CN107815664A - Chemical vapor depsotition equipment, method and purposes - Google Patents
Chemical vapor depsotition equipment, method and purposes Download PDFInfo
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- CN107815664A CN107815664A CN201711005202.5A CN201711005202A CN107815664A CN 107815664 A CN107815664 A CN 107815664A CN 201711005202 A CN201711005202 A CN 201711005202A CN 107815664 A CN107815664 A CN 107815664A
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- reaction cavity
- chemical vapor
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/342—Boron nitride
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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
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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
-
- 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
- C23C16/4411—Cooling of the reaction chamber walls
Abstract
The present invention provides a kind of chemical vapor depsotition equipment, and the chemical vapor depsotition equipment includes：Reaction cavity；Vacuum provides device, and the vacuum provides the vacuum in the device offer reaction cavity；Reacting gas is supplied in the reaction cavity by source feedway, the source feedway；Tubular heater, the tubular heater are in the reaction cavity, have open both ends and the tube chamber for accommodating growth substrate；Catalyst conveyer, the catalyst conveyer are in the reaction cavity, for catalyst transmission to be passed through into tube chamber.The present invention also provides the purposes that the equipment is used to prepare two-dimentional hexagonal boron nitride two-dimensional graphene laminated construction.The present invention also provides a kind of chemical gaseous phase depositing process.
Description
Technical field
The present invention relates to chemical vapour deposition technique field, more particularly to a kind of chemical vapor depsotition equipment, method and use
On the way.
Background technology
CVD technology is chemical vapor deposition Chemical Vapor Deposition abbreviation.Chemical vapor deposition is logical
The mode of chemical reaction is crossed, using various energy such as heating, plasma excitation or light radiation, gaseous state or steam are made in reactor
The chemical substance of state forms the technology of solid deposited thing in gas phase or gas-solid interface through chemical reaction.
Graphene and hexagonal boron nitride are current popular two-dimensional materials.All can not be most but any of which is individually a kind of
Bigization realizes their value.Stone can be opened by all pointing out the laminated construction of hexagonal boron nitride and graphene in theory and experimentally
The energy band band gap of black alkene, and can largely improve the electron mobility of graphene.
At present, for the growth of two-dimensional material, the CVD equipment overwhelming majority of use is all hot-wall tube furnace.Hot-wall tube
Stove can prepare the film not high to growth vacuum level requirements, but the repeatability tested is poor.Moreover, preparing two dimension six
Found in the practice of square boron nitride-two-dimensional graphene laminated construction, in low vacuum equipment, grown first layer hexagonal boron nitride
Afterwards, boron nitride can be oxidized.In addition, for this growth course for being strongly depend on catalyst, can't based on current source
Grown in the case where departing from catalyst.However, although the MOCVD device for being directed to preparation iii-v hetero-junctions meets
It is required that but cost is again too expensive.
The content of the invention
In view of this, the invention provides a kind of chemical vapor depsotition equipment and method and purposes.
In one aspect, the invention provides a kind of chemical vapor depsotition equipment, the chemical vapor depsotition equipment to include：
Reaction cavity；
Vacuum provides device, and the vacuum provides the vacuum in the device offer reaction cavity；
Reacting gas is supplied in the reaction cavity by source feedway, the source feedway；
Tubular heater, the tubular heater are in the reaction cavity, have open both ends and for accommodating
The tube chamber of growth substrate；
Catalyst conveyer, the catalyst conveyer is in the reaction cavity, for catalyst to be transmitted
By tube chamber.
Preferably, the cross section of the tubular heater is rectangle.
Preferably, the tubular heater horizontal setting.
Preferably, the chemical vapor depsotition equipment also includes growth substrate apparatus for adjusting position.
Preferably, the growth substrate apparatus for adjusting position is heater height adjusting means.
Preferably, the reaction cavity is cold wall reaction cavity.
Preferably, the reaction cavity has double-deck double wall water cooled housing.
Preferably, the source feedway includes reaction source memory.
Preferably, the source of the source feedway is liquid source and/or gaseous source.
Preferably, the source feedway includes for the reaction source memory of liquid source and by reacting source memory
Carrier gas bubbler.
Preferably, the reaction source memory includes cooler.
Preferably, the cooler is semiconductor cold-trap.
Preferably, reacting gas is introduced directly into tube chamber by the source feedway.
