CN110344025A - A kind of two dimension Zn doping Ca2Si nano thin-film and its chemical vapor deposition method - Google Patents
A kind of two dimension Zn doping Ca2Si nano thin-film and its chemical vapor deposition method Download PDFInfo
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- CN110344025A CN110344025A CN201910816710.4A CN201910816710A CN110344025A CN 110344025 A CN110344025 A CN 110344025A CN 201910816710 A CN201910816710 A CN 201910816710A CN 110344025 A CN110344025 A CN 110344025A
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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
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- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/42—Silicides
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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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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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
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Abstract
The invention belongs to low-dimensional nano film material fields, and in particular to a kind of two dimension Zn doping Ca2Si nano thin-film and its chemical vapor deposition method.Silica dish equipped with Ca powder is placed on to the front end area of three-temperature-zone high temperature process furnances, the silica dish equipped with Zn powder is placed on to the intermediate region of three-temperature-zone high temperature process furnances, pretreated substrate of glass is placed on the terminal region of three-temperature-zone high temperature process furnances.In argon gas and SiH4Carrier gas under, with front end, centre and the terminal region of certain heating rate heating three-temperature-zone tube furnace, reaction a period of time, reaction product is deposited in substrate of glass, reaction product is carried out to in-situ annealing processing in tube furnace again, obtains two-dimentional Zn doping Ca2Si layer material.This method preparation process is simple, and product purity is higher, is expected to can be realized extensive, high quality two-dimentional Zn doping Ca2The production of Si nano thin-film has good industrialization prospect.
Description
Technical field
The invention belongs to low-dimensional nano film material fields, and in particular to a kind of two dimension Zn doping Ca2Si nano thin-film and
The preparation method of chemical vapour deposition technique.
Background technique
Two-dimensional material is because its carrier mobility and heat diffusion are all limited in two-dimensional surface, so that this material shows
Many peculiar properties out.The fields such as the adjustable characteristic scene effect pipe of its band gap, photoelectric device, thermo-electric device are widely used；
The controllability of its spin freedom degree and paddy freedom degree causes to further investigate in spintronics and paddy person in electronics；Different two
Tie up the anisotropy of the material electrology characteristic or optical characteristics different since the special nature of crystal structure results in, including Raman
The anisotropy of the properties such as spectrum, photoluminescence spectra, the second harmonic spectrum, optical absorption spectra, thermal conductivity, conductivity, in polarised light
The fields such as electrical part, polarization thermo-electric device, bionical device, polarization optical detection have very big development potentiality.
Alkaline earth metal silicide Ca2Si material, direct band gap are about 0.31 eV, are Ca, the Si extremely long by resource longevity
Element composition, can recycle, pollution-free to the earth, and due to calcium silicon compound Ca2Si has excellent with existing silicon-based technologies
Good compatibility, it is considered to be very promising novel environmental close friend semiconductor material, in solar battery and thermoelectric conversion
Equal fields have potential application prospect.Compared with block materials, two-dimensional material has more advantages, such as it has preferably
Flexibility and high transparency, therefore, two-dimensional material has a extensive future corresponding field.Two-dimentional CaC2Phase under high pressure
Change causes higher concern, and the physical properties such as superior electric conductivity and superconductivity are studied；CaP3Nano thin-film is
A kind of two-dimensional functional material of new prediction not only with the direct band gap of 1.15 eV, but also has up to 19930 cm2·V-1·s-1Electron mobility, be for nanoelectronic application the functional material being highly desirable to.Two-dimentional Ca2Si is in environmental condition
Under it is with good stability, and show the anisotropy carrier mobility along different directions, this high carrier migration
Rate shows two-dimentional Ca2Si nano thin-film has good prospect for high performance solar batteries and other application.
The electronic structure and electrical property of material can effectively be changed by element doping.Since Zn element has and alkaline earth gold
Belong to similar property, and the radius of Zn ion is less than Ca ionic radius, therefore when Zn element mixes Ca2After Si, Zn ion holds
Easily replace the position of Ca ion hence into lattice structure, as donor doping, provides conduction electrons as carrier.Except this
Except, the doping of Zn ion can make to form more vacancy inside semiconductor, to improve the conductivity and pyroelectricity of material
Energy.Currently, adulterating Ca about Zn2The still hardly seen report of Si thermoelectric material.
