.4mM/L ~ 48mM/L.
The content of described nanometer silver in PMMA can be 10wt.% ~ 40wt.%.
Described pyroreaction temperature can be 140 ℃ ~ 160 ℃.
Can utilize 0 ℃ ~ 20 ℃ lower dryings of freeze drying box vacuum to make described matrix material.
Described substrate can be quartz glass substrate.
The nano-Ag particles of described small particle size is synthetic at PMMA matrix situ, by AgNO in adjusting reaction time, the reaction system
3With the quality of PMMA AgNO when
3With the concentration ratio of DMF, obtain high dispersive Ag/PMMA nano composite material, synthetic nanometer silver size distribution is that 2nm-20nm is controlled, pattern is spherical.
The present invention compared with prior art has advantages of following main:
1. adopt high temperature (140 ~ 160 ℃) as temperature of reaction, improve Ag
+Rate of reduction so that the nanometer silver of 10wt.% ~ 40wt.% generates simultaneously, be conducive to obtain uniform small particle size (2 ~ 20nm) nano-Ag particles in PMMA;
2. utilize at low temperatures (0 ~ 20 ℃) dry preparation Ag/PMMA nano composite material of freeze drying box, effectively stop nanometer silver further growing up and reunites the polymolecularity of assurance high-content nanometer silver in matrix material in drying process;
3. one-step synthesis, technique is simple, is beneficial to popularization, is particularly suitable for the preparation of the Ag/PMMA nano composite material of high Ag content.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the device sketch of the nano combined colloidal sol preparation of Ag/PMMA among the present invention.
Fig. 3 is the Ag/PMMA colloidal sol ultraviolet-visible absorption spectroscopy figure of example 1-4 of the present invention.
Fig. 4 be in the Ag/PMMA matrix material of example 1 of the present invention nanometer silver the FE-SEM photo.
Fig. 5 be in the Ag/PMMA matrix material of example 3 of the present invention nanometer silver the FE-SEM photo.
Fig. 6 is the TEM photo of nanometer silver in the Ag/PMMA colloidal sol of example 5 of the present invention.
Fig. 7 is the TEM photo of nanometer silver in the Ag/PMMA colloidal sol of example 6 of the present invention.
Fig. 8 is the TEM photo of nanometer silver in the Ag/PMMA colloidal sol of example 7 of the present invention.
Among the figure: 1. prolong; 2. 150ml flask; 3. oil bath pan; 4. magneton; 5. heat collecting type constant-temperature heating magnetic stirring apparatus.
Embodiment
The present invention is to provide a kind of preparation method of Ag/PMMA nano composite material of high Ag content, with N, dinethylformamide (DMF) is solvent and reductive agent, Silver Nitrate is the Ag source, polymethylmethacrylate (PMMA) is polymeric matrix, Polyvinylpyrolidone (PVP) (PVP) is dispersion agent, referring to Fig. 1, specifically adopts the method that may further comprise the steps:
(1) preparation of the nano combined colloidal sol of Ag/PMMA of high Ag content:
To dissolve AgNO
3DMF solution join by a certain percentage in the DMF/PMMA/PVP mixed system of preparation, obtained the nano combined colloidal sol of Ag/PMMA in 3 ~ 30 minutes through pyroreaction, the mass ratio of Ag and PMMA is 1:(10 ~ 2.5);
(2) preparation of the Ag/PMMA nano composite material of high Ag content:
The nano combined colloidal sol of Ag/PMMA is coated on the substrate, places the freeze drying box low-temperature vacuum drying to go out solvent DMF, obtain the Ag/PMMA nano composite material.
The invention will be further described below in conjunction with embodiment and accompanying drawing, but be not limited to following described content.
Embodiment 1:
With 3.12gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
Under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 30min, stopped heating obtains Ag/PMMA colloidal sol.
The Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 10wt.% in the Ag/PMMA matrix material that the method obtains, its ultraviolet-visible spectrogram as shown in Figure 3, near 420nm absorption peak is the surface plasma resonance absorbtion peak of nanometer silver, and absorption peak is sharp-pointed, illustrates that the size distribution of nanometer silver is even.FE-SEM result as shown in Figure 4, visible nano-Ag particles is evenly distributed among the figure, particle diameter is about 20nm.
