CN101519203A - Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof - Google Patents

Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof Download PDF

Info

Publication number
CN101519203A
CN101519203A CN200910066577A CN200910066577A CN101519203A CN 101519203 A CN101519203 A CN 101519203A CN 200910066577 A CN200910066577 A CN 200910066577A CN 200910066577 A CN200910066577 A CN 200910066577A CN 101519203 A CN101519203 A CN 101519203A
Authority
CN
China
Prior art keywords
powder
silicon
carbon
wire
preparation
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.)
Granted
Application number
CN200910066577A
Other languages
Chinese (zh)
Other versions
CN101519203B (en
Inventor
崔啟良
王秋实
张剑
梁罡
郝健
金云霞
李敏
刘丹
类伟巍
詹宝庆
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.)
Jilin University
Original Assignee
Jilin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jilin University filed Critical Jilin University
Priority to CN2009100665771A priority Critical patent/CN101519203B/en
Publication of CN101519203A publication Critical patent/CN101519203A/en
Application granted granted Critical
Publication of CN101519203B publication Critical patent/CN101519203B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention relates to a silicon-carbon-oxygen compound amorphous nanometer wire and a preparation method thereof, which belong to the technical field of one-dimension nanometer-structure materials. The nanometer wire comprises C, Si and O which are mutually bonded, and the atom proportion of C, Si and O is 13-30:38-52:100. The preparation method is as follows: silicon powder, carbon powder and silicon dioxide powder are used as raw materials and pressed into mixed powder blocks by a material mixing and block pressing progress; the block is placed into a DC electric-arc generator, argon gas is used as reaction gas, and under the condition of 20 V voltage and 100A current, exoelectrical reaction is carried out for 10 minutes to prepare the silicon-carbon-oxygen amorphous nanometer wire of white powder. The diameter of the nanometer wire is from 10 nm to 100 nm, and the length of the nanometer wire is from 10 microns to 15 microns. The invention has the advantages of simple method, environmental protection, low cost, high yield, rapid reaction, high repetitiveness, high purity of prepared sample, good stability and oxidization resistance, and the like, and has an excellent application prospect in the fields of quantum elements and photoluminescence.

