CN101311378B - Controllable doping of SiC single crystal low-dimensional nano material - Google Patents
Controllable doping of SiC single crystal low-dimensional nano material Download PDFInfo
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- CN101311378B CN101311378B CN2008100863265A CN200810086326A CN101311378B CN 101311378 B CN101311378 B CN 101311378B CN 2008100863265 A CN2008100863265 A CN 2008100863265A CN 200810086326 A CN200810086326 A CN 200810086326A CN 101311378 B CN101311378 B CN 101311378B
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Abstract
The invention relates to a new method for realizing the controllable doping of SiC single crystal low dimensional nano material by co-pyrolyzing organic precursors, which comprises the following concrete steps: (1) ball milling and well mixing two organic precursors PSZ and aluminum isopropoxide according to different proportions; (2) after mixing, cross-linking and solidifying the precursors to obtain amorphous solid; (3) putting the amorphous solid into a nylon resin ball milling tank and introducing a catalyst, and carrying out ball milling in a ball mill; (4) high temperature pyrolyzing the milled mixture. The method can realize the controlling and designing of the doping level of SiC single crystal low dimensional nano material on molecular level, therefore, the control of properties such as photoelectricity, and the like, of the SiC single crystal low dimensional nano material is realized and certain foundation for developing nano devices thereof is laid.
Description
Technical field
The present invention relates to the controllable doped method of a kind of SiC single-crystal low-dimension nano material, belong to technical field of material.
Technical background
Nanotechnology is the forward position and the focus of 21 century development in science and technology, will be significant to national future technology progress, economy and social development and national defense safety.Existing more than 50 is individual national with the main driving mechanism of nanotechnology as the 21 century technological innovation in the world, and formulated development strategy and plan in succession, to instruct and to advance national Nano-technology Development.China has formulated " National Program for Medium-to Long-term Scientific and Technological Development (2006-2020) " at the beginning of 2006, list nano science in this section one of four main directions of basic scientific research in period.
Since CNT (carbon nano-tube) in 1991 was found by professor Iijima of Japanese NEC Corporation, the research of low-dimension nano materials such as nanotube, nano wire and nano belt was the research emphasis and the focus of nanosecond science and technology always.Therefore scientist professor Lieber of Harvard University thinks: " the one dimension system is to can be used for electronics effect spread and light activated smallest dimension structure are arranged, and may become to realize the integrated key with function of nano-device ".Low-dimensional nano structure is a kind of effective research system of electricity, calorifics and the mechanical property of people's research material and dimension and quantum limitation effect dependency.These low-dimensional nano structures, might the electronics, photoelectricity, electrochemistry of preparation nano-scale during with the electromechanical device as being connected and functional unit plays a significant role.Yet low-dimensional nano structure has influenced its flow of research greatly in the difficulties such as regulation and control of dimension, pattern, phase purity and chemical ingredients.
