CN109437185B - Preparation method of nitrogen-containing semiconductor graphite - Google Patents
Preparation method of nitrogen-containing semiconductor graphite Download PDFInfo
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- CN109437185B CN109437185B CN201811528875.3A CN201811528875A CN109437185B CN 109437185 B CN109437185 B CN 109437185B CN 201811528875 A CN201811528875 A CN 201811528875A CN 109437185 B CN109437185 B CN 109437185B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 114
- 239000010439 graphite Substances 0.000 title claims abstract description 114
- 239000004065 semiconductor Substances 0.000 title claims abstract description 102
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 218
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 109
- 239000002245 particle Substances 0.000 claims abstract description 48
- 229910021382 natural graphite Inorganic materials 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 14
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 14
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 abstract description 10
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 230000005669 field effect Effects 0.000 description 47
- 239000007770 graphite material Substances 0.000 description 33
- 239000000463 material Substances 0.000 description 27
- 238000001237 Raman spectrum Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 11
- 238000001816 cooling Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- -1 magnesium nitride Chemical class 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- SJKRCWUQJZIWQB-UHFFFAOYSA-N azane;chromium Chemical compound N.[Cr] SJKRCWUQJZIWQB-UHFFFAOYSA-N 0.000 description 2
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- RRZKHZBOZDIQJG-UHFFFAOYSA-N azane;manganese Chemical compound N.[Mn] RRZKHZBOZDIQJG-UHFFFAOYSA-N 0.000 description 1
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 1
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 1
- AOPJVJYWEDDOBI-UHFFFAOYSA-N azanylidynephosphane Chemical compound P#N AOPJVJYWEDDOBI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- BIXHRBFZLLFBFL-UHFFFAOYSA-N germanium nitride Chemical compound N#[Ge]N([Ge]#N)[Ge]#N BIXHRBFZLLFBFL-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- AKJVMGQSGCSQBU-UHFFFAOYSA-N zinc azanidylidenezinc Chemical compound [Zn++].[N-]=[Zn].[N-]=[Zn] AKJVMGQSGCSQBU-UHFFFAOYSA-N 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
- H01L29/167—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table further characterised by the doping material
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- Microelectronics & Electronic Packaging (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Thin Film Transistor (AREA)
Abstract
The invention discloses a preparation method of nitrogen-containing semiconductor graphite, which is characterized in that the graphite is subjected to heat treatment in the temperature environment of 2000-3000 ℃, the activity of carbon atoms in the graphene surface is greatly increased, nitrogen elements in a nitrogen-containing nitrogen source are diffused to graphite particles under the drive of concentration gradient at high temperature, the difference between the atomic diameter of nitrogen and the diameter of carbon atoms is not large, the carbon atoms are replaced by the nitrogen atoms at high temperature, the substitutional doping of the nitrogen atoms is realized, and the nitrogen-element in-situ substitutional doped semiconductor graphite is obtained.
Description
Technical Field
The invention belongs to the technical field of graphite modification, and particularly relates to a preparation method of nitrogen-containing semiconductor graphite.
Background
In 2004, geom et al first used a micromechanical lift-off process to prepare a single-layer graphene sheet layer, and used graphene as a channel material to prepare a field effect transistor, and found that graphene has very high carrier mobility. Graphene, as a first two-dimensional material discovered, has attracted a great deal of attention and research from researchers. The honeycomb two-dimensional plane crystal formed by a layer of carbon atoms has excellent properties such as: high carrier mobility, saturated drift velocity, submicron ballistic transport performance, excellent mechanical performance, high thermal conductivity and high transparency. As silicon integrated circuit line widths have reached 7-10nm, quantum tunneling effects have limited, leading to moore's law failure in the near future. Due to the extremely high carrier mobility, high thermal conductivity, high stability and the like of the graphene, the graphene is expected to replace silicon and becomes a next-generation integrated circuit material.
The preparation methods of graphene are many, such as: methods such as micro-mechanical stripping, silicon carbide pyrolysis, gas-phase chemical deposition, oxidation reduction, chemical synthesis and the like have the problems of difficult preparation, high cost, complex process, more defects and the like, and the wide application of graphene in the fields of electronic circuits and the like cannot be realized.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of nitrogen-containing semiconductor graphite.
