CN104599862B - A kind of preparation method of polypyrrole/argentum nano composite material - Google Patents
A kind of preparation method of polypyrrole/argentum nano composite material Download PDFInfo
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- CN104599862B CN104599862B CN201510011314.6A CN201510011314A CN104599862B CN 104599862 B CN104599862 B CN 104599862B CN 201510011314 A CN201510011314 A CN 201510011314A CN 104599862 B CN104599862 B CN 104599862B
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- trisodium citrate
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- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 85
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 63
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 76
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000178 monomer Substances 0.000 claims abstract description 36
- 239000001509 sodium citrate Substances 0.000 claims abstract description 29
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 28
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 27
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 27
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims description 17
- 239000004332 silver Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 9
- 150000003233 pyrroles Chemical class 0.000 claims description 3
- 230000002045 lasting effect Effects 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 4
- 238000005406 washing Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 25
- 239000003990 capacitor Substances 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 8
- 239000011148 porous material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 16
- 239000002131 composite material Substances 0.000 description 13
- 229910052759 nickel Inorganic materials 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000002484 cyclic voltammetry Methods 0.000 description 6
- 206010011224 Cough Diseases 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000008240 homogeneous mixture Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Composite Materials (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
Abstract
The present invention relates to a kind of preparation method of polypyrrole/argentum nano composite material, pyrrole monomer is mixed into architectonical with silver nitrate solution, trisodium citrate aqueous solution is added dropwise under stirring, completion of dropping continues to stir 10 30min, 4 12h of reaction are carried out after ferric chloride aqueous solutionses are added dropwise again, after reaction terminates, suction filtration reaction solution, gained filter cake is washed 23 times with ethanol and deionized water successively, then dry, obtain being shaped as spherical or spherical polypyrrole/argentum nano composite material particle, its particle diameter is 100 250nm, aperture is 3 15nm, pore volume is 0.283 0.356cm3/g.The preparation method is not required to the equipment and instrument of costliness, and preparation method is simple, requires that relatively low, production cost is low to reaction environment.Polypyrrole/argentum nano composite material obtained by its preparation is as electrode material for super capacitor, and its specific capacitance performance and thermal stability are excellent.
Description
Technical field
The present invention relates to a kind of silver/polypyrrole nano composite material, particularly a kind of polypyrrole/argentum nano composite material
Preparation method.
Background technology
Ultracapacitor is a kind of between battery and a kind of new, efficient, practical green energy-storing dress of traditional capacitor
Put, it, can fast charging and discharging, Er Qieshou because having the advantage that conventional capacitor power density is big, rechargeable battery power density is high concurrently
Life is long, the warm limit for width of work, voltage Memorability are good, non-maintaining, generation of electricity by new energy, electric automobile, information technology, Aero-Space,
It is with a wide range of applications in the fields such as science and techniques of defence.
Polypyrrole (hereinafter referred to as PPy) Yin Qigao electrical conductivity, high environmental stability, synthesis technique be simple and environment
Friendly the features such as, its application field is directed not only to traditional conduction, field of photovoltaic materials, and in anti-corrosion, polymer battery, it is special
It is not that the fields such as biology sensor also show that wide application prospect.But utilize the marketization also face of the PPy electrochemical capacitances prepared
Face two problems, first, its capacity is smaller under the conditions of fast charging and discharging；Second, the stable circulation of conductive polymer electrodes
Property need further raising.Using composite as electrode material, the chief for raising each material and keep away that its is short, i.e., using so-called
" cooperative effect ", is conducive to improving the comprehensive electrochemical of material.
Metal/conducting polymer has important potential value in fields such as material, microelectronics, optics and chemical sensors.
The PPy and conducting metal Ag researchs for carrying out being compounded to form composite to improve polypyrrole electric conductivity have been reported, but
Its polypyrrole/argentum nano composite material formed possesses obvious core shell structure or silver particles synthesis is scattered uneven, for making
Effective utilization of active material in composite can be influenceed during for electrode material.
The content of the invention
Disperse the technical problem such as uneven in polypyrrole the invention aims to solving above-mentioned conducting metal silver to carry
For a kind of preparation method of polypyrrole/argentum nano composite material, in polypyrrole/argentum nano composite material obtained by the preparation method
Nano silver particles be dispersed in polypyrrole matrix, and significantly improve the electric conductivity of composite, make active material
More effectively utilize, the specific capacitance with preferable electric conductivity and Geng Gao can be used as electrode material for super capacitor application.
