CN103352253B - A kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method - Google Patents
A kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method Download PDFInfo
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Abstract
A kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method, it includes step in detail below: C paper is immersed in certain density catalyst ethanol solution by (1), naturally dries standby；(2) liquid organic precursor polysilazane being placed in graphite crucible, then by step 1) the C paper that introduces catalyst is placed in graphite crucible top, in 5%N in atmosphere sintering furnace2With pyrolysis certain time under the hybrid protection atmosphere of 95%Ar gas (volume ratio)；(3) by controlling pyrolysis temperature, it is achieved atom N is the control of dissolubility in catalyst droplets, and then realizes the regulation and control of n-type SiC monocrystal low-dimension nano material N doping content.The present invention can realize n-type SiC monocrystal low-dimension nano material Uniform Doped and the regulation and control of doping content thereof and design, has potential application prospect at photoelectric nano device.
Description
Technical field
The present invention relates to a kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method, belong to material preparation technology neck
Territory.
Background technology
Third generation broadband based semiconductor SiC material has high-breakdown-voltage, high heat conductance, high electron mobility and high electric float
Move the excellent physical characteristics such as speed, at necks such as harsh working environment such as high temperature, high frequency, high-power, photoelectron and radioprotective devices
Territory is with a wide range of applications.Compared to traditional Si C body material, SiC low-dimension nano material is because of the nano effect of its uniqueness
Have more excellent mechanics, the performance such as optically and electrically, preparing high-performance composite materials and constructing the sides such as nano photoelectric device
Face has shown tempting application prospect.
Based on the performance that SiC low-dimension nano material is excellent, have numerous studies work at present and report SiC low-dimension nano material
Preparation method, including organic precursor pyrolysismethod, template, carbothermic method, chemical gaseous phase deposition, direct chemical reaction method,
Arc discharge method, hydro-thermal and solvent-thermal method and thermal evaporation etc..Said method is realizing the control of SiC low-dimension nano material growth
Upper (including pattern, size and crystal growth direction etc.) is achieved with preferable progress.
But, SiC low-dimension nano material be able to one of important foundation of device application be realize its doping and doping type thereof and
The regulation and control of concentration, correlational study worked also in the starting stage.Existing research work is concentrated mainly on p-type SiC low-dimensional nanometer material
The preparation of material and doping content regulation and control (mainly to mix Al) thereof, and the nano-device such as scene effect transistor and pressure transducer
The performance of excellence has been shown in application.Comparing p-type SiC low-dimension nano material, N-shaped SiC low-dimension nano material carries due to it
Stream is sub based on electronics, thus more with potential applications in the field such as filed emission cathode material, thermoelectric material.But, based on N-shaped
The regulation and control of SiC single crystal low-dimension nano material doping content, at home and abroad there is not yet document report.
Summary of the invention
The technical problem to be solved be to provide a kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method.
Equipment and the technique of the method for the present invention are the most controlled, have good repeatability.
The present invention solves the technical scheme that above-mentioned technical problem used: this regulation and control n-type SiC monocrystal low-dimension nano material adulterates
The method of concentration, it includes step in detail below:
1) catalyst introduces: be immersed in by C paper in certain density catalyst ethanol solution, realizes urging after naturally drying
The introducing of agent.
2) high temperature pyrolysis: a certain amount of liquid organic precursor is placed in graphite crucible, and by step 1) introduce catalyst after
C paper is placed in graphite crucible top, is subsequently placed in atmosphere sintering furnace and carries out high temperature pyrolysis, at N2Protect with the mixing of Ar gas
Protect and be pyrolyzed certain time under atmosphere and can realize the preparation of n-type SiC monocrystal low-dimension nano material.
3) doping content regulation and control: by controlling pyrolysis temperature, it is achieved atom N is the control of dissolubility in catalyst droplets,
Realize the regulation and control of n-type SiC monocrystal low-dimension nano material N doping content eventually.
In described step (1), C paper is used as matrix with deposition growing SiC single crystal low-dimension nano material.
In described step (2) and (3), the raw material of use is polysilazane.Institute's use sintering furnace is graphite resistance atmosphere sintering
Stove, also can use other atmosphere sintering furnaces.
