CN108914086A - Fe2O3 doping diamond dilute magnetic semiconductor and preparation method thereof - Google Patents
Fe2O3 doping diamond dilute magnetic semiconductor and preparation method thereof Download PDFInfo
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- CN108914086A CN108914086A CN201810786224.8A CN201810786224A CN108914086A CN 108914086 A CN108914086 A CN 108914086A CN 201810786224 A CN201810786224 A CN 201810786224A CN 108914086 A CN108914086 A CN 108914086A
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- 239000010432 diamond Substances 0.000 title claims abstract description 83
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 82
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 52
- 239000004065 semiconductor Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000758 substrate Substances 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 31
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims abstract description 29
- 229910052742 iron Inorganic materials 0.000 claims abstract description 27
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 28
- 239000002243 precursor Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 22
- 230000008021 deposition Effects 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 230000005284 excitation Effects 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000008236 heating water Substances 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000011435 rock Substances 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract description 2
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 17
- 229910052710 silicon Inorganic materials 0.000 description 17
- 239000010703 silicon Substances 0.000 description 17
- 230000006911 nucleation Effects 0.000 description 7
- 238000010899 nucleation Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 5
- 229920000314 poly p-methyl styrene Polymers 0.000 description 5
- 206010063401 primary progressive multiple sclerosis Diseases 0.000 description 5
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010348 incorporation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000005307 ferromagnetism Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- -1 acyl acetone iron Chemical compound 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/278—Diamond only doping or introduction of a secondary phase in the diamond
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/276—Diamond only using plasma jets
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N50/00—Galvanomagnetic devices
- H10N50/80—Constructional details
- H10N50/85—Magnetic active materials
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- Chemical & Material Sciences (AREA)
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- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of Fe2O3 doping diamond dilute magnetic semiconductors and preparation method thereof, it is using ferric acetyl acetonade as source of iron, dehydrated alcohol is as carbon source, ferric acetyl acetonade is introduced into microwave plasma CVD device by dehydrated alcohol, Fe2O3 doping diamond is grown in substrate, ferro element is introduced into dilute magnetic diamond by realization.The present invention is introduced into for the first time using ferric acetyl acetonade as source of iron by the dehydrated alcohol of volatilization, prepares dilute magnetic diamond semiconductor using MPCVD method, and successful growth is out at room temperature with the diamond of ferromagnetic effects.And it was found that with the increase of source of iron dosage, the phenomenon that a kind of rising is presented in the magnetic intensity of diamond.Be conducive to the dilute magnetic semiconductor characteristic for farthest probing into Fe2O3 doping diamond for its research, while being also beneficial to explore the magnetic-doped more possibilities of diamond.
Description
Technical field
The invention belongs to the present invention relates to dilute magnetic semiconductor preparation fields, and in particular to a kind of at room temperature to there is dilute magnetic partly to lead
Fe2O3 doping diamond of bulk properties and preparation method thereof.
Background technique
Dilute magnetic semiconductor is a kind of spin source with important prospect, is the important support material of self-spining device of new generation.
Only before half a century, a limited computer of function, which arrives greatly, will take whole room, and today, in our pocket just
It is filled with powerful " electronic equipment ".People are to have no limits for the pursuit of the electronic equipment of miniaturization and more power
, however, heat dissipation and technological difficulties, such as tunnel-effect, affect the further development of traditional silicon-based transistor.Researcher
Continually look for solution,, can be with because mobile to specific charge wherein very potential method is exactly spintronics
Electron spin overturning is controlled using less energy.However, Schmidt et al. is once made using transition metal (such as Ni, Co)
It is injected into channel semiconductor for spin source, because of the reasons such as mismatch, the efficiency for injection of spinning is very low (being lower than 5%), and
It is not easily detected；And utilizing magnetic element doping to obtain the polarized dilute magnetic semiconductor that spins has very high Spin Injection Efficiency
(being higher than 90%).Therefore, magnetic element incorporation semiconductor becomes the object most studied extensively, such as reported magnetic ion Mn
The dilute magnetic semiconductors such as the GaAs of doping, GaN and transition metal element doped zno-based dilute magnetic semiconductor.