Preferably, the catalyst conveyer is volume to volume conveyer belt, for making catalyst be heated via the tubulose
One end of device enters the tube chamber, and leaves the tube chamber via the other end of the tubular heater.
Preferably, the cross section of the tubular heater is rectangle, and bottom surface is used to place growth substrate,
The chemical vapor depsotition equipment also includes growth substrate apparatus for adjusting position, the growth substrate position adjustments dress
It is heater height adjusting means to put,
The reaction cavity has double-deck double wall water cooled housing,
The source of the source feedway is liquid source and gaseous source,
The source feedway includes the reaction source memory for liquid source and the load by the reaction source memory
Enraged bubbler, the reaction source memory include semiconductor cold-trap,
The catalyst conveyer is volume to volume conveyer belt, for making the one end of catalyst via the tubular heater
The tube chamber is left into the tube chamber, and via the other end of the tubular heater.
In one aspect, the present invention provides above-mentioned chemical vapor deposition unit and is used to prepare two-dimentional hexagonal boron nitride-two
Tie up the purposes of graphene laminated construction.
In one aspect, the present invention provides a kind of chemical gaseous phase depositing process, the described method comprises the following steps：
A) vacuum in reaction cavity is provided, wherein tubular heater is provided with the reaction cavity, the tubulose
Heater has open both ends and the tube chamber for accommodating growth substrate, wherein the growth substrate has been placed in tube chamber；
B) reacting gas is passed through into reaction cavity；
C) tube chamber is passed through into catalyst transmission；And
D) tube chamber is heated with the tubular heater；
So that the reacting gas reacts in the presence of the catalyst and deposited in the growth substrate.
Preferably, methods described is used to prepare two-dimentional hexagonal boron nitride-two-dimensional graphene lamination, including：
Step a), b) and d) is carried out, wherein growth substrate be copper, and reacting gas is nitrogen carrying borazine,
With inert gas purge reaction cavity, and
Step a), b), c) and d) is carried out, wherein catalyst is copper, and reacting gas is methane.
The apparatus and method of the present invention can provide the growing environment of high vacuum, and can be that growth hetero-junctions constantly carries
For new catalyst.
Brief description of the drawings
Fig. 1 is the schematic diagram of an embodiment of the equipment of the present invention.
Fig. 2 is the schematic diagram of an embodiment of fluid supply bubbling mode in the feedway of source.
Fig. 3 is the schematic diagram of an embodiment of tubular heater and catalyst conveyer.
Fig. 4 is the configuration diagram of embodiment preparation process.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
Fig. 1 is the schematic diagram of an embodiment of the chemical vapor depsotition equipment of the present invention.The chemical gaseous phase of the present invention
Depositing device includes：Reaction cavity 1；Vacuum provides device 2, and it provides the vacuum in the reaction cavity 1；Source feedway 3,
Reacting gas is supplied in the reaction cavity 1 by it；Tubular heater 4, it is in the reaction cavity 1, is had and is opened
Both ends and tube chamber 6 for accommodating growth substrate；Catalyst conveyer 7, it is in the reaction cavity 1, for inciting somebody to action
Tube chamber 6 is passed through in the transmission of catalyst 8.
The equipment of the present invention is particularly suitable for preparing multilayer two-dimension material hetero-junctions.
The reaction cavity 1 of the present invention is non-hot wall reaction cavity, and it provides the environment of high vacuum, but itself does not play and add
The effect of heat.Because reaction cavity using all-metal sealing and is equipped with the valve of high vacuum, so with being used in existing CVD
Hot-wall tube furnace compare, much higher vacuum can be reached in reaction cavity, so as to be advantageous to have high request to vacuum
Chemical vapor deposition processes progress.More preferably it is to use cold wall reaction cavity, i.e., cavity wall is cooled by cooling device,
Dust pollution in very big reduction system.As example, it uses cylinder type chamber, and cavity uses double-deck double wall water-cooling structure.It is double
Layer double wall water-cooling structure includes inwall, outer wall and the water cooling labyrinth being clipped between inside and outside wall.It is all steel material, inside and outside throwing
Light, it is desirable to which outer leak rate is less than 10-12mbar·l·s-1, interior leak rate ＜ 10-11mbar·l·s-1.Interface is sealed using copper band, with
This ensures the vacuum of cavity.
