CN101924202B - Single nanowire electrochemical device and assembly and in-situ characterization method thereof - Google Patents

Single nanowire electrochemical device and assembly and in-situ characterization method thereof Download PDF

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CN101924202B
CN101924202B CN2010102750216A CN201010275021A CN101924202B CN 101924202 B CN101924202 B CN 101924202B CN 2010102750216 A CN2010102750216 A CN 2010102750216A CN 201010275021 A CN201010275021 A CN 201010275021A CN 101924202 B CN101924202 B CN 101924202B
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electrochemical device
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single nanowire
wire
film
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CN101924202A (en
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麦立强
董亚杰
徐林
韩春华
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Wuhan chulijiana New Energy Technology Co.,Ltd.
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Wuhan University of Technology WUT
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Abstract

The invention relates to a single nanowire electrochemical device and an assembly and in-situ characterization method thereof. The method comprises the following steps of: dispersing nanowire anodes of vanadium oxide nanowires, and the like, nano film cathodes of HOPG (Highly Oriented Pyrolytic Graphite), and the like or nanowire cathodes of silicon nanowires, and the like and nano film anodes of LiCoO2, and the like on a substrate; respectively making metal electrodes at both ends of the nanowires and the nano films as current collectors by adopting technologies, such as PECVD (Plasma-Enhanced Chemical Vapor Deposition), and the like; then, depositing silicon nitride or spinning a photoresist on the metal current collectors as protection layers of the current collectors by adopting the PECVD technology, and the like; and finally, dispensing a polymer electrolyte on the surface of the substrate to finish the assembly of the single nanowire electrochemical device. In the invention, charging and discharging tests are carried out on the electrochemical device, then in-situ electrical transport performance tests, micro-domain Raman spectrum analysis, and the like are carried out on the single nanowire electrodes in different charging and discharging states, the direct relation among the electrical transport, the structure and the electrochemical performance of the nanowire electrode material is established, a platform is provided for battery diagnosis, and the like and a support power supply can be provided for the nano device.

Description

Single nanowire electrochemical device and assembling thereof, in-situ characterization method
Technical field
The invention belongs to nano material and technical field of electrochemistry, be specifically related to a kind of single nanowire electrochemical device and assembling thereof, in-situ characterization method.
Background technology
The specific capacity of lithium ion cell positive and negative material has determined the specific capacity of entire cell.All there are tangible capacity attenuation phenomenon in block or micron order electrode material in the battery charging and discharging cyclic process, but the nano line electrode material receives the concern in fields such as lithium ion battery, electrochemical device because of special anisotropy and favourable electric transmission.Therefore, the capacity attenuation essence and the modification of research nanowire battery material have great importance to the exploitation of high performance lithium ion battery, electrochemical device.
What at present the electrode of nano wire lithium ion battery used is nano wire powder or nano wire film mostly, and the research of single nano-wire lithium ion battery is not appeared in the newspapers.When studying lithium ion battery or electrochemical device both at home and abroad, need take or destroy battery and device apart when carrying out transmission electron microscope under the different charging and discharging states (TEM), high-resolution-ration transmission electric-lens (HRTEM), X-ray diffraction structural characterizations such as (XRD).In-situ characterization technology to lithium ion battery relates generally to nuclear magnetic resoance spectrum (NMR), and the in-situ characterization of material electronic transport performance is not appeared in the newspapers.Yet the in-situ characterization of the electronic transport of single nano-wire, structure and chemical property and inner link are rather important to suppressing battery material capacity attenuation, exploitation high performance lithium ion battery, electrochemical device etc.
Summary of the invention
The object of the invention proposes a kind of single nanowire electrochemical device and assembling thereof, in-situ characterization method to above-mentioned technical problem.
To achieve these goals, technical scheme of the present invention is single nanowire electrochemical device assembling and in-situ characterization, it is characterized in that work electrode is a single nano-wire, can carry out the in-situ characterization of electronic transport and structure to nano wire at different charging and discharging states.