SiC semi-conductor low-dimensional nano structure owing to distinctive nano effect shows many performances such as photoelectricity that are better than the conventional bulk material, becomes a focus of recent research.SiC has broad-band gap (4H-SiC is 3.26eV, and 6H-SiC is 2.86eV, and 3C-SiC is 2.2eV) and higher voltage breakdown, and (4H-SiC is 2.2MVcm
-1, 6H-SiC is 2.5MVcm
-1, 3C-SiC is 2.12MVcm
-1), (4H-SiC is 3.7Wcm to high heat conductance
-1K
-1, 6H-SiC is 4.9Wcm
-1K
-1, 3C-SiC is 3.2Wcm
-1K
-1), (4H-SiC is 1000cm to high electron mobility
2V
-1s
-1, 6H-SiC is 400cm
2V
-1s
-1, 3C-SiC is 800cm
2V
-1s
-1) and high electronic drifting rate (4H-SiC and 6H-SiC are 2 * 10
7Cms
-1, 3C-SiC is 2.5 * 10
7Cms
-1), be third generation wide bandgap semiconductor materials, be mainly used in harsh Working environment such as high temperature, high frequency, high-power, photoelectron and radioprotective device, have huge and application potential widely.The SiC material can not melt under any temperature simultaneously, the distillation phenomenon when being higher than 1800 ℃, temperature takes place, SiC has quite high stability when being lower than 1500 ℃, thereby has avoided the instability problem under semiconductor material commonly used such as the high temperature conditions such as Si and GaP.In addition, the SiC low-dimension nano material has very high hardness, toughness, wear resistance, high thermal resistance, low good characteristics such as thermal expansivity, at preparation high performance composite, high strength small size composite element, nano surface reinforced composite and construct aspect such as nano photoelectric device and have very tempting application prospect.According to the literature, the method for preparing the SiC low-dimension nano material mainly contains template (most of carbon nanotube that adopts is as template), carbothermic method, chemical vapor deposition (CVD), direct chemical reaction method, arc discharge method, hydro-thermal and solvent-thermal method and thermal evaporation etc.Aforesaid method has enriched the preparation science of SiC low-dimension nano material greatly, yet does not at home and abroad appear in the newspapers so far for the controllable doped of SiC single-crystal low-dimension nano material.
Summary of the invention
Technical problem to be solved by this invention provides the controllable doped method of a kind of SiC single-crystal low-dimension nano material.The equipment of method of the present invention and technology simple controllable, and has a good repeatability, in synthetic SiC single-crystal low-dimension nano material, promptly realize mixing, biggest advantage is to realize that the doping to low-dimension nano material designs and regulates and control, thereby reaches the regulation and control to its photoelectric properties.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the method for this SiC single-crystal low-dimension nano material, and it comprises following concrete steps:
1) ball milling mixes: two kinds of organic precursors of raw material are placed the ball grinder planetary ball mill by different ratios, make raw material mix;
2) crosslinked at low temperature solidifies: the organic precursor ball milling mixes the back and solidifies in carrying out crosslinked at low temperature under protective atmosphere, obtains non-crystalline solids;
3) high-energy ball milling is pulverized: non-crystalline solids are packed into carry out dry ball milling in the nylon resin ball grinder in high energy ball mill and pulverize, introduce catalyzer in the time of ball milling, make that non-crystalline state powder and catalyst mix are even;
4) high temperature pyrolysis: the mixture behind the high-energy ball milling carries out high temperature pyrolysis, at certain pyrolysis temperature single-crystal low-dimension nano material that the pyrolysis certain hour can obtain having different dopings under protective atmosphere.
In the described step (1), the raw material that uses is polysilazane and aluminum isopropylate, thereby also can adopt the organic precursor that contains other metallic elements to realize the doping of corresponding other elements.
In described step (1) and (3), the mill preferentially selected for use is situated between and is the SiC Ceramic Balls, and the ball grinder that uses is the nylon resin ball grinder, also can use ceramic ball grinder, avoids using metal ball grinder such as stainless steel to reduce other contaminating impurities.
In the described step (3), employed ball milling method is a high-energy ball milling, and the catalyzer of being introduced is FeCl
2Also can adopt other metallic element and compound thereof, as Fe, Fe (NO
3)
3, Ni and Co etc.
In described step (2) and (4), institute uses sintering oven to be the tubular type atmosphere sintering furnace, also can adopt other atmosphere sintering furnaces.
In described step (2) and (4), for the growth of controlling single-crystal low-dimension nano material and avoid polluting, at N
2With carry out pyrolysis under the gases such as Ar.