Diamond has that forbidden band is wide, disruptive field intensity is high, carrier mobility is high, dielectric constant is low and good heat conductivity etc. is excellent
Different performance, while the features such as have both stable chemical property, high rigidity, strong wearability and capability of resistance to radiation, it is that one kind has hair
High temperature, the high-power semiconductor material with wide forbidden band for opening up future, are known as forth generation semiconductor preferred material.Therefore, to Fe2O3 doping
The preparation process of diamond thin explore and is of great significance.However, not having the document and patent of this diamond-like at present
Report, it is very sensitive to growth parameter(s) because such diamond growth conditions are complicated, so being difficult to obtain by conventional method.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of Fe2O3 doping in view of the deficiency of the prior art
Iron is successfully mixed diamond thin by diamond dilute magnetic semiconductor and preparation method thereof, and with the increase of iron incorporation,
The variation tendency risen is presented in the magnetic intensity of diamond thin, can get Buddha's warrior attendant at room temperature with dilute magnetic semiconductor characteristic
Stone.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, it is using ferric acetyl acetonade as source of iron, dehydrated alcohol conduct
Ferric acetyl acetonade is introduced into microwave plasma CVD device by dehydrated alcohol, is grown in substrate by carbon source
Ferro element is introduced into diamond thin by Fe2O3 doping diamond thin, realization, obtains Fe2O3 doping diamond dilute magnetic semiconductor.
According to the above scheme, the substrate is cleaned by ultrasonic using diamond suspension in advance, increases silicon chip surface energy, benefit
In diamond nucleation.For example, the substrate is selected from silicon wafer etc..
According to the above scheme, ferric acetyl acetonade is dissolved in dehydrated alcohol, is passed through microwave plasma by heating volatilization
Learn the deposition chamber of vapor phase growing apparatus.Wherein, concentration of the ferric acetyl acetonade in dehydrated alcohol is 0.25~2.5g/L；Heating
Volatilization can be carried out by the mixed solution of heating water bath ferric acetyl acetonade and dehydrated alcohol, and heating temperature range is 35~50
℃。
It is further preferred that ferric acetyl acetonade is dissolved in dehydrated alcohol, pass through the carrying of heating volatilization and inert carrier gas
It is passed through the deposition chamber of microwave plasma CVD device.Wherein, the flow of inert carrier gas is 5~10sccm, lazy
Property carrier gas can choose the rare gas such as argon gas.
According to the above scheme, the technological parameter of microwave plasma CVD device is：It is passed through into deposition chamber
Hydrogen adjusts air pressure in microwave power and vacuum chamber, and excitation generates plasma, and hydrogen flowing quantity is 100~200sccm, microwave
Power is 700~1100W, and operating air pressure is 10~12kPa, and substrate temperature is 700~900 DEG C, reaction time 6-28h.
Preferably, main the present invention also provides a kind of preparation method of more specifically Fe2O3 doping diamond dilute magnetic semiconductor
Want that steps are as follows：
1) substrate pretreatment：Substrate (such as silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate table
Face energy, is conducive to diamond nucleation；
2) preparation of precursor solution：For ferric acetyl acetonade as source of iron, dehydrated alcohol is molten by ferric acetyl acetonade as carbon source
Solution obtains precursor solution in the dehydrated alcohol in conical flask；
3) device prepares：It is put into substrate in the deposition chamber of microwave plasma CVD device, to cavity
It vacuumizes (being 10-100Pa to vacuum degree), is passed through hydrogen in cavity, adjusts air pressure in microwave power and vacuum chamber, excitation generates
Plasma, the technological parameter used are：Hydrogen flowing quantity is 100~200sccm, and microwave power is 700~1100W, work gas
Pressure is 10~12kPa, and substrate temperature is 700~900 DEG C；
4) heating water bath is carried out to precursor solution, heating temperature is 35~50 DEG C, to increase the volatilization of solution；It is passed through load
Gas, carrier gas channel flow through precursor solution, can both increase the volatilization of solution, are also conducive to the transmission of ferric acetyl acetonade, the work used
Skill parameter is：Argon flow is 0-10sccm, and the concentration of acyl acetone iron and dehydrated alcohol mixed solution is 0.25~2.5g/L；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, and reaction time 6-28h obtains iron
Doped diamond thin films.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is introduced into for the first time using ferric acetyl acetonade as source of iron by the dehydrated alcohol of volatilization, using microwave etc.