The technical scheme of the invention is as follows:
a preparation method of nitrogen-containing semiconductor graphite comprises the following steps: and mixing a nitrogen source with the graphite particles, and then treating at the constant temperature of 3000 ℃ of 2000-1000 min, wherein in the process, nitrogen element is diffused to the graphite particles under the drive of the concentration gradient in the graphite particles to obtain the nitrogen-containing semiconductor graphite.
In a preferred embodiment of the invention, the method further comprises the step of carrying out ultrasonic treatment or micromechanical stripping on the nitrogen-containing semiconductor graphite.
Further preferably, the ultrasonic treatment is ultrasonic treatment in water, ethanol or DMF.
In a preferred embodiment of the present invention, the graphite particles are natural graphite particles, artificial graphite particles, or carbon source particles that can be converted into graphite at 2000-3000 ℃.
Further preferably, the artificial graphite particles are highly oriented pyrolytic graphite particles.
In a preferred embodiment of the present invention, the nitrogen source comprises at least one of nitrogen, ammonia, silicon nitride, polyacrylonitrile, melamine, magnesium nitride, calcium nitride, carbon nitride, titanium nitride, zirconium nitride, hafnium nitride, vanadium nitride, niobium nitride, chromium nitride, molybdenum nitride, tungsten nitride, aluminum nitride, germanium nitride, vanadium nitride, copper nitride, chromium nitride, zinc nitride, iron nitride, manganese nitride, and phosphorus pentanitride.
Further preferably, the nitrogen source is at least one of silicon nitride, titanium nitride, and nitrogen carbide.
In a preferred embodiment of the present invention, the mass ratio of the nitrogen element in the nitrogen source to the graphite particles is 0.2-50: 100.
In a preferred embodiment of the present invention, the constant temperature treatment is carried out at 2400-3000 ℃ for 10-60 min.
The invention has the beneficial effects that:
1. according to the method, graphite is subjected to heat treatment in the temperature environment of 2000-3000 ℃, the activity of carbon atoms in the graphene surface is greatly increased, nitrogen elements in a nitrogen-containing nitrogen source are diffused to graphite particles under the drive of a concentration gradient at high temperature, the difference between the atomic diameter of nitrogen and the atomic diameter of carbon is not large, the carbon atoms are replaced by the nitrogen atoms at high temperature, the replacement doping of the nitrogen atoms is realized, the nitrogen-element in-situ replacement doped semiconductor graphite is obtained, the nitrogen-element in-situ replacement doped semiconductor graphite is used as a channel material to prepare a field effect tube, and a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube.
2. The method is simple, realizes the regulation of the nitrogen content in the graphite by regulating the temperature and the constant temperature time of the graphitization furnace and the proportion of the natural graphite particles and the nitrogen source, is easy to realize continuous preparation, and has the characteristics of low cost, easy scale production and the like.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
In the following embodiments, the graphite field effect transistor uses gold as a source/drain electrode, a back gate is a heavily doped P-type silicon wafer, and an insulating layer is SiO2And the thickness is 300 nm.
Example 1
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 2800 ℃, the constant temperature time is 30min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 0.77% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 32230-34020cm2between/V.s.
Example 2
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 30min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around, and the nitrogen content was 0.88% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 34120-35200cm2between/V.s.
Example 3
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 100min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 0.94% by XPS analysis. Preparing field effect transistor from the nitrogen-containing semiconductor graphiteAs a channel material, the channel material is tested by using a semiconductor integrated tester keithlchcy 4200A SCS, and the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 35400-37700cm2between/V.s.
Example 4
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 1min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 0.49% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 26980-29600cm2between/V.s.
Example 5
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 1000min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The preparation of the field effect transistor is carried out by taking the nitrogen-containing semiconductor graphite as a channel material and carrying out a graphite field by utilizing a semiconductor comprehensive tester keithley 4200A SCSAnd testing an effect tube, wherein the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around, and the nitrogen content was 1.05% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 31700-34500cm2between/V.s.
Example 6
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 60min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 30: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 1.82% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 31360-33800cm2between/V.s.
Example 7
Mixing natural graphite particles and nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), heating natural graphite particles and nitrogen source in a high temperature furnace at 3000 deg.C for 60minThe mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen element in the nitrogen source) to the natural graphite particles is 50:100, and the nitrogen-containing semiconductor graphite is obtained after the high-temperature furnace is cooled. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared in the vicinity, and the nitrogen content was 2.21% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 26250 and 28320cm2between/V.s.