In addition, the size and thickness of the two-dimensional nano-film that stripping method is prepared not can be effectively controlled, and yield is lower.And
The two-dimensional nano-film crystallinity obtained using sputtering method is poor, crystallite dimension very little, and has been easy metal residual.Compared to it
Under, the two-dimensional nano-film size of chemical vapor deposition preparation is bigger, and crystallinity is higher, and it is thin to be able to achieve single layer, bilayer and few layer
The high-quality growth of membrane sample, therefore the present invention is prepared for two-dimentional Zn doping Ca using chemical vapour deposition technique2Si nano thin-film.
Summary of the invention
It is an object of the present invention to provide a kind of two dimension Zn to adulterate Ca2Si nano thin-film and its chemical vapor deposition method.This
The preparation method used of invention is the synthetic method using chemical vapor deposition, grows the two of high quality on the glass substrate
It ties up Zn and adulterates Ca2Si nano thin-film.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of two dimension Zn doping Ca2The chemical vapor deposition method of Si nano thin-film, the described method comprises the following steps:
(1) substrate of glass is pre-processed to remove the impurity of substrate surface；
(2) taking molar ratio is the Ca powder and Zn powder of 40:0.5 ~ 3, and the silica dish equipped with Ca powder is placed on three-temperature-zone height
Silica dish equipped with Zn powder is placed on the intermediate region of three-temperature-zone high temperature process furnances by the front end area of warm tube furnace, pre- to locate
Substrate of glass after reason is placed on the terminal region of three-temperature-zone high temperature process furnances；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, is led to the flow velocity of 40 ~ 60 sccm
Enter argon gas and drains furnace air；Repeating the above steps 2 ~ 4 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, and with the heating of 25 ~ 35 DEG C/min
The front end area of rate heating three-temperature-zone high temperature process furnances adds to 600 ~ 700 DEG C, while with the heating rate of 15 ~ 25 DEG C/min
Substrate of glass is heated to 400 ~ 500 DEG C, with the heating rate of 35 ~ 45 DEG C/min in the intermediate region of hot three-temperature-zone high temperature process furnances
The terminal region at place reacts 20 ~ 60 min to 500 ~ 600 DEG C, makes the atomic ratio 2:1 of Ca and Si, reaction product deposition
In substrate of glass；Reaction product is carried out to in-situ annealing processing in tube furnace and adulterates Ca to get to two dimension Zn2Si thin layer material
Material.
The method of step (1) the pretreated glass substrate are as follows: substrate of glass is sequentially placed into acetone, dehydrated alcohol, is gone
Each cleaning 15min of ultrasound in ionized water.
Step (2) the Ca powder purity is 99.9 %, and Zn powder purity is 99.9 %.
Step (4) the argon gas flow velocity being passed through is 40 ~ 60 sccm, SiH4Gas flow rate is 15 ~ 30 sccm.
Annealing temperature described in step (4) is 400 ~ 500 DEG C, and annealing time is 0.5 ~ 5 h.
The beneficial effects of the present invention are: Ca is adulterated with two-dimentional Zn prepared by chemical vapour deposition technique2Si nano thin-film, phase
Be compared to other preparation methods, preparation process is simple, can be made large area and purity is high nano thin-film, product purity compared with
Height is expected to can be realized extensive, high quality two-dimentional Zn doping Ca2The production of Si nano thin-film has good industrialization
Prospect.
Detailed description of the invention
Fig. 1 is that chemical vapour deposition technique prepares two dimension Zn doping Ca2The flow diagram of Si nano thin-film；
Fig. 2 is that 2 gained two dimension Zn of embodiment adulterates Ca2The XRD diagram of Si nano thin-film；
Fig. 3 is that 2 gained two dimension Zn of embodiment adulterates Ca2The scanning electron microscope (SEM) photograph of Si nano thin-film.