Compared with prior art, the invention has the advantages that:
1. the present invention has realized the controllable doped of SiC single-crystal low-dimension nano material;
2. equipment and technology are simple, have very high repeatability, and controllability is strong, simply control the low-dimension nano material that some key process parameters in the synthesis technique can obtain to have different dopings;
3. synthetic low-dimension nano material purity height, any surface finish;
4. the low-dimension nano material productive rate is higher, can reach～50%.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) figure of the embodiment of the invention one prepared Al doped SIC monocrystal nanowire;
Fig. 2 is scanning electron microscope (SEM) figure of the embodiment of the invention one prepared Al doped SIC monocrystal nanowire;
Fig. 3 is power spectrum (EDX) figure of the embodiment of the invention one prepared Al doped SIC monocrystal nanowire;
Fig. 4 is transmission electron microscope (TEM) figure of the embodiment of the invention one prepared Al doped SIC monocrystal nanowire;
Fig. 5 is the high-resolution-ration transmission electric-lens (TEM) of the embodiment of the invention one prepared Al doped SIC monocrystal nanowire and corresponding selected diffraction (SAED) figure thereof;
Fig. 6 is scanning electron microscope (SEM) figure of the embodiment of the invention two prepared Al doped SIC monocrystal nanowires;
Fig. 7 is transmission electron microscope (TEM) figure of the embodiment of the invention two prepared Al doped SIC monocrystal nanowires;
Fig. 8 is scanning electron microscope (SEM) figure of the embodiment of the invention three prepared Al doped SIC monocrystal nanowires;
Fig. 9 is transmission electron microscope (TEM) figure of the embodiment of the invention three prepared Al doped SIC monocrystal nanowires;
Figure 10 is transmission electron microscope (TEM) figure of the embodiment of the invention four prepared Al doped SIC monocrystal nanowires;
Figure 11 is transmission electron microscope (TEM) figure of the embodiment of the invention five prepared Al doped SIC monocrystal nanowires;
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment one
Take by weighing initial feed (5wt% aluminum isopropylate+95wt% polysilazane) 10g altogether, planetary ball mill is 12 hours in the nylon resin ball grinder of packing into, mixes to be placed in the 99 alumina-ceramic crucibles, at the N of 0.1MPa
2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing, obtain non-crystalline state SiAlCN solid with 10 ℃/min.The SiAlCN solid is packed in the nylon resin ball grinder, add the FeCl of 3wt%
2Powder carries out dry ball milling as catalyzer and pulverized 24 hours in high energy ball mill; the SiAlCN powder that obtains after then high-energy ball milling being pulverized places 99 alumina-ceramic crucibles; under (200ml/min) Ar atmosphere protection that flows of 0.1MPa, in tube furnace, be warmed up to 1450 ℃ from room temperature and carry out high temperature pyrolysis with 10 ℃/min; be incubated 2 hours, furnace cooling is to room temperature then.The adulterated SiC monocrystal nanowire typical case's low power of Al and high power SEM, TEM, HRTEM, SAED and EDX shown in Fig. 1～5, show that the adulterated SiC monocrystal nanowire of Al is a monocrystalline, perfect structure respectively, mean diameter pact～300nm, any surface finish, even thickness, length are tens μ m.Calculated as can be known by the XRD detected result, the lattice parameter a of SiC and c compare with doped samples not and reduce by 0.36 and 0.8% respectively, show that Al has mixed in the middle of the SiC lattice, and the EDS detected result shows that the Al doping is 1.25at%.
Embodiment two
Take by weighing initial feed (0.2wt% aluminum isopropylate+99.8wt% polysilazane) 10g altogether, planetary ball mill is 12 hours in the nylon resin ball grinder of packing into, mixes to be placed in the 99 alumina-ceramic crucibles, at the N of 0.1MPa
2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing, obtain non-crystalline state SiAlCN solid with 10 ℃/min.The SiAlCN solid is packed in the nylon resin ball grinder, add the FeCl of 3wt%
2Powder carries out dry ball milling as catalyzer and pulverized 24 hours in high energy ball mill; the SiAlCN powder that obtains after then high-energy ball milling being pulverized places 99 alumina-ceramic crucibles; under (200ml/min) Ar atmosphere protection that flows of 0.1MPa, in tube furnace, be warmed up to 1450 ℃ from room temperature and carry out high temperature pyrolysis with 10 ℃/min; be incubated 2 hours, furnace cooling is to room temperature then.Al typical SEM of adulterated SiC monocrystal nanowire and TEM shown in Fig. 6 and 7, show the adulterated SiC monocrystal nanowire of Al mean diameter～250nm respectively, and any surface finish, even thickness, length are several μ m.Calculated as can be known by the XRD detected result, the lattice parameter a of SiC and c compare with doped samples not and reduce by 0.21 and 0.53% respectively, show that Al has mixed in the middle of the SiC lattice, and the EDS detected result shows that the Al doping is 0.52at%.