Technical scheme
A kind of preparation method of polypyrrole/argentum nano composite material, specifically includes following steps：
Silver nitrate and pyrrole monomer dissolving are formed into homogeneous mixed system in deionized water, continuing will be dense under stirring
Spend and be added thereto for 0.1-0.5mol/L trisodium citrate aqueous solution by 3-10mL/min speed, completion of dropping continues to stir
10-30min, then concentration is added thereto for 0.3-0.9mol/L ferric chloride aqueous solutionses by 3-10mL/min speed, control
Temperature processed is 0-10 DEG C of progress reaction 4-12h, and reaction terminates the reaction solution suction filtration of rear gained, the filter cake of gained successively with ethanol and
Deionized water is washed 2-3 times, and it is 60-80 DEG C of drying then to control temperature, that is, obtains polypyrrole/argentum nano composite material；
Above-mentioned silver nitrate used, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：
Pyrrole monomer：Trisodium citrate is 1:8-14:2.5-4；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1-3.
Polypyrrole/argentum nano composite material obtained by above-mentioned preparation method, it is shaped as spherical or spherical particle, its grain
Footpath is 100-250nm, and aperture is 3-15nm, and pore volume is 0.283-0.356cm3/ g, silver particles are dispersed in polypyrrole square
In battle array, specific capacitance is obviously improved than pure polypyrrole, polypyrrole/argentum nano composite material is made after working electrode, in 2mV/s
Test condition under, it can be deduced that, the contribution specific capacitance value of polypyrrole in the composite reaches 284.8- 350.3F/g.
Beneficial effects of the present invention
The preparation method of a kind of polypyrrole/argentum nano composite material of the present invention, due to being gathered in preparation process using in situ
Legal addition trisodium citrate, as the complexing agent of silver nitrate solution and the stabilizer of system, is effective uniform offer of silver particles
Ensure；The presence of trisodium citrate and silver nitrate plays certain inducing action, and lemon to the grown junction point of polypyrrole ion
Lemon acid trisodium has certain constraint as surfactant to the length of polypyrrole chain, spherical scattered to forming polypyrrole/silver
Particle has the good effect of cutting out；Silver improves the poly- pyrrole of final gained as dopant as good conducting metal simultaneously
Cough up/the electric conductivity of argentum nano composite material.
Further, polypyrrole/silver nanoparticle obtained by a kind of preparation method of polypyrrole/argentum nano composite material of the invention
Composite is shaped as spherical or spherical particle, and its particle diameter is 100-250nm, and particle diameter is 3-15nm, pore volume is
0.283-0.356cm3/ g, silver particles are dispersed in polypyrrole matrix, and specific capacitance is obviously improved than pure polypyrrole, will be poly-
Pyrroles/argentum nano composite material is made after working electrode, under 2mV/s test condition, it can be deduced that, polypyrrole is in composite wood
Contribution specific capacitance value in material reaches the F/g of 284.8- 350.3, therefore can be used as the electrode material of ultracapacitor.
Brief description of the drawings
Fig. 1, the gained polypyrrole of embodiment 1/argentum nano composite material SEM figures；
Fig. 2, the gained polypyrrole of embodiment 1/argentum nano composite material XRD spectrum；
Fig. 3, the gained polypyrrole of embodiment 1/argentum nano composite material cyclic voltammetry curve；
Fig. 4, the polypyrrole of the gained of comparative examples 1 SEM figures.
Embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of polypyrrole/argentum nano composite material, specifically includes following steps：
0.2123g silver nitrates and 1.005ml pyrrole monomers are dissolved in 200ml deionized waters and form homogeneous mixture
7.5ml concentration is added it for 0.5mol/L trisodium citrate aqueous solution by 3mL/min speed under system, lasting stirring
In, completion of dropping continue stir 20min, then by 50ml concentration for 0.3mol/L ferric chloride aqueous solutionses press 10mL/min speed
Rate is added thereto, and it is 0 DEG C of progress reaction 6h to control temperature, and reaction terminates the reaction solution suction filtration of rear gained, and the filter cake of gained is successively
Washed with ethanol and deionized water 3 times, it is 60 DEG C of drying then to control temperature, that is, obtains spherical or spherical polypyrrole/silver
Nano composite material；
Above-mentioned silver nitrate used, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：
Pyrrole monomer：Trisodium citrate is 1:12:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1.