In described step (2) and (3), introduced catalyst is Co (NO3)2.Also can use other metallic element and
Compound, such as FeCl2、Fe(NO3)3、Ni(NO3)2Deng；The protective atmosphere used is the N of 5%2With 95% Ar gas (body
Long-pending ratio), also can use the protective atmosphere of other proportionings.
Compared with prior art, it is an advantage of the current invention that:
1. the present invention is by controlling pyrolysis temperature to realize atom N control of dissolubility in high temperature catalyst drop, it is achieved that
The control of SiC single crystal low-dimension nano material doping content and design；
2. the n-type SiC monocrystal low-dimension nano material prepared by the present invention has uniform N foreign atom spatial distribution, also
Realize the uniform N doping of SiC low-dimension nano material.
Accompanying drawing explanation
Fig. 1 is the scanning under different amplification of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention one
Electronic Speculum (SEM) figure；
Fig. 2 is the transmission under different amplification of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention one
Electronic Speculum (TEM) figure, selected diffraction (SAED) and high-resolution-ration transmission electric-lens (HRTEM) figure；
Fig. 3 is power spectrum (EDX) figure of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention one；
Fig. 4 is Si, the C of n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention one and the face of N element is swept
Mapping；
Fig. 5 is the scanning under different amplification of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention two
Electronic Speculum (SEM) figure；
Fig. 6 is the scanning under different amplification of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention three
Electronic Speculum (SEM) figure；
Fig. 7 is the X-ray diffraction of the n-type SiC monocrystal low-dimension nano material obtained by the embodiment of the present invention one, two and three
(XRD) collection of illustrative plates.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one
C paper is immersed in the Co (N0 of 0.05mol/L3)2In the ethanol solution of (purity 99%), take out after 3 minutes and be placed in
Naturally dry standby under air ambient.Weigh initial feed polysilazane 0.6g and be placed in graphite crucible (purity 99.5%), at stone
Ink crucible top adds a cover the C paper after immersion treatment, is placed in together in graphite resistance sintering furnace, then in the flowing of 0.1MPa
(200ml/min) mixed gas (5%N2And 95%Ar, volume ratio) under protective atmosphere, with 25 DEG C/min from room temperature to
1350 DEG C, carry out high temperature pyrolysis, be incubated 2 hours, cool to room temperature afterwards with the furnace.Fig. 1 is the N-shaped of prepared N doping
SiC single crystal nano wire typical case's low power and high power scanning electron microscope (SEM) photo, show that prepared N-shaped SiC nanowire has higher
Productivity and higher purity, any surface finish；Fig. 2 is the transmission under the different amplification of prepared N-shaped SiC nanowire
Electronic Speculum (TEM), SEAD (SAED) collection of illustrative plates and corresponding high-resolution-ration transmission electric-lens (HRTEM) photo thereof, show made
Standby N-shaped SiC nanowire is monocrystalline 3C-SiC, and has preferable crystallinity；Fig. 3 is prepared N-shaped SiC nanowire
Power spectrum (EDX), show in SiC nanowire containing N foreign atom, concentration is 10.14at.%；Fig. 4 is prepared N-shaped
In SiC nanowire, Si, C and N element Surface scan collection of illustrative plates, show that N foreign atom has in SiC single crystal low-dimension nano material
Uniform spatial distribution.
Embodiment two
C paper is immersed in the Co (NO of 0.05mol/L3)2In the ethanol solution of (purity 99%), take out after 3 minutes and be placed in
Naturally dry standby under air ambient.Weigh initial feed polysilazane 0.6g and be placed in graphite crucible (purity 99.5%), at stone
Ink crucible top adds a cover the C paper after immersion treatment, is placed in together in graphite resistance sintering furnace, then in the flowing of 0.1MPa
(200ml/min) mixed gas (5%N2And 95%Ar, volume ratio) under protective atmosphere, with 25 DEG C/min from room temperature to
1400 DEG C, carry out high temperature pyrolysis, be incubated 2 hours, cool to room temperature afterwards with the furnace.Fig. 5 is the N-shaped of prepared N doping
SiC single crystal nano wire typical case's low power and high power scanning electron microscope (SEM) photo, show that prepared N-shaped SiC nanowire has higher
Productivity and higher purity, any surface finish；Analyze through power spectrum (EDX) and show that in SiC nanowire, N concentration of dopant atoms is
8.28at.%.Show with embodiment one Comparative result analysis, by the regulation and control to pyrolysis temperature, it is possible to realize N-shaped SiC nanowire
The regulation and control of middle N concentration of dopant atoms.