Gas ions chemical vapour deposition technique prepares dilute magnetic diamond thin, and successful growth has partly leading for ferromagnetic effects at room temperature out
Body diamond film.This method has the introduction volume of source of iron easily controllable；Also, using microwave plasma to gaseous component into
Row reduction, due to the high-power height of microwave energy density, makes gas be easier to dissociate, and group has greater activity, conducive to iron
Doping.
Secondly, the Fe2O3 doping diamond thin that through the invention prepared by the method, with the increase of iron incorporation, Buddha's warrior attendant
The phenomenon that a kind of rising is presented in the magnetic intensity of stone film is conducive to farthest probe into the intrinsic of Fe2O3 doping diamond thin
Physical property, while being also beneficial to explore the magnetic-doped more possibilities of diamond.
Furthermore the method for the invention plasma is covered on above substrate, provides enough temperature for substrate, etc.
The self-heating mode of gas ions promotes group in the deposition of silicon chip surface；In addition, the method for the present invention also has microwave power can
The advantages that tune, deposition pressure is lower.
Detailed description of the invention
Fig. 1 is the optical photograph of Fe2O3 doping diamond dilute magnetic semiconductor prepared by the present invention.
Fig. 2 is the apparatus structure schematic diagram that the present invention prepares Fe2O3 doping diamond thin, wherein 1, microwave source；2, vacuum
Pumping port；3, vacuum chamber；4, water bath heating device；5, chip bench；6, cylindrical quartz pipe；7, it is dissolved with ferric acetyl acetonade
Ethanol solution；8, argon bottle；9, gas cylinder pressure reducing valve；10, hydrogen cylinder.
Fig. 3 is the electron spectrum test chart of #2 sample in embodiment.
Fig. 4 is the electron spectrum test chart of #3 sample in embodiment.
Fig. 5 is the electron spectrum test chart of #5 sample in embodiment.
Specific embodiment
Further the present invention will be described with reference to the accompanying drawings and examples, but the contents of the present invention are not limited solely to
The following examples.
The present invention provides a kind of device for preparing Fe2O3 doping diamond dilute magnetic semiconductor, but be not restricted to that the device is realized
Technical solution of the present invention, any device that can be realized technical solution of the present invention.
As shown in Fig. 2, in following embodiments, the device for preparing Fe2O3 doping diamond thin includes：1, microwave source；2, vacuum
Pumping port；3, vacuum chamber；4, water bath heating device；5, chip bench；6, cylindrical quartz pipe；7, it is dissolved with ferric acetyl acetonade
Ethanol solution；8, argon bottle；9, gas cylinder pressure reducing valve；10, hydrogen cylinder.Vacuum pump bleeding point 2 is by vacuum pipe and vacuum
It pumps and is connected (for vacuumizing the air in chamber 3 to vacuum), vacuum pipe is equipped with vacuum fine adjustment valve；Hydrogen Line and vacuum
Chamber 3 is connected, and vacuum chamber 3 is cylinder, and (close to the position of silicon wafer, silicon wafer is located at true at the periphery middle part of vacuum chamber 3
On the chip bench at 3 center of plenum chamber) it is equipped with cylindrical quartz pipe 6；The microwave of 2.45GHz is entered by microwave source 1 through quartz ampoule 6 true
Coupling in plenum chamber 3 after gas enters cavity, absorbs microwave energy ionization and generates plasma；Ferric acetyl acetonade is by volatilizing
Ethyl alcohol and argon gas bring vacuum chamber 3 into through pipeline.