Using Dutch PANalytical company X ' pert PW3040/60 to the spherical or spherical polypyrrole of above-mentioned gained/
Argentum nano composite material is measured, and its particle diameter is 100-250nm.
It is full-automatic than the spherical or class of surface and micropore analyzer to above-mentioned gained using Merck ＆ Co., Inc of U.S. ASAP2020
Spherical polypyrrole/argentum nano composite material is measured, and its aperture is 3-15nm, and its pore volume is 0.283cm3/g。
Using spherical or class of the Dutch FEI Co. Quanta 200FEG environmental scanning electron microscopes to above-mentioned gained
Spherical polypyrrole/argentum nano composite material is scanned, and the SEM of gained is schemed as shown in figure 1, polypyrrole/silver nanoparticle composite wood
Material shows scattered spherical structure, shows control effect of the application to particle morphology of silver nitrate and trisodium citrate.Using
Spherical or spherical poly- pyrroles of X-ray diffractometer X ' the pert Pro of Dutch PANalytical analytical instrument company to above-mentioned gained
Cough up/argentum nano composite material is measured, the XRD of gained is as shown in Fig. 2 from figure 2 it can be seen that the wherein θ of the angle of diffraction 2 exists
Peak between 20-30 ° is the diffraction maximum for belonging to polypyrrole, positioned at 2 θ=38.1 °, 44.3 °, 64.5 °, 77.3 °, 81.5 ° of point and
Sharp diffraction maximum is belonging respectively to (111), (200), (220) of argent, (311), the diffraction maximum of (222) crystal face, is indicated above
Material obtained by above-mentioned preparation method is the composite of polypyrrole and silver.
By polypyrrole/argentum nano composite material of above-mentioned gained according to polypyrrole/argentum nano composite material: conductive black:
Binding agent=65: the ratio of 25: 10 (mass ratioes) is well mixed, and is then coated on porous nickel conducting base, finally in normal temperature
Lower vacuum drying 10h is sweet with saturation using platinum electrode as auxiliary electrode using the porous nickel conducting base after drying as working electrode
Mercury electrode (SCE) is that reference electrode constitutes three-electrode system, and working media uses 1mol/L metabisulfite solutions, in Shanghai Chen Hua instrument
The CHI660d electrochemical workstations of device Co., Ltd carry out electrochemical capacitor performance to material using cyclic voltammetry and surveyed
Examination, under 2mV/s test condition, the cyclic voltammetry curve of gained is as shown in figure 3, from figure 3, it can be seen that above-mentioned poly- pyrrole
Cough up/argentum nano composite material is made after electrode, the contribution specific capacitance value of polypyrrole in the composite reaches 350.3F/g.
Comparative examples 1
1.005ml pyrrole monomers are dispersed in 200ml deionized waters, are by 50mL concentration under continued mechanical stirring
0.3mol/L ferric chloride aqueous solutionses are added thereto by 10mL/min speed, and it is 0 DEG C of progress reaction 8h, reaction to control temperature
Suction filtration after end, obtained filter cake is washed 3 times respectively with ethanol and deionized water successively, and it is 60 DEG C of bakings then to control temperature
It is dry, that is, obtain polypyrrole particle.
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1.
Using polypyrrole of the Dutch FEI Co. Quanta 200FEG environmental scanning electron microscopes to above-mentioned gained
Grain is scanned, and the SEM of gained figure is as shown in figure 4, polypyrrole build-up of particles is chain, the polypyrrole of situ aggregation method synthesis
Grain does not have well-regulated pattern.
Fig. 1 and Fig. 4 are contrasted, it can be seen that a kind of preparation side of polypyrrole/argentum nano composite material of the invention
In the presence of having silver nitrate and sodium citrate in method, preparation process, the shape of particle of gained is by inter-adhesive spherical
Chain-like aggregates become monodispersed spheroidal particle, are indicated above generation of the presence of silver nitrate and sodium citrate to polypyrrole
Play structure inducing action.
By the polypyrrole particle of above-mentioned gained according to polypyrrole particle: conductive black: binding agent=65: 25: 10 (mass ratioes)
Ratio be well mixed, then polypyrrole particle is coated on porous nickel conducting base, finally by electrode at normal temperatures vacuum dry
Dry 10h, using the porous nickel conducting base after drying as working electrode, using platinum electrode as auxiliary electrode, with saturated calomel electrode
(SCE) three-electrode system is constituted for reference electrode, working media uses 1mol/L metabisulfite solutions, limited in Shanghai Chen Hua instrument
The CHI660d electrochemical workstations of company carry out electrochemical capacitor performance test using cyclic voltammetry to material.