A kind of single nanowire electrochemical device of the present invention is characterized in that, this electrochemical device work electrode is a single nano-wire, processes by following assemble method, and number of assembling steps is followed successively by:
1) will be such as nano wires such as vanadium oxide nanowires, lithium-barium oxide nano wire, lithium manganese oxide nano wire, lithium iron phosphate oxide nano wire positive pole with such as nano thin-film negative poles such as high order pyrolytic graphite sheets; Perhaps be dispersed in the silicon chip that there is the thick SiO2 of one deck 10～100nm on the surface, perhaps on dimethyl silicone polymer (PDMS) substrate etc. such as nano wire negative poles such as silicon nanowires, tin oxide nano-wires with such as nano thin-film positive poles such as lithium and cobalt oxides;
2) adopt electron beam lithography or other proper technologies to make Cr and Au, Ti and Al or other suitable metal electrodes as collector at the two ends of nano wire and nano thin-film respectively;
3) using plasma strengthens chemical vapour deposition (CVD) (PECVD), ald (ALD) or other proper technologies deposited silicon nitride or other suitable materials on metal collector and perhaps adopts photoetching or other proper technologies on metal collector, to prepare the protective layer of insulated photo-etching rubber (like SU8 etc.) as collector through spin coating or other proper technologies as the protective layer of collector;
4) will be such as LiClO 4, LiBF 4Or LiCF 3SO 3Deng lithium salts; With a kind of in PEO (PEO), polymethyl methacrylate (PMMA), polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), propene carbonate (PC), the ethylene carbonate (EC) or blend dissolving preparation polymer dielectric more than two kinds; Polymer dielectric is dripped the surface that is coated in substrate; After dry (like 40 ℃, 60 ℃ oven dry), promptly accomplish the assembling of single nanowire electrochemical device.
2. the in-situ characterization method of single nanowire electrochemical device comprises the steps:
1) battery is carried out cyclic voltammetric test and constant current, constant voltage charge-discharge test, battery was left standstill under different charging and discharging states 1 minute～1 hour, then single nano-wire electrode on the said substrate is carried out the electronic transport performance test of original position;
2) the described nano line electrode under the different charging and discharging states is carried out the original position structural characterization, like the microcell Raman spectrum analysis.
The invention has the beneficial effects as follows: the present invention proposes a kind of single nanowire electrochemical device and assembling thereof, in-situ characterization method; For structure, electronic transport and the chemical property correlation research of nanowire electrochemical device material, Battery Diagnostic etc. provide a kind of platform; Can explain the essence of electrochemical device capacity attenuation, and can be nano-device and provide support for power.
The assembling of single nanowire electrochemical device need not used conductive additive and binding agent among the present invention; The nano wire working electrode material forms good the contact with electrolyte; To electrode is the bigger film of area, and the chemical property that therefore records can reflect the intrinsic electrochemical behavior of nano wire.Electronic transport and structural characterization to nano wire all are to carry out in position, can truly reflect conductivity and the structural change of nano line electrode at different charging and discharging states, disclose the essence of material capacity decay, performance degradation.
Description of drawings
Fig. 1 is the structural representation of single nanowire electrochemical device;
Fig. 2 is the single V of embodiment 1 3O 7H 2The cyclic voltammetry curve of O nano wire;
Fig. 3 is the single V of embodiment 1 3O 7H 2The O nano wire is at the electronic transport performance curve of different charging and discharging states;
Wherein, (A) initial condition, (B) 100 skins were laid electricity 200 seconds, and (C) charging of 100 skins peace is 200 seconds, and (D) 100 skins were laid electricity 400 seconds, and (E) charging of 100 skins peace is 400 seconds;
Fig. 4 is the cyclic voltammetry curve of the single coaxial Si/a-Si nano wire of embodiment 2;
Fig. 5 is the electronic transport performance curve of the single coaxial Si/a-Si nano wire of embodiment 2 at different charging and discharging states.