Embodiment 1
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, specific step is as follows：
1) substrate pretreatment：Substrate (silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate surface energy,
Conducive to diamond nucleation；
2) preparation of precursor solution：Ferric acetyl acetonade is as source of iron, and dehydrated alcohol is as carbon source, by 0.1g acetylacetone,2,4-pentanedione
Dissolved ferric iron obtains precursor solution in the 400ml dehydrated alcohol in conical flask；
3) device prepares：In the deposition chamber of microwave plasma CVD device, silicon wafer is placed in substrate
Platform upper center position vacuumizes (being 10-100Pa to vacuum degree) to cavity, hydrogen is passed through into cavity, adjusts microwave power
With air pressure in vacuum chamber, excitation generates plasma, and the technological parameter used is：Hydrogen flowing quantity is 200sccm, and microwave power is
800W, operating air pressure 11kPa, substrate temperature are 800 DEG C；
4) constant temperature water bath heating is carried out to the conical flask for filling precursor solution, heating temperature is 45 DEG C, and argon flow
For 0sccm；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, reaction time 6h, closes microwave
Source, gas source, power supply, cooling water, it is cooling to cavity, it takes out sample, obtains Fe2O3 doping diamond thin (labeled as #1 sample).
The magnetic property of Fe2O3 doping diamond thin is tested by comprehensive physical property measuring system PPMS, after tested after, discovery
There is no magnetism for the #1 sample.
Embodiment 2
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, specific step is as follows：
1) substrate pretreatment：Substrate (silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate surface energy,
Conducive to diamond nucleation；
2) preparation of precursor solution：Ferric acetyl acetonade is as source of iron, and dehydrated alcohol is as carbon source, by 0.2g acetylacetone,2,4-pentanedione
Dissolved ferric iron obtains precursor solution in the 400ml dehydrated alcohol in conical flask；
3) device prepares：In the deposition chamber of microwave plasma CVD device, silicon wafer is placed in substrate
Platform upper center position vacuumizes (being 10-100Pa to vacuum degree) to cavity, hydrogen is passed through into cavity, adjusts microwave power
With air pressure in vacuum chamber, excitation generates plasma, and the technological parameter used is：Hydrogen flowing quantity is 200sccm, and microwave power is
800W, operating air pressure 11kPa, substrate temperature are 800 DEG C；
4) constant temperature water bath heating being carried out to the conical flask for filling precursor solution, heating temperature is 45 DEG C, and is passed through argon gas,
Argon flow is 5sccm；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, reaction time 10h, closes microwave
Source, gas source, power supply, cooling water, it is cooling to cavity, it takes out sample, obtains Fe2O3 doping diamond thin (labeled as #2 sample).
The magnetic property of Fe2O3 doping diamond thin is tested by comprehensive physical property measuring system PPMS, after tested after, discovery
There is no magnetism for the #2 sample.Fig. 3 is the electron spectrum test chart of the #2 sample, iron content 0.054wt%.
Embodiment 3
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, specific step is as follows：
1) substrate pretreatment：Substrate (silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate surface energy,
Conducive to diamond nucleation；
2) preparation of precursor solution：Ferric acetyl acetonade is as source of iron, and dehydrated alcohol is as carbon source, by 0.2g acetylacetone,2,4-pentanedione
Dissolved ferric iron obtains precursor solution in the 400ml dehydrated alcohol in conical flask；
3) device prepares：In the deposition chamber of microwave plasma CVD device, silicon wafer is placed in substrate
Platform upper center position vacuumizes (being 10-100Pa to vacuum degree) to cavity, hydrogen is passed through into cavity, adjusts microwave power
With air pressure in vacuum chamber, excitation generates plasma, and the technological parameter used is：Hydrogen flowing quantity is 200sccm, and microwave power is
800W, operating air pressure 11kPa, substrate temperature are 800 DEG C；
4) constant temperature water bath heating being carried out to the conical flask for filling precursor solution, heating temperature is 45 DEG C, and is passed through argon gas,
Argon flow is 5sccm；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, reaction time 15h, closes microwave
Source, gas source, power supply, cooling water, it is cooling to cavity, sample is taken out, obtaining Fe2O3 doping diamond thin, (i.e. Fe2O3 doping diamond is dilute
Magnetic semiconductor is labeled as #3 sample).
The magnetic property of Fe2O3 doping diamond thin is tested by comprehensive physical property measuring system PPMS, after tested after, discovery
The #3 sample shows faint ferromagnetism at low temperature.
Fig. 4 is the electron spectrum test chart of the #3 sample, iron content 0.199wt%.