Specific embodiment
It is exemplified below specific embodiment the present invention is explained further, but the present invention is not limited solely to these implementations
Example.
Embodiment 1
A kind of chemical vapor deposition preparation two dimension Zn doping Ca2The method of Si nano thin-film, the specific steps are as follows:
(1) by substrate of glass be sequentially placed into acetone, dehydrated alcohol, in deionized water 15 min of each cleaning of ultrasound to remove substrate table
The impurity in face；
(2) taking molar ratio is the Ca powder and Zn powder of 40:0.5, by the quartz equipped with the Ca powder that 3.5 grams of purity are 99.9 %
Ware is placed on the front end area of three-temperature-zone high temperature process furnances, and the silica dish equipped with the Zn powder that 0.1 gram of purity is 99.9 % is put
It sets in the intermediate region of three-temperature-zone high temperature process furnances, pretreated substrate of glass is placed on the end of three-temperature-zone high temperature process furnances
Region；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, argon is passed through with the flow velocity of 40 sccm
Gas drains furnace air；Repeating the above steps 3 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, the argon gas flow velocity being passed through be 40
Sccm, SiH4Gas flow rate is 15 sccm；And with the front end of the heating rate of 25 DEG C/min heating three-temperature-zone high temperature process furnances
Region to 600 DEG C, while with the heating rate of 15 DEG C/min heating three-temperature-zone high temperature process furnances intermediate region to 400 DEG C,
With the terminal region where the heating rate heating substrate of glass of 35 DEG C/min to 500 DEG C, 60 min are reacted, make Ca's and Si
Atomic ratio is 2:1, and reaction product is deposited on substrate of glass；By reaction product with 400 DEG C of annealing temperature in tube furnace
It carries out in-situ annealing and handles 5 h to get Ca is arrived2Si layer material.
Embodiment 2
A kind of chemical vapor deposition preparation two dimension Zn doping Ca2The method of Si nano thin-film, the specific steps are as follows:
(1) by substrate of glass be sequentially placed into acetone, dehydrated alcohol, in deionized water 15 min of each cleaning of ultrasound to remove substrate table
The impurity in face；
(2) taking molar ratio is the Ca powder and Zn powder of 40:3, by the silica dish equipped with the Ca powder that 3.5 grams of purity are 99.9 %
It is placed on the front end area of three-temperature-zone high temperature process furnances, the silica dish equipped with the Zn powder that 0.5 gram of purity is 99.9 % is placed
The intermediate region of high temperature process furnances in three-temperature-zone, pretreated substrate of glass are placed on the end region of three-temperature-zone high temperature process furnances
Domain；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, argon is passed through with the flow velocity of 40 sccm
Gas drains furnace air；Repeating the above steps 3 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, the argon gas flow velocity being passed through be 40
Sccm, SiH4Gas flow rate is 30 sccm；And with the front end of the heating rate of 30 DEG C/min heating three-temperature-zone high temperature process furnances
Region to 660 DEG C, while with the heating rate of 25 DEG C/min heating three-temperature-zone high temperature process furnances intermediate region to 500 DEG C,
With the terminal region where the heating rate heating substrate of glass of 40 DEG C/min to 560 DEG C, 30 min are reacted, make Ca's and Si
Atomic ratio is 2:1, and reaction product is deposited on substrate of glass；By reaction product with 500 DEG C of annealing temperature in tube furnace
It carries out in-situ annealing and handles 0.5 h to get Ca is arrived2Si layer material.