As a result show, above-mentioned polypyrrole particle is made after electrode, under 2mV/s test condition, the specific capacitance of polypyrrole
It is worth for 228.8F/g.
Contrasted by embodiment 1 and comparative examples 1, as a result show polypyrrole obtained by preparation method of the present invention/
Argentum nano composite material compared to polypyrrole in pattern with being improved a lot on chemical property, it is preferably to be used as super electricity
The electrode material of container.
Embodiment 2
A kind of preparation method of polypyrrole/argentum nano composite material, specifically includes following steps：
0.2123g silver nitrates and 0.650ml pyrrole monomers are dissolved in 200ml deionized waters and form homogeneous mixture
System, continues that 12.5ml concentration is pressed to 5mL/min speed addition under stirring for 0.3mol/L trisodium citrate aqueous solution
Wherein, completion of dropping continues to stir 20min, then the ferric chloride aqueous solutionses that 50ml concentration is 0.9mol/L are pressed into 5mL/min's
Speed is added thereto, and it is 5 DEG C of progress reaction 4h to control temperature, and reaction terminates the reaction solution suction filtration of rear gained, the filter cake of gained according to
Secondary to be washed with ethanol and deionized water 3 times, it is 60 DEG C of drying then to control temperature, that is, obtain spherical or spherical polypyrrole/
Argentum nano composite material；
Above-mentioned silver nitrate used, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：
Pyrrole monomer：Trisodium citrate is 1:8:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:3.
After measured, its particle diameter is 100- to spherical or spherical polypyrrole/argentum nano composite material of above-mentioned gained
250nm, aperture is 3-15nm, and pore volume is 0.356cm3/g。
By polypyrrole/argentum nano composite material of above-mentioned gained according to polypyrrole/argentum nano composite material: conductive black:
Binding agent=65: the ratio of 25: 10 (mass ratioes) is well mixed, and is then coated on porous nickel conducting base, finally in normal temperature
Lower vacuum drying 10h is sweet with saturation using platinum electrode as auxiliary electrode using the porous nickel conducting base after drying as working electrode
Mercury electrode (SCE) is that reference electrode constitutes three-electrode system, and working media uses 1mol/L metabisulfite solutions, in Shanghai Chen Hua instrument
The CHI660d electrochemical workstations of device Co., Ltd carry out electrochemical capacitor performance to material using cyclic voltammetry and surveyed
Examination, under 2mV/s test condition, above-mentioned polypyrrole/argentum nano composite material is made after electrode, and polypyrrole is in the composite
Contribution specific capacitance value reach 284.8F/g.
Embodiment 3
A kind of preparation method of polypyrrole/argentum nano composite material, specifically includes following steps：
0.2123g silver nitrates and 1.005ml pyrrole monomers are dissolved in 200ml deionized waters and form homogeneous mixture
System, continues that 37.5ml concentration is pressed to 10mL/min speed addition under stirring for 0.1mol/L trisodium citrate aqueous solution
Wherein, completion of dropping continues to stir 20min, then the ferric chloride aqueous solutionses that 50ml concentration is 0.6mol/L are pressed into 10mL/min's
Speed is added thereto, and it is 10 DEG C of progress reaction 12h to control temperature, and reaction terminates the reaction solution suction filtration of rear gained, the filter cake of gained
Washed 3 times with ethanol and deionized water successively, it is 60 DEG C of drying then to control temperature, that is, obtains spherical or spherical poly- pyrrole
Cough up/argentum nano composite material；
Above-mentioned silver nitrate used, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：
Pyrrole monomer：Trisodium citrate is 1:12:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:2.
After measured, its particle diameter is 100- to spherical or spherical polypyrrole/argentum nano composite material of above-mentioned gained
250nm, aperture is 3-15nm, and pore volume is 0.287cm3/g。
By polypyrrole/argentum nano composite material of above-mentioned gained according to polypyrrole/argentum nano composite material: conductive black:
Binding agent=65: the ratio of 25: 10 (mass ratioes) is well mixed, and is then coated on porous nickel conducting base, finally in normal temperature
Lower vacuum drying 10h is sweet with saturation using platinum electrode as auxiliary electrode using the porous nickel conducting base after drying as working electrode
Mercury electrode (SCE) is that reference electrode constitutes three-electrode system, and working media uses 1mol/L metabisulfite solutions, in Shanghai Chen Hua instrument
The CHI660d electrochemical workstations of device Co., Ltd carry out electrochemical capacitor performance to material using cyclic voltammetry and surveyed
Examination, under 2mV/s test condition, polypyrrole/argentum nano composite material is made after electrode, the tribute of polypyrrole in the composite
Offer specific capacitance value and reach 296.4F/g.
