CN108315814A - A kind of preparation method of gallium alkene - Google Patents
A kind of preparation method of gallium alkene Download PDFInfo
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- CN108315814A CN108315814A CN201810368966.9A CN201810368966A CN108315814A CN 108315814 A CN108315814 A CN 108315814A CN 201810368966 A CN201810368966 A CN 201810368966A CN 108315814 A CN108315814 A CN 108315814A
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- C—CHEMISTRY; METALLURGY
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- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract
The invention discloses a kind of preparation methods of gallium alkene comprising following steps:1) Si substrates are cleaned successively, degasification and annealing, obtains (111) 7 × 7 surfaces Si;2) heating gallium source makes gallium atom grow into (111) 7 × 7 surfaces Si in the form of thermal evaporation, then carries out in-situ annealing processing, is reconstructed on (111) 7 × 7 surfaces Si and forms 3 surfaces Ga 3 × √ of √;3) it is 30~60 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom grow into 3 surfaces Ga 3 × √ of √ in the form of thermal evaporation, generates transition zone;4) it is room temperature to adjust substrate temperature, and heating gallium source is made gallium atom be grown into transition layer surface in the form of thermal evaporation, forms the gallium alkene of the monoatomic layer in hexagon cellular structure.It prepares the gallium alkene of monoatomic layer using molecular beam epitaxy technique under ultra-high vacuum environment, is conducive to gallium alkene microstructure and property Quality Research.
Description
Technical field
The present invention relates to two-dimensional material technologies of preparing, and in particular to a kind of preparation method of gallium alkene.
Background technology
" gallium alkene " refers to the type graphene two dimensional crystal material being combined by gallium atom.This two-dimensional material has
Very excellent characteristic, such as high surface area ratio, high Young's modulus of elasticity, excellent thermal conductivity, in absorption, catalysis, light
Electricity etc. shows huge applications potential, and the electronic device to construct novel provides new opportunities.
Currently, the single-element class graphene two dimensional crystal material successfully prepared mainly have silene, germanium alkene, tin alkene, boron alkene,
Phosphorus alkene and gallium alkene.Wherein first five kind alkene material has all been successfully prepared using growth technology, and gallium alkene only has U.S. Hughes
The researcher of Rice University is obtained using solid-liquid stripping method.However, solid-liquid stripping method is the preparation side of a kind of " from top to bottom "
Method is unfavorable for gallium alkene microstructure and property Quality Research, is also unable to get the gallium alkene of monoatomic layer.Therefore, it is necessary to develop one
The gallium alkene preparation method of kind " from bottom to top ".
Invention content
The object of the present invention is to provide a kind of preparation methods of gallium alkene, molecular beam epitaxy technique are utilized, in ultrahigh vacuum
Under environment, the gallium alkene of monoatomic layer is prepared, is conducive to gallium alkene microstructure and property Quality Research.
The preparation method of gallium alkene of the present invention comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is cleaned, is removed successively to Si substrates
Gas and annealing obtain (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, then carries out in-situ annealing processing, in Si
It reconstructs and is formed on (111) -7 × 7 surfacesR30 ° of surface;Part gallium atom is had during in-situ annealing to serve as a contrast from Si
Bottom surface is desorbed, and remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiR30 ° of surface;
3) growth of transition zone:It is 30~60 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom with the shape of thermal evaporation
Formula is grown intoR30 ° of surface generatesThe transition zone of structure, the transition zone are monatomic film;
4) growth of gallium alkene:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be grown in the form of thermal evaporation
To transition layer surface, the gallium alkene of the monoatomic layer in hexagon cellular structure is formed.
Further, the specific method of cleaning is in the step 1):Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then
It puts and is cleaned by ultrasonic in acetone again.
Further, the specific method of degasification is in the step 1):Si substrates after cleaning are placed on ultrahigh vacuum intracavitary,
6~12h of degasification under conditions of temperature is 450~650 DEG C, then cools to room temperature.
Further, the specific method of annealing is in the step 1):By the Si substrates after degasification from room temperature in 5~20s
1000~1300 DEG C are risen to, is annealed 3~10 times, each annealing time is 5~20s.
Further, the temperature of the in-situ annealing processing in the step 2) is 500~600 DEG C, and the time is 5~50min.
Further, the step 2), 3) and 4) in the heating temperature in gallium source be 600~900 DEG C.
The present invention utilizes molecular beam epitaxy technique, and under ultra-high vacuum environment, " from bottom to top " makes gallium atomic epitaxy grow
Gallium alkene is formed, gallium alkene obtained is monoatomic layer, is in hexagon cellular structure, relative to using gallium alkene made from " from top to bottom ",
It is more conducive to its microstructure and property Quality Research, more orderly gallium alkene can also be obtained.