Among the figure: 1-substrate, 2-nano line electrode, 3-polymer dielectric, the metal collector of 4-band protective layer, 5-nano-film electrode, the metal collector of 6-band protective layer.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
Embodiment 1:
The technical scheme of single nanowire electrochemical device assembling comprises the steps, carries out successively:
1) will adopt the V of Hydrothermal Preparation 3O 7H 2O nano wire positive pole and high order pyrolytic graphite sheet film negative pole are dispersed in the surface has the thick SiO of one deck 60nm 2Silicon chip on; Wherein, V 3O 7H 2The preparation method of O nano wire can be with reference to following document: H, Qiao, et al.Electrochem.Commun.8,21-26 (2006); Y.Oka, et al.J.Solid State Chem.89,372-377 (1990); High order pyrolytic graphite sheet film adopts the preparation of tear tape method, can be with reference to following document K.S.Novoselov, and et al.Science, 306,666-669 (2004);
2) adopt electron beam lithography to make Cr (5nm) and Au (80nm) metal electrode respectively at the two ends of described nano wire and nano thin-film as collector;
3) adopt the PECVD technology on metal collector, to deposit the protective layer of the thick silicon nitride of 500nm as collector;
4) with LiClO 4With PEO, and propene carbonate and ethylene carbonate (propene carbonate and ethylene carbonate mol ratio 1: 5) blend dissolving preparation polymer dielectric, LiClO 4Concentration is 1.0M, and polymer dielectric is dripped the surface that is coated in substrate, after 60 ℃ of oven dry, promptly accomplishes the assembling of single nanowire electrochemical device.
The technical scheme that the single nanowire electrochemical device in-situ characterization adopts comprises the steps, carries out successively:
1) battery is carried out cyclic voltammetric test and constant current charge-discharge test, battery was left standstill 5 minutes, under different charging and discharging states then to single V on the substrate 3O 7H 2The O nano line electrode carries out the electronic transport performance test of original position; Wherein, the equipment of electrical performance testing is following: Keithley 6220 characteristic of semiconductor analyzers provide constant-current source, and current precision reaches 100fA; The high internal resistance voltmeter of Trek 800 types measuring voltage, the voltmeter internal resistance is greater than 10 16Ohm; Adopt the electronic transport characteristic of Aligent4156C test nano wire; The probe station model is TTP-4.
2) to the single V under the different charging and discharging states 3O 7H 2The O nano line electrode carries out original position structural characterizations such as microcell Raman spectrum analysis.Wherein, the model of Raman spectrum analysis appearance is WITec CRM-200.
Embodiment 2:
The technical scheme that the single nanowire electrochemical device assembling is adopted comprises the steps, carries out successively:
1) with coaxial Si/a-Si nano wire negative pole and LiCoO 2The anodal dispersed deposition of film has the thick SiO of one deck 60nm on the surface 2Silicon chip on; Wherein, coaxial Si/a-Si nano wire adopts the chemical vapour deposition technique preparation, and the preparation method is with reference to following document: L.F.Cui, et al.Nano Lett., 9,491-495 (2009); LiCoO 2Film adopts the magnetron sputtering preparation, and film deposition conditions is: deposit 10 minutes, annealed 2.5 hours for 500 ℃;
2) adopt electron beam lithography to make Cr (5nm) and Au (80nm) metal electrode respectively at the two ends of nano wire and nano thin-film as collector;
3) adopt the PECVD technology on metal collector, to deposit the protective layer of the thick silicon nitride of 500nm as collector;
4) with LiClO 4With polymethyl methacrylate, and propene carbonate and ethylene carbonate (propene carbonate and ethylene carbonate mol ratio 1: 5) blend dissolving preparation polymer dielectric, LiClO 4Electrolyte concentration is 1.5M, and polymer dielectric is dripped the surface that is coated in substrate, after 60 ℃ of oven dry, promptly accomplishes the assembling of single nanowire electrochemical device.
The technical scheme that the single nanowire electrochemical device in-situ characterization adopts comprises the steps:
1) battery is carried out cyclic voltammetric test and constant current charge-discharge test, battery was left standstill under different charging and discharging states 5 minutes, then single coaxial Si/a-Si nano line electrode on the substrate is carried out the electronic transport performance test of original position; Wherein, the unit type of electrochemistry and electrical performance testing is with embodiment 1;
2) the single coaxial Si/a-Si nano line electrode under the different charging and discharging states is carried out original position structural characterizations such as microcell Raman spectrum analysis.Wherein, the model of Raman spectrum analysis appearance is WITec CRM-200.