The above results show that changing generation and pattern of the length in reaction time to polypyrrole particle has certain regulation and control to make
With, and then polypyrrole particle is have impact on as the electrochemical properties of electrode material for super capacitor.
In summary, the preparation method of polypyrrole/argentum nano composite material obtained by the present invention, by adjusting in reactant
The mol ratio of silver nitrate, pyrrole monomer and citrate ion, ferric trichloride, and corresponding reaction time and temperature are controlled, most
Particle diameter is obtained eventually for 100-250nm, and aperture is 3-15nm, and pore volume is 0.283-0.356cm3/ g polypyrrole/silver nanoparticle is multiple
Condensation material, is made into after working electrode, under 2mV/s test condition, it can be deduced that, the tribute of polypyrrole in the composite
Offer specific capacitance value and reach 284.8-350.3F/g, therefore can be used as the electrode material of ultracapacitor.
Described above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, some improvement and modification can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of polypyrrole/argentum nano composite material, it is characterised in that comprise the following steps that：
Silver nitrate and pyrrole monomer dissolving are formed into homogeneous mixed system in deionized water, are by concentration under lasting stirring
0.1-0.5mol/L trisodium citrate aqueous solution is added thereto by 3-10mL/min speed, and completion of dropping continues to stir 10-
30min, then concentration is added thereto for 0.3-0.9mol/L ferric chloride aqueous solutionses by 3-10mL/min speed, control temperature
Spend for 0-10 DEG C of progress reaction 4-12h, reaction terminates the reaction solution suction filtration of rear gained, the filter cake of gained successively with ethanol and go from
Sub- water washing 2-3 times, it is 60-80 DEG C of drying then to control temperature, that is, obtains polypyrrole/argentum nano composite material；
Above-mentioned silver nitrate used, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：Pyrroles
Monomer：Trisodium citrate is 1:8-14:2.5-4；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1-3.
2. a kind of preparation method of polypyrrole/argentum nano composite material as claimed in claim 1, it is characterised in that nitre used
Sour silver, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：Pyrrole monomer：Trisodium citrate
For 1:8-12:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1-3.
3. a kind of preparation method of polypyrrole/argentum nano composite material as claimed in claim 2, it is characterised in that nitre used
Sour silver, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：Pyrrole monomer：Trisodium citrate
For 1:12:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:1.
4. a kind of preparation method of polypyrrole/argentum nano composite material as claimed in claim 2, it is characterised in that nitre used
Sour silver, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：Pyrrole monomer：Trisodium citrate
For 1:8:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:3.
5. a kind of preparation method of polypyrrole/argentum nano composite material as claimed in claim 2, it is characterised in that nitre used
Sour silver, pyrrole monomer, the amount of trisodium citrate aqueous solution, for calculation in the molar ratio, i.e. silver nitrate：Pyrrole monomer：Trisodium citrate
For 1:12:3；
The amount of ferric chloride aqueous solutionses used, for calculation in the molar ratio, i.e. pyrrole monomer：Ferric trichloride is 1:2.
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| CN108982624B (en) * | 2018-05-28 | 2020-03-24 | 桂林电子科技大学 | Polypyrrole @ ferrocene/gold nanoparticle composite material and preparation method and application thereof |
| CN111354513B (en) * | 2018-12-20 | 2021-12-28 | 南京理工大学 | Silver-doped polypyrrole-coated graphite composite material and preparation method thereof |
| US10526441B1 (en) | 2019-01-23 | 2020-01-07 | King Fahd University Of Petroleum And Minerals | Polypyrrole-coated silver particles for surface enhanced Raman scattering |
| CN113426425B (en) * | 2021-06-21 | 2022-12-23 | 西南科技大学 | Silver-based composite adsorbent for removing radioactive iodine and preparation method and application thereof |
| CN113845880A (en) * | 2021-09-29 | 2021-12-28 | 西安热工研究院有限公司 | Silver nanowire @ polypyrrole-ferroferric oxide composite wave-absorbing material and preparation method thereof |
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