Embodiment 4
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, specific step is as follows：
1) substrate pretreatment：Substrate (silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate surface energy,
Conducive to diamond nucleation；
2) preparation of precursor solution：Ferric acetyl acetonade is as source of iron, and dehydrated alcohol is as carbon source, by 0.4g acetylacetone,2,4-pentanedione
Dissolved ferric iron obtains precursor solution in the 400ml dehydrated alcohol in conical flask；
3) device prepares：In the deposition chamber of microwave plasma CVD device, silicon wafer is placed in substrate
Platform upper center position vacuumizes (being 10-100Pa to vacuum degree) to cavity, hydrogen is passed through into cavity, adjusts microwave power
With air pressure in vacuum chamber, excitation generates plasma, and the technological parameter used is：Hydrogen flowing quantity is 200sccm, and microwave power is
800W, operating air pressure 11kPa, substrate temperature are 800 DEG C；
4) constant temperature water bath heating being carried out to the conical flask for filling precursor solution, heating temperature is 45 DEG C, and is passed through argon gas,
Argon flow is 5sccm；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, reaction time 20h, closes microwave
Source, gas source, power supply, cooling water, it is cooling to cavity, sample is taken out, obtaining Fe2O3 doping diamond thin, (i.e. Fe2O3 doping diamond is dilute
Magnetic semiconductor is labeled as #4 sample).
The magnetic property of Fe2O3 doping diamond thin is tested by comprehensive physical property measuring system PPMS, after tested after, discovery
The #4 sample shows weak ferromagnetism at low temperature.
Embodiment 5
The preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, specific step is as follows：
1) substrate pretreatment：Substrate (silicon wafer) is cleaned by ultrasonic using diamond suspension, increases substrate surface energy,
Conducive to diamond nucleation；
2) preparation of precursor solution：Ferric acetyl acetonade is as source of iron, and dehydrated alcohol is as carbon source, by 0.5g acetylacetone,2,4-pentanedione
Dissolved ferric iron obtains precursor solution in the 400ml dehydrated alcohol in conical flask；
3) device prepares：In the deposition chamber of microwave plasma CVD device, silicon wafer is placed in substrate
Platform upper center position vacuumizes (being 10-100Pa to vacuum degree) to cavity, hydrogen is passed through into cavity, adjusts microwave power
With air pressure in vacuum chamber, excitation generates plasma, and the technological parameter used is：Hydrogen flowing quantity is 200sccm, and microwave power is
800W, operating air pressure 11kPa, substrate temperature are 800 DEG C；
4) constant temperature water bath heating being carried out to the conical flask for filling precursor solution, heating temperature is 45 DEG C, and is passed through argon gas,
Argon flow is 5sccm；
5) vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, simultaneously
Stablize plasmoid, the technological parameter used is：Intracavitary air pressure is 10~12kPa, reaction time 28h, closes microwave
Source, gas source, power supply, cooling water, it is cooling to cavity, sample is taken out, obtaining Fe2O3 doping diamond thin, (i.e. Fe2O3 doping diamond is dilute
Magnetic semiconductor is labeled as #5 sample).
The magnetic property of Fe2O3 doping diamond thin is tested by comprehensive physical property measuring system PPMS, after tested after, discovery
The #5 sample has ferromagnetic effects, forbidden bandwidth 1.49eV at room temperature.
Fig. 5 is the electron spectrum test chart of the #5 sample, iron content 0.46wt%.
Above-described embodiment 1-5 prepares 5 samples, and detail parameters are as shown in table 1.As shown in Table 1：Relative to embodiment 1
For, ar gas acting is not only conducive to the transmission of ferric acetyl acetonade in embodiment 2-5, but also can increase the volatilization of solution, this is all
The introduction volume of iron can be increased；In 5 samples, with being incremented by for precursor solution concentration and time, the dosage of source of iron is successively increased,
In conjunction with the Magnetic Test result of each sample, it is possible to find, with the increase of source of iron dosage, the magnetic intensity of diamond thin is presented one
The phenomenon that kind rises.But as the content of iron in embodiment 1-5 increases, the miscellaneous phase in diamond sample is increase accordingly, and institute
It is still excellent diamonds sample that must have at room temperature, which has No. 5 samples of dilute magnetic semiconductor characteristic,.