Example 8
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 60min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 0.2: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a raman spectrum with a D peak which is not particularly significant, and the nitrogen content is 0.09% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 19950 and 20210cm2between/V.s.
Example 9
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 3000 ℃, the constant temperature time is 60min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 20: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 1.92% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 34420-36670cm2between/V.s.
Example 10
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 2000 ℃, the constant temperature time is 60min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 10: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 0.34% by XPS analysis. The nitrogen-containing semiconductor is formedPreparing a field effect transistor by using graphite, taking the graphite as a channel material, and then testing by using a semiconductor comprehensive tester keithley 4200A SCS, wherein the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 21630-23020cm2between/V.s.
Example 11
Uniformly mixing natural graphite particles and a nitrogen source (at least one of silicon nitride, titanium nitride and nitrogen carbide), then placing the mixture into a high-temperature furnace to heat the natural graphite particles and the nitrogen source, wherein the temperature of the high-temperature furnace is 2400 ℃, the constant temperature time is 120min, the mass ratio of the effective content of nitrogen (the effective content of nitrogen refers to the mass of nitrogen elements in the nitrogen source) to the natural graphite particles is 20: 100, and cooling the high-temperature furnace to obtain the nitrogen-containing semiconductor graphite. The nitrogen-containing semiconductor graphite is used as a channel material for preparing a field effect tube, a semiconductor comprehensive tester keithley 4200A SCS is used for testing the graphite field effect tube, and the nitrogen-doped graphite material obtained by the method is N-type semiconductor graphite. The obtained nitrogen-containing semiconductor graphite has a high D peak in Raman spectrum of 1620cm-1A D' peak appeared around the peak, and the nitrogen content was 0.86% by XPS analysis. The nitrogen-containing semiconductor graphite is used for preparing a field effect transistor, the graphite is used as a channel material, and then a semiconductor comprehensive tester keithley 4200A SCS is used for testing, so that the conclusion is that the prepared nitrogen-doped graphite material is an N-type semiconductor graphite material. The carrier mobility of the graphite field effect transistor is 25530-27650cm2between/V.s.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (3)
1. A preparation method of nitrogen-containing semiconductor graphite is characterized by comprising the following steps: the method comprises the following steps: mixing a nitrogen source with natural graphite particles, and then carrying out constant temperature treatment at 3000 ℃ of 2400-; the nitrogen source is at least one of silicon nitride, titanium nitride and nitrogen carbide; the mass ratio of nitrogen element in the nitrogen source to the natural graphite particles is 0.2-50: 100.
2. The method of claim 1, wherein: the method also comprises the step of carrying out ultrasonic treatment or micromechanical stripping on the nitrogen-containing semiconductor graphite.
3. The method of claim 2, wherein: the ultrasonic treatment is ultrasonic treatment in water, ethanol or DMF.
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| CN102034975A (en) * | 2010-11-15 | 2011-04-27 | 中国科学院青岛生物能源与过程研究所 | Nitrogen-doped graphite carbon serving as anode material of lithium ion battery, and preparation method and application thereof |
| CN104667953A (en) * | 2013-11-29 | 2015-06-03 | 中国科学院过程工程研究所 | Nitrogen-doped graphdiyne as well as preparation method and application thereof |
| CN105417532A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | One-step preparation method for high nitrogen doped graphene |
| CN105752973A (en) * | 2016-03-31 | 2016-07-13 | 常州大学 | Method for preparing nitrogen-doped graphene material in electrochemical stripping mode |
| WO2017101470A1 (en) * | 2015-12-18 | 2017-06-22 | 华为技术有限公司 | Negative electrode active material of lithium ion secondary battery and preparation method therefor, negative electrode plate of lithium ion secondary battery, and lithium ion secondary battery |
| CN108658064A (en) * | 2018-08-08 | 2018-10-16 | 广东电网有限责任公司 | A kind of nitrogen-doped graphene and preparation method thereof |
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| CN104667953A (en) * | 2013-11-29 | 2015-06-03 | 中国科学院过程工程研究所 | Nitrogen-doped graphdiyne as well as preparation method and application thereof |
| WO2017101470A1 (en) * | 2015-12-18 | 2017-06-22 | 华为技术有限公司 | Negative electrode active material of lithium ion secondary battery and preparation method therefor, negative electrode plate of lithium ion secondary battery, and lithium ion secondary battery |
| CN105417532A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | One-step preparation method for high nitrogen doped graphene |
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