Description of the drawings
Fig. 1 is the structural schematic diagram for the device for being used to prepare gallium alkene;
Fig. 2 is of the inventionThe STM on surface schemes;
Fig. 3 is the STM figures of the transition zone of the present invention;
Fig. 4 is the STM figures of the gallium alkene layer of the present invention.
In figure, 1-vacuum chamber, 2-specimen holders, 3-sample transmission rods, 4-magnetic force handles, 5-DC power supplies, 6-crucibles,
7-heating furnaces, 8-substrates.
Specific implementation mode
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Referring to Fig. 1, shown in a kind of device being used to prepare gallium alkene, including vacuum chamber 1, specimen holder 2, sample transmission rod 3, magnetic force
4 heating furnace 7 of handle and crucible 6;The magnetic force handle 4 is set to outside vacuum chamber 1, is connect with one end of sample transmission rod 3, the sample transmission rod
3 other end is connect with specimen holder 2, and the specimen holder 2 is controlled by sample transmission rod 3 for fixing sample and enters or exit vacuum
Chamber;The heating furnace 7 is set to 1 bottom of vacuum chamber;The crucible 6 is set in heating furnace 7, for placing gallium source;Using direct current
Sample and gallium source are heated in source 5.When specific works, the Si substrates after cleaning are fixed on specimen holder 2, magnetic force handle 4 is utilized
Drive sample transmission rod 3 that Si substrates are sent into vacuum chamber 1, Si substrates are located at the surface of heating furnace, and gallium source is placed in crucible 6,
Crucible 6 is placed in heating furnace 7 again, Si substrates and gallium source are heated using DC power supply 5 respectively.
Embodiment one, a kind of preparation method of gallium alkene comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is first carried out at cleaning successively to Si substrates
Reason, Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again;Then degassing processing is carried out, it will
Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, and degasification 8h under conditions of temperature is 500 DEG C is then cooled to room temperature;Again
It is made annealing treatment, the Si substrates after degasification is risen to 1200 DEG C from room temperature in 15s, are annealed 7 times, each annealing time is
15s obtains clean (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, and the heating temperature in gallium source is 750 DEG C, gallium atom
Coverage 1/2ML, wherein 1ML refers to the Si atomic densities in Si (111) face, 7.84*10 every square centimeter14A atom, then into
The processing of row in-situ annealing, annealing temperature are 550 DEG C, annealing time 30min, have during in-situ annealing part gallium atom from
Si substrate surfaces are desorbed, and remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiR30 ° of surface;It is surplus
Under the coverage of gallium atom be about 1/3ML, if the amount of remaining gallium atom is very little, Si substrates can be made locally to be still Si
(111) -7 × 7, it cannot be formedIt is too many then to make Si substrate out-of-flatnesses, it is formedIsland,
The coverage of remaining gallium atom is controlled by controlling in-situ annealing technological parameter;
3) growth of transition zone:It is 50 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toThe heating temperature on R30 ° of surface, gallium source is 750 DEG C, and gallium atom flies out and is adsorbed inSurface
Realize epitaxial growth, when the coverage of gallium atom reaches 1.4ML, transition zone growth is completed, and transition zone is monoatomic gallium film,
It is formedStructure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
Transition layer surface is grown to, the heating temperature in gallium source is 750 DEG C, and gallium atom flies out and is adsorbed in transition layer surface, when gallium atom
When coverage reaches 2ML, the gallium alkene growth of monoatomic layer is completed.
Using scanning tunneling microscope in situ detection Si (111)The surface shape of layer, transition zone and gallium alkene layer
Looks.Referring to Fig. 2, shown in Si (111)Layer surface pattern, a are a wide range of, i.e. 500 × 500nm, b are small model
It encloses, i.e. 15nm × 15nm, observation is it is found that in the formation of Si substrate surfaces after in-situ annealing is handledSurface is flat
It is whole uniform, and complete gallium atom and completely cover Si substrate surfaces, it provides the foundation for the preparation of transition zone.Referring to Fig. 3, institute
The transition zone surface topography shown, c are a wide range of, i.e. 500 × 500nm, d are small range, i.e. 70nm × 70nm, and observation is it is found that system
The transition zone obtained is monoatomic film, and surfacing provides the foundation for the preparation of gallium alkene layer.Referring to Fig. 4, the gallium alkene
Layer surface pattern, c are a wide range of, i.e. 80 × 80nm, d are small range, i.e. 4nm × 4nm, and observation is it is found that gallium alkene obtained is single
Atomic layer shows hexagon cellular structure.