Embodiment 3
A kind of chemical vapor deposition preparation two dimension Zn doping Ca2The method of Si nano thin-film, the specific steps are as follows:
(1) by substrate of glass be sequentially placed into acetone, dehydrated alcohol, in deionized water 15 min of each cleaning of ultrasound to remove substrate table
The impurity in face；
(2) taking molar ratio is the Ca powder and Zn powder of 40:2.5, and the silica dish for the Ca powder that 2.3 grams of purity are 99.9 % is put
The front end area in three-temperature-zone high temperature process furnances is set, the silica dish equipped with the Zn powder that 0.3 gram of purity is 99.9 % is placed on
The intermediate region of three-temperature-zone high temperature process furnances, pretreated substrate of glass are placed on the end region of three-temperature-zone high temperature process furnances
Domain；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, argon is passed through with the flow velocity of 60 sccm
Gas drains furnace air；Repeating the above steps 3 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, the argon gas flow velocity being passed through be 60
Sccm, SiH4Gas flow rate is 15 sccm；And with the front end of the heating rate of 35 DEG C/min heating three-temperature-zone high temperature process furnances
Region to 700 DEG C, while with the heating rate of 25 DEG C/min heating three-temperature-zone high temperature process furnances intermediate region to 450 DEG C,
With the terminal region where the heating rate heating substrate of glass of 45 DEG C/min to 600 DEG C, 40 min are reacted, make Ca's and Si
Atomic ratio is 2:1, and reaction product is deposited on substrate of glass；By reaction product with 400 DEG C of annealing temperature in tube furnace
It carries out in-situ annealing and handles 5 h to get Ca is arrived2Si layer material.
Embodiment 4
A kind of chemical vapor deposition preparation two dimension Zn doping Ca2The method of Si nano thin-film, the specific steps are as follows:
(1) by substrate of glass be sequentially placed into acetone, dehydrated alcohol, in deionized water 15 min of each cleaning of ultrasound to remove substrate table
The impurity in face；
(2) taking molar ratio is the Ca powder and Zn powder of 40:1.5, and the silica dish for the Ca powder that 4.5 grams of purity are 99.9 % is put
The front end area in three-temperature-zone high temperature process furnances is set, the silica dish equipped with the Zn powder that 0.3 gram of purity is 99.9 % is placed on
The intermediate region of three-temperature-zone high temperature process furnances, pretreated substrate of glass are placed on the end region of three-temperature-zone high temperature process furnances
Domain；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, argon is passed through with the flow velocity of 60 sccm
Gas drains furnace air；Repeating the above steps 3 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, the argon gas flow velocity being passed through be 60
Sccm, SiH4Gas flow rate is 30 sccm；And with the front end of the heating rate of 35 DEG C/min heating three-temperature-zone high temperature process furnances
Region to 700 DEG C, while with the heating rate of 25 DEG C/min heating three-temperature-zone high temperature process furnances intermediate region to 500 DEG C,
With the terminal region where the heating rate heating substrate of glass of 45 DEG C/min to 600 DEG C, 40 min are reacted, make Ca's and Si
Atomic ratio is 2:1, and reaction product is deposited on substrate of glass；By reaction product with 500 DEG C of annealing temperature in tube furnace
It carries out in-situ annealing and handles 1 h to get Ca is arrived2Si layer material.
Table 1 is that the calculated two dimension Zn of embodiment 1 ~ 4 adulterates Ca2Atomic ratio, carrier concentration and the load of Si nano thin-film
Flow the properties such as transport factor.
1 two dimension Zn of table adulterates Ca2Atomic ratio, carrier concentration and the carrier mobility of Si nano thin-film
As can be seen from Table 1, compared to undoped Ca2Si nano thin-film, after being adulterated by Zn, Ca2The load of Si nano thin-film
It flows sub- concentration and improves the 1-2 order of magnitude, while carrier mobility reaches as high as 9879.56 cm2·V-1 ·s-1, this height
Carrier concentration and high carrier mobility show two-dimentional Zn doping Ca2Si nano thin-film for high performance solar batteries and
The application of nano electron device has good prospect.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, all should belong to covering scope of the invention.