Embodiment 2:
1, with 1.56gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 15min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 20wt.% in the Ag/PMMA matrix material that the method obtains, its ultraviolet-visible spectrogram as shown in Figure 3, near 420nm absorption peak is the surface plasma resonance absorbtion peak of nanometer silver, and absorption peak is sharp-pointed, illustrates that the size distribution of nanometer silver is even.
Embodiment 3:
1, with 1.04gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 5min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 30wt.% in the Ag/PMMA matrix material that the method obtains, its ultraviolet-visible spectrogram as shown in Figure 3, near 420nm absorption peak is the surface plasma resonance absorbtion peak of nanometer silver, and absorption peak is sharp-pointed, illustrates that the size distribution of nanometer silver is even.FE-SEM result as shown in Figure 5, visible nano-Ag particles is evenly distributed among the figure, particle diameter is about 20nm.
Embodiment 4:
1, with 0.78gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 3min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 40wt.% in the Ag/PMMA matrix material that the method obtains, its ultraviolet-visible spectrogram as shown in Figure 3, near 420nm absorption peak is the surface plasma resonance absorbtion peak of nanometer silver, and absorption peak is sharp-pointed, illustrates that the size distribution of nanometer silver is even.
Embodiment 5:
1, with 0.78gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 1min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 40wt.% in the Ag/PMMA matrix material that the method obtains, TEM result as shown in Figure 6, visible nano-Ag particles is evenly distributed among the figure, particle diameter is about 2nm.
Embodiment 6:
1, with 0.78gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 5min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 40wt.% in the Ag/PMMA matrix material that the method obtains, TEM result as shown in Figure 7, visible nano-Ag particles is evenly distributed among the figure, particle diameter is about 10nm.
Embodiment 7:
1, with 0.78gPMMA(M=300,000), 50mlDMF and 0.32gPVP(M=40,000) put into reaction vessel, under 156 ℃ of heating conditions, be stirred to whole dissolvings.Again with 0.4896gAgNO
3Mix at normal temperatures AgNO with 10mlDMF
3All dissolving forms the nanometer silver seed solution.
2, under mechanical stirring and oil bath heating condition the nanometer silver seed solution is poured in the DMF/PMMA/PVP mixed system, behind high temperature (156 ℃) the reaction 10min, stopped heating obtains Ag/PMMA colloidal sol.
3, the Ag/PMMA colloidal sol for preparing evenly is coated on the substrate of handling well, places freeze drying box to remove DMF 0 ℃ of lower vacuum-drying, obtain the Ag/PMMA nano composite material.
Content of nanometer silver is 40wt.% in the Ag/PMMA matrix material that the method obtains, TEM result as shown in Figure 8, visible nano-Ag particles is evenly distributed among the figure, particle diameter is about 15nm.
In above-described embodiment, can adopt device as shown in Figure 2 to prepare the nano combined colloidal sol of Ag/PMMA.This device is existing installation, and it mainly is comprised of prolong 1,150ml flask 2, oil bath pan 3, magneton 4 and heat collecting type constant-temperature heating magnetic stirring apparatus 5.
Claims (8)
1. the preparation method of the Ag/PMMA nano composite material of a high Ag content is characterized in that take DMF as solvent and reductive agent, Silver Nitrate is the Ag source, polymethylmethacrylate is polymeric matrix, and Polyvinylpyrolidone (PVP) is stablizer, adopts the method that may further comprise the steps:
(1) preparation of the nano combined colloidal sol of high Ag content Ag/PMMA:
To dissolve AgNO
3DMF solution join by a certain percentage in the DMF/PMMA/PVP mixed system, obtained the nano combined colloidal sol of described Ag/PMMA in 3 ~ 30 minutes through pyroreaction, the mass ratio of contained nanometer silver and PMMA is 1:(10 ~ 2.5 in the colloidal sol); Described DMF, PMMA and PVP are respectively the english abbreviations of DMF, polymethylmethacrylate, Polyvinylpyrolidone (PVP);
(2) preparation of high Ag content Ag/PMMA nano composite material:
The nano combined colloidal sol of Ag/PMMA is coated on the substrate, places freeze drying box low-temperature vacuum drying desolventizing DMF, obtain described Ag/PMMA nano composite material.
2. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1 is characterized in that: will dissolve AgNO
3DMF solution join in the DMF/PMMA/PVP mixed system by the volume ratio of 1:5.
3. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1, it is characterized in that: described PMMA is high molecular PMMA, its molecular-weight average is 250,000 ~ 350,000.
4. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1 is characterized in that: Ag
+Concentration in DMF is controlled at 2.4mM/L ~ 48mM/L.
5. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1, it is characterized in that: the content of nanometer silver in PMMA is 10wt.% ~ 40wt.%.
6. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1, it is characterized in that: described pyroreaction temperature is 140 ℃ ~ 160 ℃.
7. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1 is characterized in that: utilize 0 ℃ ~ 20 ℃ lower dryings of freeze drying box vacuum to make described matrix material.
8. the preparation method of high Ag content Ag/PMMA nano composite material as claimed in claim 1, it is characterized in that: described substrate is quartz glass substrate.
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| CN103995104A (en) * | 2014-04-17 | 2014-08-20 | 广东工业大学 | Protein sensing membrane, and making method and use thereof |
| CN104588645A (en) * | 2015-02-04 | 2015-05-06 | 山西大学 | Silver nanometer cluster compound with antibacterial activity and preparation method thereof |
| CN105108168A (en) * | 2015-09-08 | 2015-12-02 | 北京印刷学院青岛研究院有限公司 | Preparation method of nano-silver particle coated by novel macromolecule protective agent |
| CN107000065A (en) * | 2014-12-26 | 2017-08-01 | 昭和电工株式会社 | The manufacture method of nano silver wire, the nano silver wire obtained by this method and the ink containing the nano silver wire |
| CN111467247A (en) * | 2020-04-24 | 2020-07-31 | 中国人民解放军总医院 | Preparation method of nano-silver/PMMA (polymethyl methacrylate) denture base composite material |
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| CN114918424A (en) * | 2022-05-18 | 2022-08-19 | 浙江海钛新材料科技股份有限公司 | Method and device for efficiently preparing low-temperature nano silver paste from silver formate |
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| CN103995104A (en) * | 2014-04-17 | 2014-08-20 | 广东工业大学 | Protein sensing membrane, and making method and use thereof |
| CN107000065A (en) * | 2014-12-26 | 2017-08-01 | 昭和电工株式会社 | The manufacture method of nano silver wire, the nano silver wire obtained by this method and the ink containing the nano silver wire |
| CN107000065B (en) * | 2014-12-26 | 2019-12-27 | 昭和电工株式会社 | Method for producing silver nanowire, silver nanowire obtained by the method, and ink containing the silver nanowire |
| CN104588645A (en) * | 2015-02-04 | 2015-05-06 | 山西大学 | Silver nanometer cluster compound with antibacterial activity and preparation method thereof |
| CN105108168A (en) * | 2015-09-08 | 2015-12-02 | 北京印刷学院青岛研究院有限公司 | Preparation method of nano-silver particle coated by novel macromolecule protective agent |
| CN111467247A (en) * | 2020-04-24 | 2020-07-31 | 中国人民解放军总医院 | Preparation method of nano-silver/PMMA (polymethyl methacrylate) denture base composite material |
| CN113234351A (en) * | 2021-05-10 | 2021-08-10 | 深圳市凌普鑫科技有限公司 | Water-based organic nano ink applied to organic thin film device and preparation method |
| CN114918424A (en) * | 2022-05-18 | 2022-08-19 | 浙江海钛新材料科技股份有限公司 | Method and device for efficiently preparing low-temperature nano silver paste from silver formate |
| CN115850544A (en) * | 2022-12-21 | 2023-03-28 | 浙江工业大学 | Ag @ PMMA nanocomposite material, preparation method thereof and preparation method of PVDF-based dielectric composite material |
| CN115850544B (en) * | 2022-12-21 | 2023-10-20 | 浙江工业大学 | Ag@PMMA nanocomposite, preparation method thereof and preparation method of PVDF-based dielectric composite |
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Application publication date: 20130424 |