Embodiment three
Take by weighing initial feed (1wt% aluminum isopropylate+99wt% polysilazane) 10g altogether, planetary ball mill is 12 hours in the nylon resin ball grinder of packing into, mixes to be placed in the 99 alumina-ceramic crucibles, at the N of 0.1MPa
2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing, obtain non-crystalline state SiAlCN solid with 10 ℃/min.The SiAlCN solid is packed in the nylon resin ball grinder, add the FeCl of 3wt%
2Powder carries out dry ball milling as catalyzer and pulverized 24 hours in high energy ball mill; the SiAlCN powder that obtains after then high-energy ball milling being pulverized places 99 alumina-ceramic crucibles; under (200ml/min) Ar atmosphere protection that flows of 0.1MPa, in tube furnace, be warmed up to 1450 ℃ from room temperature and carry out high temperature pyrolysis with 10 ℃/min; be incubated 2 hours, furnace cooling is to room temperature then.Al typical SEM of adulterated SiC monocrystal nanowire and TEM shown in Fig. 8 and 9, show the adulterated SiC monocrystal nanowire of Al mean diameter～150nm respectively, and any surface finish, even thickness, length are tens μ m.Calculated as can be known by the XRD detected result, the lattice parameter a of SiC and c compare with doped samples not and reduce by 0.31 and 0.78% respectively, show that Al has mixed in the middle of the SiC lattice, and the EDS detected result shows that the Al doping is 1.05at%.
Embodiment four
Take by weighing initial feed (0.5wt% aluminum isopropylate+99.5wt% polysilazane) 10g altogether, planetary ball mill is 12 hours in the nylon resin ball grinder of packing into, mixes to be placed in the 99 alumina-ceramic crucibles, at the N of 0.1MPa
2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing, obtain non-crystalline state SiAlCN solid with 10 ℃/min.The SiAlCN solid is packed in the nylon resin ball grinder, add the FeCl of 3wt%
2Powder carries out dry ball milling as catalyzer in high energy ball mill pulverized 24 hours, and the SiAlCN powder that obtains after then high-energy ball milling being pulverized places 99 alumina-ceramic crucibles, at (200ml/min) N that flows of 0.1MPa
2Be warmed up to 1700 ℃ with 10 ℃/min from room temperature under the atmosphere protection in tube furnace and carry out high temperature pyrolysis, be incubated 2 hours, furnace cooling is to room temperature then.The typical TEM of the adulterated SiC monocrystal nanowire of Al as shown in figure 10.Show the adulterated SiC monocrystal nanowire of Al mean diameter～250nm, any surface finish, even thickness, length are several μ m.The EDS detected result shows that the doping of Al is 0.88at%.