Embodiment 3:
The technical scheme that the single nanowire electrochemical device assembling is adopted comprises the steps, carries out successively:
1) with β-AgVO 3Nano wire positive pole and high order pyrolytic graphite sheet book film negative pole are dispersed on the substrate of dimethyl silicone polymer (PDMS) insulation; Wherein, β-AgVO 3Nano wire adopts Hydrothermal Preparation, can be with reference to following document: L.Q.Mai, and et al.Nano Lett., 10,2604-2608 (2010); The preparation method of high order pyrolytic graphite sheet is with embodiment 1;
2) adopt electron beam lithography to make Ti (5nm) and Al (80nm) metal electrode respectively at the two ends of nano wire and nano thin-film as collector;
3) adopt photoetching technique on metal collector, to prepare the protective layer of the thick SU8 photoresist of 500nm as collector;
4) with LiBF 4With polyvinylidene fluoride, and propene carbonate and ethylene carbonate (propene carbonate and ethylene carbonate mol ratio 1: 1) blend dissolving preparation polymer dielectric, LiBF 4Electrolyte concentration is 1.2M, and polymer dielectric is dripped the surface that is coated in substrate, after 40 ℃ of oven dry, promptly accomplishes the assembling of single nanowire electrochemical device.
The technical scheme that the single nanowire electrochemical device in-situ characterization adopts comprises the steps:
1) battery is carried out cyclic voltammetric test and constant voltage charge-discharge test, battery was left standstill 1 hour, under different charging and discharging states then to single β-AgVO on the substrate 3Nano line electrode carries out the electronic transport performance test of original position; Wherein, the unit type of electrochemistry and electrical performance testing is with embodiment 1;
2) to the single β-AgVO under the different charging and discharging states 3Nano line electrode carries out original position structural characterizations such as microcell Raman spectrum analysis.Wherein, the model of Raman spectrum analysis appearance is WITec CRM-200.
Embodiment 4:
The technical scheme that the single nanowire electrochemical device assembling is adopted comprises the steps, carries out according to this:
1) with V 2O 5Nano wire positive pole and high order pyrolytic graphite sheet negative pole are dispersed in the surface has the thick SiO of one deck 10nm 2Silicon chip on; Wherein, adopt hydro thermal method or vapor phase method to prepare V 2O 5Nano wire can be with reference to following document: M.C.Wu, et al.J.Solid State Chem.182,2285-2289 (2009); J.Liu, et al.Sens.Actuators, B 115,481-487 (2006); The preparation method of high order pyrolytic graphite sheet is with embodiment 1;
2) adopt electron beam lithography to make Cr (5nm) and Au (80nm) metal electrode respectively at the two ends of nano wire and nano thin-film as collector;
3) adopt the PECVD technology on metal collector, to deposit the protective layer of the thick silicon nitride of 500nm as collector;
4) with LiClO 4With PEO, and propene carbonate blend dissolving preparation polymer dielectric, LiClO 4Electrolyte concentration is 1.4M, and polymer dielectric is dripped the surface that is coated in substrate, after 40 ℃ of oven dry, promptly accomplishes the assembling of single nanowire electrochemical device.
The technical scheme that the single nanowire electrochemical device in-situ characterization adopts comprises the steps, carries out successively:
1) battery is carried out cyclic voltammetric test and constant current charge-discharge test, battery was left standstill 10 minutes, under different charging and discharging states then to single V on the substrate 2O 5Nano line electrode carries out the electronic transport performance test of original position; Wherein, the unit type of electrochemistry and electrical performance testing is with embodiment 1;
2) to the single V under the different charging and discharging states 2O 5Nano line electrode carries out original position structural characterizations such as microcell Raman spectrum analysis.Wherein, the model of Raman spectrum analysis appearance is WITec CRM-200.
Embodiment 5:
The technical scheme that the single nanowire electrochemical device assembling is adopted comprises the steps, carries out successively:
1) with Si nano wire negative pole and LiCoO 2The anodal dispersed deposition of film has the thick SiO of one deck 100nm on the surface 2Silicon chip on; Wherein, the Si nano wire adopts the chemical vapour deposition technique preparation, and the preparation method is with reference to following document: A.M.Morales, and C.M.Lieber.Science, 279,208 (1998); LiCoO 2The preparation method of film is with embodiment 2;
2) adopt electron beam lithography to make Cr (5nm) and Au (80nm) metal electrode respectively at the two ends of nano wire and nano thin-film as collector;
3) adopt the ALD technology on metal collector, to deposit the thick Al of 500nm 2O 3Protective layer as collector;
4) with LiCF 3SO 3With polyacrylonitrile, and propene carbonate and ethylene carbonate (propene carbonate and ethylene carbonate mol ratio 1: 2) blend dissolving preparation polymer dielectric, LiCF 3SO 3Electrolyte concentration is 1M, and polymer dielectric is dripped the surface that is coated in substrate, after 40 ℃ of oven dry, promptly accomplishes the assembling of single nanowire electrochemical device.