Claims (6)
1. a kind of two dimension Zn adulterates Ca2The chemical vapor deposition method of Si nano thin-film, it is characterised in that:
It the described method comprises the following steps:
(1) substrate of glass is pre-processed to remove the impurity of substrate surface；
(2) taking molar ratio is the Ca powder and Zn powder of 40:0.5 ~ 3, and the silica dish equipped with Ca powder is placed on three-temperature-zone height
Silica dish equipped with Zn powder is placed on the intermediate region of three-temperature-zone high temperature process furnances by the front end area of warm tube furnace, pre- to locate
Substrate of glass after reason is placed on the terminal region of three-temperature-zone high temperature process furnances；
(3) vacuum degree of high temperature process furnances is evacuated to 10 Pa hereinafter, being then shut off vacuum valve, is led to the flow velocity of 40 ~ 60 sccm
Enter argon gas and drains furnace air；Repeating the above steps 2 ~ 4 times replaces furnace air by argon gas completely；
(4) argon gas and SiH are passed through into tube furnace with certain rate4Mixed gas, and with the heating of 25 ~ 35 DEG C/min speed
Rate heats the front end area of three-temperature-zone high temperature process furnances to 600 ~ 700 DEG C, while with the heating of the heating rate of 15 ~ 25 DEG C/min
Substrate of glass institute is heated to 400 ~ 500 DEG C, with the heating rate of 35 ~ 45 DEG C/min in the intermediate region of three-temperature-zone high temperature process furnances
Terminal region to 500 ~ 600 DEG C, react 20 ~ 60 min, make the atomic ratio 2:1 of Ca and Si, reaction product is deposited on
Substrate of glass；Reaction product is carried out to in-situ annealing processing in tube furnace and adulterates Ca to get to two dimension Zn2Si thin layer material
Material.
2. two dimension Zn according to claim 1 adulterates Ca2The chemical vapor deposition method of Si nano thin-film, which is characterized in that
The method of step (1) the pretreated glass substrate are as follows: substrate of glass is sequentially placed into acetone, dehydrated alcohol, in deionized water
Ultrasonic each cleaning 15min.
3. two dimension Zn according to claim 1 adulterates Ca2The chemical vapor deposition method of Si nano thin-film, which is characterized in that
Step (2) the Ca powder purity is 99.9 %, and Zn powder purity is 99.9 %.
4. two dimension Zn according to claim 1 adulterates Ca2The chemical vapor deposition method of Si nano thin-film, which is characterized in that
Step (4) the argon gas flow velocity being passed through is 40 ~ 60 sccm, SiH4Gas flow rate is 15 ~ 30 sccm.
5. two dimension Zn according to claim 1 adulterates Ca2The chemical vapor deposition method of Si nano thin-film, which is characterized in that
Annealing temperature described in step (4) is 400 ~ 500 DEG C, and annealing time is 0.5 ~ 5 h.
6. a kind of two-dimentional Zn such as the method preparation of any one of claim 1 ~ 5 adulterates Ca2Si nano thin-film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112875659A (en) * | 2021-03-11 | 2021-06-01 | 北京大学 | Method for realizing uniform fluorine doping of hexagonal boron nitride in situ |
| CN112981368A (en) * | 2021-02-03 | 2021-06-18 | 北航（四川）西部国际创新港科技有限公司 | Improved CVD equipment and preparation method for realizing co-infiltration deposition of aluminum-silicon coating by using improved CVD equipment |
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| EP0178200A1 (en) * | 1984-09-10 | 1986-04-16 | FAIRCHILD CAMERA & INSTRUMENT CORPORATION | Method of control for chemical vapor deposition |
| CN103194729A (en) * | 2013-03-27 | 2013-07-10 | 中国科学院物理研究所 | Method for preparing metal chalcogenide film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112981368A (en) * | 2021-02-03 | 2021-06-18 | 北航（四川）西部国际创新港科技有限公司 | Improved CVD equipment and preparation method for realizing co-infiltration deposition of aluminum-silicon coating by using improved CVD equipment |
| CN112981368B (en) * | 2021-02-03 | 2022-06-07 | 北航（四川）西部国际创新港科技有限公司 | Improved CVD equipment and preparation method for realizing co-infiltration deposition of aluminum-silicon coating by using improved CVD equipment |
| CN112875659A (en) * | 2021-03-11 | 2021-06-01 | 北京大学 | Method for realizing uniform fluorine doping of hexagonal boron nitride in situ |
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