Embodiment two, a kind of preparation method of gallium alkene comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is first carried out at cleaning successively to Si substrates
Reason, Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again;Then degassing processing is carried out, it will
Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, and degasification 12h under conditions of temperature is 450 DEG C is then cooled to room temperature;Again
It being made annealing treatment, the Si substrates after degasification is risen to 1000 DEG C from room temperature in 5s, are annealed 3 times, each annealing time is 5s,
Obtain clean (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, and the heating temperature in gallium source is 600 DEG C, gallium atom
Coverage 1/2ML, then carry out in-situ annealing processing, annealing temperature is 500 DEG C, annealing time 50min, in-situ annealing process
In have part gallium atom and be desorbed from Si substrate surfaces, remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiThe coverage on R30 ° of surface, remaining gallium atom is about 1/3ML;
3) growth of transition zone:It is 30 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toThe heating temperature on R30 ° of surface, gallium source is 600 DEG C, and gallium atom flies out and is adsorbed inSurface
Realize epitaxial growth, when the coverage of gallium atom reaches 1.4ML, transition zone growth is completed, and transition zone is monoatomic gallium film,
It is formedStructure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
Transition layer surface is grown to, the heating temperature in gallium source is 600 DEG C, and gallium atom flies out and is adsorbed in transition layer surface, when gallium atom
When coverage reaches 2ML, the gallium alkene growth of monoatomic layer is completed.
Embodiment three, a kind of preparation method of gallium alkene comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is first carried out at cleaning successively to Si substrates
Reason, Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again;Then degassing processing is carried out, it will
Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, and degasification 6h under conditions of temperature is 650 DEG C is then cooled to room temperature;Again
It is made annealing treatment, the Si substrates after degasification is risen to 1300 DEG C from room temperature in 20s, are annealed 10 times, each annealing time is
20s obtains clean (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, and the heating temperature in gallium source is 900 DEG C, gallium atom
Coverage 1/2ML, then carry out in-situ annealing processing, annealing temperature is 600 DEG C, annealing time 5min, in-situ annealing process
In have part gallium atom and be desorbed from Si substrate surfaces, remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiThe coverage on R30 ° of surface, remaining gallium atom is about 1/3ML;
3) growth of transition zone:It is 60 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toThe heating temperature on R30 ° of surface, gallium source is 900 DEG C, and gallium atom flies out and is adsorbed inSurface
Realize epitaxial growth, when the coverage of gallium atom reaches 1.4ML, transition zone growth is completed, and transition zone is monoatomic gallium film,
It is formedStructure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
Transition layer surface is grown to, the heating temperature in gallium source is 900 DEG C, and gallium atom flies out and is adsorbed in transition layer surface, when gallium atom
When coverage reaches 2ML, the gallium alkene growth of monoatomic layer is completed.
Example IV, a kind of preparation method of gallium alkene comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is first carried out at cleaning successively to Si substrates
Reason, Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again;Then degassing processing is carried out, it will
Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, and degasification 10h under conditions of temperature is 480 DEG C is then cooled to room temperature;Again
It is made annealing treatment, the Si substrates after degasification is risen to 1100 DEG C from room temperature in 10s, are annealed 5 times, each annealing time is
10s obtains clean (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, and the heating temperature in gallium source is 800 DEG C, gallium atom
Coverage 1/2ML, then carry out in-situ annealing processing, annealing temperature is 520 DEG C, annealing time 35min, in-situ annealing process
In have part gallium atom and be desorbed from Si substrate surfaces, remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiThe coverage on R30 ° of surface, remaining gallium atom is about 1/3ML;
3) growth of transition zone:It is 40 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toThe heating temperature on R30 ° of surface, gallium source is 800 DEG C, and gallium atom flies out and is adsorbed inSurface
Realize epitaxial growth, when the coverage of gallium atom reaches 1.4ML, transition zone growth is completed, and transition zone is monoatomic gallium film,
It is formedStructure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
Transition layer surface is grown to, the heating temperature in gallium source is 800 DEG C, and gallium atom flies out and is adsorbed in transition layer surface, when gallium atom
When coverage reaches 2ML, the gallium alkene growth of monoatomic layer is completed.