Embodiment three
C paper is immersed in the Co (NO of 0.05mol/L3)2In the ethanol solution of (purity 99%), take out after 3 minutes and be placed in
Naturally dry standby under air ambient.Weigh initial feed polysilazane 0.6g and be placed in graphite crucible (purity 99.5%), at stone
Ink crucible top adds a cover the C paper after immersion treatment, is placed in together in graphite resistance sintering furnace, then in the flowing of 0.1MPa
(200ml/min) mixed gas (5%N2And 95%Ar, volume ratio) under protective atmosphere, with 25C/min from room temperature to
1450 DEG C, carry out high temperature pyrolysis, be incubated 2 hours, cool to room temperature afterwards with the furnace.Fig. 6 is the N-shaped of prepared N doping
SiC single crystal nano wire typical case's low power and high power scanning electron microscope (SEM) photo, show that prepared N-shaped SiC nanowire has higher
Productivity and higher purity, any surface finish；Analyze through power spectrum (EDX) and show that in SiC nanowire, N concentration of dopant atoms is
4.12at.%.It is analyzed can further demonstrate that with the result of embodiment one, two, by the regulation and control to pyrolysis temperature, it is possible to
Realize the regulation and control of N concentration of dopant atoms in N-shaped SiC nanowire.Fig. 7 be pyrolysis temperature be respectively 1350 DEG C (embodiments one),
The X-ray diffraction (XRD) of N-shaped SiC nanowire prepared under the conditions of 1400 DEG C (embodiments two) and 1450 DEG C (embodiment three)
Collection of illustrative plates, shows that prepared nano material is 3C-SiC phase (Fig. 7 a), and its diffraction peak and unadulterated standard diffraction card
Data (JPCDS29-1129) contrast, and all there occurs that obvious peak position moves, illustrate that its lattice paprmeter there occurs change, thus demonstrate,prove
Understand that prepared 3C-SiC nano wire achieves the doping of atom N.
The present invention propose a kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method, by control pyrolysis temperature
To realize atom N control of dissolubility in high temperature catalyst drop, and then realize regulation and control and the design of its doping content.This
Bright technique is simple, reproducible, and prepared n-type SiC monocrystal low-dimension nano material purity is high, any surface finish, and has all
Even N foreign atom spatial distribution, has potential application prospect in photoelectric nano device.
Claims (1)
1. the method regulating and controlling n-type SiC monocrystal low-dimension nano material doping content, it includes step in detail below:
1) C paper is immersed in the Co (NO of 0.05mol/L3)2Ethanol solution in, after 3 minutes take out be placed under air ambient naturally dry standby, Co (NO3)2Purity be 99%；
2) weigh initial feed polysilazane 0.6g to be placed in graphite crucible; the purity of graphite is 99.5%; C paper after immersion treatment is added a cover at graphite crucible top, is placed in graphite resistance sintering furnace, together then at 0.1MPa; under the mixed gas protected atmosphere of 200ml/min flow rate; with 25 DEG C/min from room temperature to pyrolysis temperature, carry out high temperature pyrolysis, be incubated 2 hours; cooling to room temperature afterwards with the furnace, wherein mixed gas is by volume for 5%N2Mixed gas with 95%Ar；
3) doping content regulation and control: pyrolysis temperature is 1350 DEG C, and N doping content is 10.14at.%；Pyrolysis temperature is 1400 DEG C, and N doping content is 8.28at.%；Pyrolysis temperature is 1450 DEG C, and N doping content is 4.12at.%.
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| CN105088182B (en) * | 2015-08-19 | 2017-04-19 | 宁波工程学院 | N-doped SiC nanoneedle and application thereof |
| CN108760104B (en) * | 2018-07-03 | 2020-10-09 | 宁波工程学院 | N-doped SiC nanobelt high-sensitivity pressure sensor and preparation method thereof |
| CN108706588B (en) * | 2018-07-03 | 2022-02-22 | 宁波工程学院 | N-doped SiC nanobelt with large width-thickness ratio and preparation method thereof |
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