Table 1
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (10)
1. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor, it is characterised in that it is anhydrous using ferric acetyl acetonade as source of iron
Ferric acetyl acetonade is introduced into microwave plasma CVD device by ethyl alcohol as carbon source, by dehydrated alcohol, in base
Fe2O3 doping diamond thin is grown on bottom, obtains Fe2O3 doping diamond dilute magnetic semiconductor.
2. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 1, it is characterised in that acetylacetone,2,4-pentanedione
The deposition chamber that dissolved ferric iron is passed through microwave plasma CVD device in dehydrated alcohol, by heating volatilization.
3. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 1, it is characterised in that acetylacetone,2,4-pentanedione
Dissolved ferric iron is passed through microwave plasma CVD dress in dehydrated alcohol, through heating volatilization and the carrying of inert carrier gas
The deposition chamber set.
4. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 2 or 3, it is characterised in that levulinic
Concentration of the ketone iron in dehydrated alcohol is 0.25 ~ 2.5g/L.
5. a kind of preparation method of Fe2O3 doping diamond thin according to claim 2 or 3, it is characterised in that pass through water-bath
The mixed solution for heating ferric acetyl acetonade and dehydrated alcohol, accelerates its volatilization, and water bath heating temperature range is 35 ~ 50 DEG C.
6. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 3, it is characterised in that inert carrier gas
Flow be 5 ~ 10sccm.
7. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 1, it is characterised in that microwave etc. from
The technological parameter of daughter chemical vapor deposition unit is：It is passed through hydrogen into deposition chamber, adjusts in microwave power and vacuum chamber
Air pressure, excitation generate plasma, hydrogen flowing quantity be 100 ~ 200sccm, microwave power be 700 ~ 1100W, operating air pressure be 10 ~
12kPa, substrate temperature are 700 ~ 900 DEG C, reaction time 6-28h.
8. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 1, it is characterised in that the substrate
It is cleaned by ultrasonic in advance using diamond suspension.
9. the preparation method of Fe2O3 doping diamond dilute magnetic semiconductor according to claim 1, it is characterised in that key step
It is as follows：
1）Substrate pretreatment：Substrate is cleaned by ultrasonic using diamond suspension, increases substrate surface energy, is conducive to diamond
Forming core；
2）The preparation of precursor solution：Ferric acetyl acetonade is dissolved in as source of iron, dehydrated alcohol as carbon source by ferric acetyl acetonade
In dehydrated alcohol in conical flask, precursor solution is obtained；
3）Device prepares：It is put into substrate in the deposition chamber of microwave plasma CVD device, cavity is taken out true
Sky is passed through hydrogen in cavity, adjusts air pressure in microwave power and vacuum chamber, and excitation generates plasma, the technological parameter used
For：Hydrogen flowing quantity is 100 ~ 200sccm, and microwave power is 700 ~ 1100W, and operating air pressure is 10 ~ 12kPa, substrate temperature 700
~900℃；
4）Heating water bath is carried out to precursor solution, heating temperature is 35 ~ 50 DEG C, to increase the volatilization of solution；It is passed through carrier gas, is carried
Feed channel flows through precursor solution, can both increase the volatilization of solution, is also conducive to the transmission of ferric acetyl acetonade, the technological parameter used
For：Argon flow is 0-10sccm, and the concentration of ferric acetyl acetonade and dehydrated alcohol mixed solution is 0.25 ~ 2.5g/L；
5）The vacuum fine adjustment valve for adjusting deposition chamber keeps the intracorporal air pressure of deposit cavity within limits, while making
Gas ions are in stable condition, and the technological parameter used is：Intracavitary air pressure is 10 ~ 12kPa, reaction time 6-28h, obtains Fe2O3 doping gold
Hard rock film, i.e. Fe2O3 doping diamond dilute magnetic semiconductor.
10. Fe2O3 doping diamond dilute magnetic semiconductor prepared by method described in claim 1.
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| CN114059159A (en) * | 2021-11-18 | 2022-02-18 | 北京大学东莞光电研究院 | Diamond growth method |
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