Embodiment five, a kind of preparation method of gallium alkene comprising following steps:
1) Si substrates are used, it is crystal orientation to select (111) crystal face of Si substrates, is first carried out at cleaning successively to Si substrates
Reason, Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again;Then degassing processing is carried out, it will
Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, and degasification 8h under conditions of temperature is 485 DEG C is then cooled to room temperature;Again
It is made annealing treatment, the Si substrates after degasification is risen to 1150 DEG C from room temperature in 14s, are annealed 4 times, each annealing time is
6s obtains clean (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, heating
Gallium source makes gallium atom grow into (111) -7 × 7 surfaces Si in the form of thermal evaporation, and the heating temperature in gallium source is 600 DEG C, gallium atom
Coverage 1/2ML, then carry out in-situ annealing processing, annealing temperature is 570 DEG C, annealing time 20min, in-situ annealing process
In have part gallium atom and be desorbed from Si substrate surfaces, remaining gallium atom reconstructs formation on (111) -7 × 7 surfaces SiThe coverage on R30 ° of surface, remaining gallium atom is about 1/3ML;
3) growth of transition zone:It is 60 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toThe heating temperature on R30 ° of surface, gallium source is 600 DEG C, and gallium atom flies out and is adsorbed inSurface
Realize epitaxial growth, when the coverage of gallium atom reaches 1.4ML, transition zone growth is completed, and transition zone is monoatomic gallium film,
It is formedStructure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
Transition layer surface is grown to, the heating temperature in gallium source is 600 DEG C, and gallium atom flies out and is adsorbed in transition layer surface, when gallium atom
When coverage reaches 2ML, the gallium alkene growth of monoatomic layer is completed.
Claims (6)
1. a kind of preparation method of gallium alkene, it is characterised in that include the following steps:
1) use Si substrates, it is crystal orientation to select (111) crystal face of Si substrates, Si substrates are cleaned successively, degasification and
Annealing, obtains (111) -7 × 7 surfaces Si;
2)Si(111)The growth of substrate:It is higher than 3.0 × 10 in vacuum degree-10Under conditions of mbar, gallium source is heated
So that gallium atom is grown into (111) -7 × 7 surfaces Si in the form of thermal evaporation, then carry out in-situ annealing processing, Si (111) -7 ×
It reconstructs and is formed on 7 surfacesSurface;
3) growth of transition zone:It is 30~60 DEG C to adjust substrate temperature, and heating gallium source makes gallium atom be given birth in the form of thermal evaporation
It grows toSurface generatesThe transition zone of structure;
4) growth of gallium alkene layer:Adjusting substrate temperature is room temperature, and heating gallium source makes gallium atom be grown into the form of thermal evaporation
Transition layer surface forms the gallium alkene of the monoatomic layer in hexagon cellular structure.
2. the preparation method of gallium alkene according to claim 1, it is characterised in that:The specific method cleaned in the step 1)
It is:Si substrates are firstly placed in alcohol and are cleaned by ultrasonic, then puts and is cleaned by ultrasonic in acetone again.
3. the preparation method of gallium alkene according to claim 1, it is characterised in that:The specific method of degasification in the step 1)
It is:Si substrates after cleaning are placed on ultrahigh vacuum intracavitary, 6~12h of degasification under conditions of temperature is 450~650 DEG C, then
It is cooled to room temperature.
4. the preparation method of gallium alkene according to claim 1, it is characterised in that:The specific method annealed in the step 1)
It is:Si substrates after degasification are risen to 1000~1300 DEG C from room temperature in 5~20s, are annealed 3~10 times, each annealing time
For 5~20s.
5. the preparation method of gallium alkene according to claim 1, it is characterised in that:In-situ annealing processing in the step 2)
Temperature be 500~600 DEG C, the time be 5~50min.
6. the preparation method of gallium alkene according to claim 1, it is characterised in that:The step 2), 3) and 4) in gallium source
Heating temperature is 600~900 DEG C.
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Citations (3)
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CN1481578A (en) * | 2000-12-18 | 2004-03-10 | Ħ��������˾ | Semiconductor structure including monocrystalline film |
US20050023552A1 (en) * | 2003-07-28 | 2005-02-03 | National Chiao-Tung University | Growth of GaAs epitaixial layers on Si substrate by using a novel GeSi buffer layer |
CN104465725A (en) * | 2014-11-24 | 2015-03-25 | 华南理工大学 | In0.3Ga0.7As thin film growing on Si substrate and preparing method |
-
2018
- 2018-04-23 CN CN201810368966.9A patent/CN108315814A/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1481578A (en) * | 2000-12-18 | 2004-03-10 | Ħ��������˾ | Semiconductor structure including monocrystalline film |
US20050023552A1 (en) * | 2003-07-28 | 2005-02-03 | National Chiao-Tung University | Growth of GaAs epitaixial layers on Si substrate by using a novel GeSi buffer layer |
CN104465725A (en) * | 2014-11-24 | 2015-03-25 | 华南理工大学 | In0.3Ga0.7As thin film growing on Si substrate and preparing method |
Non-Patent Citations (1)
Title |
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陶敏龙: "有机/无机二维材料的制备及量子效应", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20180724 |