The technical scheme that the single nanowire electrochemical device in-situ characterization adopts comprises the steps:
1) battery is carried out cyclic voltammetric test and constant current charge-discharge test, battery was left standstill under different charging and discharging states 30 minutes, then single Si nano line electrode on the substrate is carried out the electronic transport performance test of original position; Wherein, the unit type of electrochemistry and electrical performance testing is with embodiment 1;
2) the single Si nano line electrode under the different charging and discharging states is carried out original position structural characterizations such as microcell Raman spectrum analysis.Wherein, the model of Raman spectrum analysis appearance is WITec CRM-200.

Claims (12)

1. a single nanowire electrochemical device is characterized in that, this electrochemical device work electrode is a single nano-wire, processes by following assemble method, and number of assembling steps is followed successively by:
1) the anodal and nano thin-film negative pole with nano wire, perhaps nano wire negative pole and nano thin-film positive pole are dispersed on the substrate of insulation;
2) make metal electrode as collector at the two ends of described nano wire and nano thin-film respectively;
3) on metal collector, deposit protective layer;
4) polymer dielectric is dripped the surface that is coated in substrate, promptly accomplish the assembling of single nanowire electrochemical device.
2. a kind of single nanowire electrochemical device as claimed in claim 1; It is characterized in that; Described nano wire positive pole comprises vanadium oxide nanowires, lithium-barium oxide nano wire, lithium manganese oxide nano wire or lithium iron phosphate oxide nano wire, and corresponding nano thin-film negative pole comprises high order pyrolytic graphite flake nano film.
3. a kind of single nanowire electrochemical device as claimed in claim 1 is characterized in that, described nano wire negative pole comprises silicon nanowires or tin oxide nano-wire, and corresponding nano thin-film positive pole comprises the lithium and cobalt oxides nano thin-film.
4. a kind of single nanowire electrochemical device as claimed in claim 1 is characterized in that, the method for described making metal electrode collector comprises electronic beam photetching process.
5. a kind of single nanowire electrochemical device as claimed in claim 1 is characterized in that, the metal electrode that is used as collector comprises Cr and Au, perhaps Ti and Al.
6. a kind of single nanowire electrochemical device as claimed in claim 1 is characterized in that, the described protective layer that on metal collector, deposits comprises silicon nitride or insulated photo-etching rubber.
7. a kind of single nanowire electrochemical device as claimed in claim 6 is characterized in that, described protective layer is that the manufacture method of silicon nitride comprises plasma enhanced chemical vapor deposition method.
8. a kind of single nanowire electrochemical device as claimed in claim 6 is characterized in that, described protective layer is that the manufacture method of insulated photo-etching rubber comprises spin coating method.
9. a kind of single nanowire electrochemical device as claimed in claim 1 is characterized in that, described electrolyte comprises and contains LiClO 4, LiBF 4Or LiCF 3SO 3Polymer dielectric, said polymer dielectric is an a kind of or concurrent mixture electrolyte more than two kinds in PEO, polymethyl methacrylate, polyacrylonitrile, polyvinylidene fluoride, propene carbonate, the ethylene carbonate.
10. the in-situ characterization method of the described a kind of single nanowire electrochemical device of claim 1 is characterized in that it comprises the steps:
1) electrochemical device is carried out charge-discharge test, battery is left standstill under different charging and discharging states, then single nano-wire electrode on the described substrate is carried out the electronic transport performance test of original position;
2) the described nano line electrode under the different charging and discharging states is carried out the original position structural characterization.
11. the in-situ characterization method of a kind of single nanowire electrochemical device as claimed in claim 10 is characterized in that, the described time of leaving standstill is 1 minute ~ 1 hour.
12. the in-situ characterization method of a kind of single nanowire electrochemical device as claimed in claim 10 is characterized in that the method for described original position structural characterization comprises the microcell Raman spectrum analysis.
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