Description

Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof
Technical field
The invention belongs to the technical field of one-dimensional nano structure material, particularly a kind of silicon-carbon-oxygen compound amorphous nanometer wire and simple preparation method thereof.
Background technology
In recent years, one-dimensional nano structure material is as nanotube, nano wire, nanometer rod, because its unique optical property and quantum transmission effects are having wide application prospect aspect molecular circuit and the quantum components and parts.In nano material family, the nano material of Si and C always is the focus of research.The nano material of silicon and carbon can prepare by several different methods, Gu Gu as LASER HEATING, gas-liquid-growth method, gas-growth method, sol-gel processing etc.
Present Si and the monodimension nanometer material of C mainly contain: carbon nanotube, silicon nanowires, nanometer silica line, silicon carbide nanometer line etc.Mainly, also do not prepare highly purified amorphous nanometer wire based on monocrystal nanowire.SiCO has been subjected to paying close attention to widely as a kind of type material, and its characteristic is mainly on high-temperature stability, oxidation-resistance.Functional property is mainly in low-k, photoluminescence, specific conductivity.The prior art close with the present invention can successfully prepare the film of SiCO polymkeric substance, but the SiCO amorphous nanometer wire do not reported also referring to Thin Solid Films 515 (2007) 5035-5039.The SiCO amorphous nanometer wire will be because its nano-meter characteristic will possess better functional property.
Summary of the invention
The technical problem to be solved in the present invention is to disclose a kind of SiCO amorphous nanometer wire; And the preparation method is simple, output height, sample purity height.
Concrete technical scheme of the present invention is:
A kind of silicon-carbon-oxygen compound amorphous nanometer wire, C, Si become key to form nano wire with O each other, and C, Si and O atomic ratio are 13~30: 38~52: 100.
The length of nano wire is 10~150 μ m, and diameter is 10~100nm.
The preparation method of silicon-carbon-oxygen compound amorphous nanometer wire of the present invention is with Si powder, C powder and SiO 2Powder is a raw material, and their mol ratio is 1: 0.5~1: 1; Preparation has batch mixing briquetting process and arc-over to generate the nano wire process;
Described batch mixing briquetting process is with Si powder, C powder and SiO 2Powder is put into mixer and is mixed; Again powder mix is pressed into the mixing powder agglomates;
Described arc-over generates the nano wire process, is to put into the anode of the reaction chamber of direct current arc electric discharge device with mixing powder agglomates, and reaction chamber is evacuated charges into argon gas again; At voltage is that 20~40V, electric current are exoelectrical reaction 5~10 minutes under the condition of 80~120A, antianode water-cooled, collects the powder of white in anode; The anode of described arc discharge device is the copper pot, and negative electrode is a tungsten electrode.
Among the preparation method of silicon-carbon-oxygen compound amorphous nanometer wire of the present invention, described reaction chamber is evacuated and charges into argon gas again, and vacuum tightness is less than 5pa, and charging into ar pressure is 5~25kPa.
Among the preparation method of silicon-carbon-oxygen compound amorphous nanometer wire of the present invention, described raw material, purity can be 99.9% or higher, granularity can be 200 orders or thinner, the excessive formation that is unfavorable for mixing powder agglomates of granularity; Described briquetting can be pressed into cylindrical mixing powder agglomates, also can be pressed into the mixing powder agglomates of other cubical shape, and the shape and the size of mixing powder agglomates determine according to tabletting machine cavity and copper pot anodic size; Powder mix is pressed into when mixing powder agglomates, can uses general tabletting machine, pressure is at 5~15MPa, can be not loose when concrete pressure size can be moved with the mixing powder agglomates after pressing for well.
Method of the present invention is simple, environmental protection, low cost; Nano wire preparation has the output height, is swift in response, repeatable high; Advantages such as sample purity height, good stability, good in oxidation resistance; The SiCO amorphous nanometer wire is because its nano-meter characteristic and semi-conductor material characteristic have broad application prospects at the quantum components and parts, and SiCO also has good application prospects at photoluminescence, potential making Ultra-Violet Laser emissive source.
Description of drawings
Fig. 1 is embodiment 1 a direct current arc electric discharge device structure iron of the present invention.
Fig. 2 is the SEM figure of the SiCO amorphous nanometer wire of embodiment 2 preparations.
Fig. 3 is the EDX figure of the SiCO amorphous nanometer wire of embodiment 2 preparations.
Fig. 4 is the TEM figure of the SiCO amorphous nanometer wire of embodiment 2 preparations.
Fig. 5 is the electron-diffraction diagram of the SiCO amorphous nanometer wire of embodiment 2 preparations.
Fig. 6 is the XRD spectra of the SiCO amorphous nanometer wire of embodiment 2 preparations.
Fig. 7 is the XPS spectrum figure of the nano wire of embodiment 2 preparations.
Fig. 8 is the SEM figure of the SiCO amorphous nanometer wire of embodiment 3.
Fig. 9 is the EDX figure of the SiCO amorphous nanometer wire of embodiment 3.
Figure 10 is the nano wire SEM figure of embodiment 4 preparations.
Figure 11 is the EDX figure of the nano wire of embodiment 4 preparations.
Embodiment
Embodiment 1 direct current arc electric discharge device structure iron
Illustrate that in conjunction with Fig. 1 the present invention prepares the direct current electric arc device structure diagram of SiCO amorphous nanometer wire.1 is the outer lens of direct current electric arc device, and 2 is cooling stave, and 3 is the negative electrode that is made of tungsten bar, and 4 is the anode that is made of the copper pot, is the reaction initial feed in the copper pot, and 5 is water-in, and 6 is water outlet, and 7 is inlet mouth, and 8 is the air outlet.
In the copper pot, feed the key of water coolant, produce high temperature during discharge in the copper pot, after discharge stops,, thereby obtain amorphous nanometer wire, reach the effect of quenching because the effect of water coolant descends the temperature in the copper pot rapidly for the preparation amorphous nanometer wire.
The whole process of the best SiCO amorphous nanometer wire of embodiment 2 preparations.With 200 purpose Si powder, C powder and SiO 2Powder is that the ratio of 1:1:1 is put into mixer and mixed according to mol ratio.Take out the powder mix of 3g, use the tabletting machine briquetting, depressing to diameter at 10Mpa pressure is that 1cm, height are the right cylinder mixing powder agglomates of 3cm.The mixing powder agglomates that is pressed into is put into the reaction chamber anode of direct current arc electric discharge device.The anode of arc discharge device is the copper pot, and negative electrode is a tungsten electrode.The reaction chamber of direct current arc electric discharge device is evacuated (less than 5pa), fills the 10kPa argon gas then, in the copper pot, feed water coolant.Begin discharge, sustaining voltage is 20V in discharge process, and electric current is 100A.React after 5 minutes, the powder of collecting white in anodic copper pot is the SiCO nano wire.Fig. 2 provides the nano wire of above-mentioned condition preparation, and the length of nano wire is 100~150 μ m.Fig. 3 provides the EDX figure of the nano wire of above-mentioned condition preparation, can draw nano wire and be C, Si are arranged, three kinds of O are elementary composition, atomic ratio is 17: 23: 59.Fig. 4 provides the TEM figure of the nano wire of above-mentioned condition preparation, and the diameter of nano wire is 50~100nm.Fig. 5, Fig. 6 provide the electron-diffraction diagram and the XRD spectra of the nano wire of above-mentioned condition preparation, prove that nano wire is an amorphous nanometer wire.Fig. 7 provides the XPS spectrum figure of the nano wire of above-mentioned condition preparation, proves C, Si, and three kinds of elements of O are in strong, form nano wire.Wherein Fig. 7 a is the full spectrogram of XPS, and Fig. 7 b is Si element XPS spectrum figure, and Fig. 7 c is C element XPS spectrum figure, and Fig. 7 d is O element XPS spectrum figure.
The whole process of embodiment 3 preparation SiCO amorphous nanometer wires.With 200 purpose Si powder, C powder and SiO 2Powder is that the ratio of 1:0.5:1 is put into mixer and mixed according to mol ratio.Take out the powder mix of 3g, use the tabletting machine briquetting, the pressure of briquetting is 10Mpa, and being pressed into diameter is 1cm, and height is the cylindrical mixing powder agglomates of 3cm.The mixing powder agglomates that is pressed into is put into the reaction chamber anode of direct current arc electric discharge device.The anode of arc discharge device is the copper pot, and negative electrode is a tungsten electrode.The reaction chamber of direct current arc electric discharge device is evacuated (less than 5pa), fills the 25kPa argon gas then, in the copper pot, feed water coolant.Begin discharge, sustaining voltage is 40V in discharge process, and electric current is 120A.React after 10 minutes, the powder of collecting white in anodic copper pot is the SiCO nano wire.Fig. 8 provides the nano wire SEM figure of above-mentioned condition preparation, and the length of nano wire is 10~100 μ m, and diameter is 10~100nm, skewness.Fig. 9 provides the nano wire EDX figure of above-mentioned condition preparation, and can draw nano wire is that C is arranged, Si, and three kinds of O are elementary composition, and atomic ratio is 8:31:60, and the C constituent content of amorphous nanometer wire obviously reduces.
The whole process of embodiment 4 preparation SiCO amorphous nanometer wires.With 200 purpose Si powder, C powder and SiO 2Powder is that the ratio of 1:1:1 is put into mixer and mixed according to mol ratio.Take out the powder mix of 3g, use the tabletting machine briquetting, the pressure of briquetting is 5Mpa, and being pressed into diameter is 1cm, and height is the cylindrical mixing powder agglomates of 3cm.The mixing powder agglomates that is pressed into is put into the reaction chamber anode of direct current arc electric discharge device.The anode of arc discharge device is the copper pot, and negative electrode is a tungsten electrode.The reaction chamber of direct current arc electric discharge device is evacuated (less than 5pa), fills the 10kPa argon gas then, in the copper pot, feed water coolant.Begin discharge, sustaining voltage is 20V in discharge process, and electric current is 80A.React after 5 minutes, the powder of collecting white in anodic copper pot is the SiCO nano wire.Figure 10 provides the nano wire SEM figure of above-mentioned condition preparation, and the length of nano wire is the EDX figure of 50~100 μ m. Figure 11 nano wire of providing above-mentioned condition preparation, and can draw nano wire is that C is arranged, Si, and three kinds of O are elementary composition, and atomic ratio is 17:23:58.