Embodiment five
Take by weighing initial feed (1wt% aluminum isopropylate+99wt% polysilazane) 10g altogether, planetary ball mill is 12 hours in the nylon resin ball grinder of packing into, mixes to be placed in the 99 alumina-ceramic crucibles, at the N of 0.1MPa
2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing, obtain non-crystalline state SiAlCN solid with 10 ℃/min.The SiAlCN solid is packed in the nylon resin ball grinder, add the FeCl of 3wt%
2Powder carries out dry ball milling as catalyzer in high energy ball mill pulverized 24 hours, and the SiAlCN powder that obtains after then high-energy ball milling being pulverized places 99 alumina-ceramic crucibles, at (200ml/min) N that flows of 0.1MPa
2Be warmed up to 1700 ℃ with 10 ℃/min from room temperature under the atmosphere protection in tube furnace and carry out high temperature pyrolysis, be incubated 2 hours, furnace cooling is to room temperature then.The typical TEM of the adulterated SiC monocrystal nanowire of Al shows the adulterated SiC monocrystal nanowire of Al mean diameter～350nm respectively as shown in figure 11, and any surface finish, even thickness, length are tens μ m.The EDS detected result shows that the doping of Al is 1.13at%.
The present invention proposes a kind of method of new employing organic precursor copyrolysis, ratio by two kinds of organic precursors of regulation and control initial feed, can be implemented on the molecular level regulation and control and design to SiC single-crystal low-dimension nano material doped level, thereby realize regulation and control, for certain basis is established in the research and development of its nano-device to performances such as SiC single-crystal low-dimension nano material photoelectricity.The equipment of method of the present invention and technology simple controllable, and have good repeatability, in synthetic SiC single-crystal low-dimension nano material, promptly realize mixing.This method realizes solid-liquid-gas-solid (Solid-Liquid-Gas-Solid:SLGS) growth mechanism of low-dimension nano material uniqueness is synthesized in the design of doping and regulation and control owing to this technology.
Claims (3)
1. novel method that the SiC single-crystal low-dimension nano material is controllable doped, it comprises following concrete steps:
1) aluminum isopropylate with polysilazane and 0.2～5wt% places nylon resin ball grinder ball milling to mix;
2) mix the back at N
2Carry out crosslinking curing in 260 ℃ of temperature under the atmosphere, obtain non-crystalline solids;
3) non-crystalline solids are packed in high energy ball mill, carry out dry ball milling in the nylon resin ball grinder and pulverize, introduce 3wt%FeCl simultaneously
2As catalyzer, make that non-crystalline state powder and catalyst mix are even;
4) mixture behind the high-energy ball milling under 1450-1700 ℃ of temperature in Ar or N
2High temperature pyrolysis is 2 hours under the atmosphere, can obtain having the SiC single-crystal low-dimension nano material of different al doping.
2. the controllable doped method of SiC single-crystal low-dimension nano material according to claim 1 is characterized in that: the raw material that uses in the described step (1) is organic precursor.
3. the controllable doped method of SiC single-crystal low-dimension nano material according to claim 2 is characterized in that: in described step (2) and (4), the protective atmosphere that is adopted is N
2Or Ar.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102041554B (en) * | 2011-01-19 | 2012-10-03 | 青岛大学 | Method for producing N-doped SiC nanowires with field emission properties |
| CN103352253B (en) * | 2013-01-15 | 2016-08-17 | 宁波工程学院 | A kind of regulate and control n-type SiC monocrystal low-dimension nano material doping content method |
| CN103255468B (en) * | 2013-01-15 | 2015-11-25 | 宁波工程学院 | A kind of preparation method of High purity silicon oxide/silicon carbide nanometer chain-like heterostructure |
| CN103928276B (en) * | 2014-04-29 | 2016-07-06 | 宁波工程学院 | A kind of method improving SiC filed emission cathode material high-temperature electronic launch stability |
| CN104445202B (en) * | 2014-11-25 | 2017-04-12 | 德清州晶新材料科技有限公司 | High-purity aluminum-doped silicon carbide powder and synthetic method thereof |
| CN104867799B (en) * | 2014-12-19 | 2017-02-22 | 青岛科技大学 | La in-situ doping one-dimensional nano SiC field emission material preparation method |
| 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 |
| CN113735593B (en) * | 2021-09-30 | 2022-09-30 | 陕西科技大学 | SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and preparation method thereof |
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