Claims (4)

1, a kind of silicon-carbon-oxygen compound amorphous nanometer wire is characterized in that, C, Si become key to form nano wire with O each other, and C, Si and O atomic ratio are 13~30: 38~52: 100.
2, according to the described silicon-carbon-oxygen compound amorphous nanometer wire of claim 1, it is characterized in that, described nano wire, length is 10~150 μ m, diameter is 10~100nm.
3, a kind of preparation method of silicon-carbon-oxygen compound amorphous nanometer wire of claim 1 is characterized in that, with Si powder, C powder and SiO 2Powder is a raw material, and their mol ratio is 1: 0.5~1: 1; Preparation has batch mixing briquetting process and arc-over to generate the nano wire process;
Described batch mixing briquetting process is with Si powder, C powder and SiO 2Powder is put into mixer and is mixed; Again powder mix is pressed into the mixing powder agglomates;
Described arc-over generates the nano wire process, is to put into the anode of the reaction chamber of direct current arc electric discharge device with mixing powder agglomates, and reaction chamber is evacuated charges into argon gas again; At voltage is that 20~40V, electric current are exoelectrical reaction 5~10 minutes under the condition of 80~120A, antianode water-cooled, collects the powder of white in anode; The anode of described arc discharge device is the copper pot, and negative electrode is a tungsten electrode.
According to the preparation method of the described silicon-carbon-oxygen compound amorphous nanometer wire of claim 3, it is characterized in that 4, described reaction chamber is evacuated and charges into argon gas again, vacuum tightness is less than 5pa, and charging into ar pressure is 5~25kPa.
CN2009100665771A 2009-02-27 2009-02-27 Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof Expired - Fee Related CN101519203B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009100665771A CN101519203B (en) 2009-02-27 2009-02-27 Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009100665771A CN101519203B (en) 2009-02-27 2009-02-27 Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof

Publications (2)

Publication Number Publication Date
CN101519203A true CN101519203A (en) 2009-09-02
CN101519203B CN101519203B (en) 2010-12-08

Family

ID=41080029

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009100665771A Expired - Fee Related CN101519203B (en) 2009-02-27 2009-02-27 Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof

Country Status (1)

Country Link
CN (1) CN101519203B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139374A (en) * 2011-03-08 2011-08-03 吉林大学 Method for preparing metal zinc nanometer wire
CN103896282A (en) * 2012-12-25 2014-07-02 北京有色金属研究总院 Method used for preparing silicon oxide nanowires via green compact of silicon carbide powder
CN115029129A (en) * 2022-06-23 2022-09-09 渤海大学 Luminescent ion doped silicon dioxide fluorescent powder and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139374A (en) * 2011-03-08 2011-08-03 吉林大学 Method for preparing metal zinc nanometer wire
CN102139374B (en) * 2011-03-08 2012-10-03 吉林大学 Method for preparing metal zinc nanometer wire
CN103896282A (en) * 2012-12-25 2014-07-02 北京有色金属研究总院 Method used for preparing silicon oxide nanowires via green compact of silicon carbide powder
CN103896282B (en) * 2012-12-25 2015-09-30 北京有色金属研究总院 The silicon carbide powder pressed compact preparation method of silica white nano-wire
CN115029129A (en) * 2022-06-23 2022-09-09 渤海大学 Luminescent ion doped silicon dioxide fluorescent powder and preparation method thereof
CN115029129B (en) * 2022-06-23 2024-01-19 渤海大学 Luminescent ion doped silicon dioxide fluorescent powder and preparation method thereof

Also Published As

Publication number Publication date
CN101519203B (en) 2010-12-08

Similar Documents

Publication Publication Date Title
CN101250639B (en) Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof
Cao et al. Room-temperature ultraviolet-emitting In 2 O 3 nanowires
CN1084527C (en) Co-Sb thermoelectric materials and mfg. method thereof
Zhang et al. Optical and electrochemical properties of nanosized CuO via thermal decomposition of copper oxalate
Wu et al. Preparation and photoluminescence of yttrium hydroxide and yttrium oxide doped with europium nanowires
CN103981381B (en) Method for preparing nano aluminum oxide dispersion enhanced copper-base composite material according to sol-gel method
CN111940750B (en) Preparation method of alloy powder material
JP2006001779A (en) Method for producing sic nanoparticles by nitrogen plasma
CN101519203B (en) Silicon-carbon-oxygen compound amorphous nanometer wire and preparation method thereof
Liu et al. Photoluminescence of rare earth3+ doped uniaxially aligned HfO2 nanotubes prepared by sputtering with electrospun polyvinylpyrolidone nanofibers as templates
CN101264888A (en) Method for preparing nano-stage tungsten carbide powder
CN109233821B (en) Multicolor luminous carbon quantum dot and preparation method and application thereof
Xiaoxu et al. Synthesis of Y2O3 phosphor by a hydrolysis and oxidation method
CN109437912A (en) A kind of preparation method of the silica in situ cladding silicon carbide nuclear-shell structured nano-composite material of morphology controllable
CN101513996B (en) An aluminum nitride nanometer comb and preparation method thereof
CN101941691A (en) Preparation method of single-walled carbon nanotube
Yue et al. Controlled synthesis, asymmetrical transport behavior and luminescence properties of lanthanide doped ZnO mushroom-like 3D hierarchical structures
CN102627263B (en) Method for preparing magnesium-doped aluminum nitride nanowire
CN100460330C (en) One-D nano zinc oxide and vacuum electric arc prepn. process
WO2005117032A1 (en) METHOD FOR PRODUCING Nb3Sn SUPERCONDUCTIVE WIRE BY POWDER PROCESS
CN102139374B (en) Method for preparing metal zinc nanometer wire
Wang et al. Synthesis of nanostructured La2O3/La2O2CO3: Eu phosphors from arc-discharged graphene-contained composites
KR100428948B1 (en) A production method of tungsten nano powder without impurities and its sintered part
CN107151000A (en) The preparation method of zinc selenide hollow sub-microsphere
KR101641839B1 (en) Preparation method of Si/SiC composite nanoparticles by fusion process of solid phase reaction and plasma decomposition

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20101208

Termination date: 20120227