Vacuum provides device 2 and is connected with reaction cavity 1, and high vacuum is provided into reaction cavity 1.In Fig. 1, skeleton map
Show that vacuum provides device 2, but it there can be complicated structure in practice.As example, vacuum, which provides device 2, to be included
Vacuum acquiring system, vacuum measurement and vacuum-control(led) system.Vacuum acquiring system can be for example with mechanical pump and molecular pump
Pump group, to realize the high vacuum of whole system.The target base vacuum of the system design is 10-5~10-6Pa.So selecting
When pump group, the preferred larger molecular pump of pumping speed.Vacuum measurement and control system can be for example, by automatic butterfly valves and vacuum
Measuring instrument forms closed loop feedback, so as to control the air pressure in reaction chamber so that the condition tested every time can be steady
It is fixed.Vacuum measurement instrument can for example include vacuum gauge and supporting power supply.
Source feedway 3 is connected with reaction cavity 1, the supply response gas into reaction cavity 1.Source feedway 3 can be with
Including reacting source memory (not shown), for storage reaction source.In view of the material of the equipment growth of the present invention can be passed through
Expansibility, it is preferable that the equipment is simultaneously equipped with liquid source supply mode 31 and gaseous source supply mode 32.So, entering
During row plane SH wave, even if the type in the source that each layer is applicable is different, this equipment can also be competent at.Correspondingly, source feedway bag
Include the reaction source memory and air inlet component for liquid reaction source, and suitable for vapor reaction source reaction source memory and
Air inlet component.It is understood that although liquid source 31 and gaseous source 32 are respectively connecting to reaction cavity 1 in Fig. 1, they
It can also merge before reaction cavity is entered, that is, share same interface and be connected to reaction cavity.This is not limited by the present invention.
Reaction source memory for fluid supply can be for example closed tank body.When the reaction for participating in chemical gas phase reaction
When the boiling point of material in itself is higher, it is difficult to directly obtain reactant steam.In the case, reactant is carried using carrier gas to enter
Reaction cavity.As shown in Fig. 2 liquid source supply can be by the way of Bubbling method, by gas mass flow gauge to closed
Gas of carrier gas is passed through in the tank body of the source of bank savings.When gas of carrier gas is by liquid reaction material resource bubbling, a part of reactant vaporization to load
In gas bubble, until close to or up the saturation in carrier gas.Contain reactant molecule in gas of carrier gas after bubbling.Liquid will be contained
The carrier gas of body source molecule is transported in reaction cavity, so as to which gaseous reactant is carried in reaction cavity.In view of liquid
Source may need that cooler can be included to maintain the storage temperature required for liquid source in Cord blood, reaction source memory.
Cooler can be semiconductor cold-trap.
When being passed through carrier gas, to ensure the amount of reactant, controller unit such as gas mass flow gauge control can be used to carry
Gas supplies.
Reaction source memory for gaseous source can be conventional gas cylinder, gas tank etc..Supplied for the gas of gaseous source,
Controller unit such as gas mass flow gauge can equally be used.
When using two or more reactants, before reactant is supplied into reaction cavity, it can will contain reactant
Carrier gas and/or or reactant gas access a mixed gas tank for being used for gas buffer, reaction will be re-supplied to after gas mixing
In cavity.
Preferably, by special pipeline, such as airflow duct (not shown), reaction gas or reaction mixture gas are introduced directly into
Reach high-temperature region so that air-flow accurately can smoothly reach growth substrate surface.
The features described above of source feedway can be with independent assortment, so as to controllably supply gaseous reactant material to reaction zone.
Tubular heater 4 is in the reaction cavity 1, has open both ends and the pipe for accommodating growth substrate 5
Chamber 6.Tubular heater 4 can be disposed with substantial horizontal.In Fig. 1, growth substrate 5 is directly placed at the bottom of tubular heater 4
Portion, but it can not also be contacted with tubular heater, such as be located at by bed support in tube chamber 6.Tubular heater 4 rises
To heating tube chamber 6 so as to providing the effect of the temperature needed for chemical vapor deposition.
Preferably, the cross section of tubular heater 4 is rectangle.In other words, heater is designed to four face closures, such as Fig. 3
It is shown, only reserve the catalyst movement that two sides open end picks and places and supplemented for sample.The heater can use tantalum wire
Or tungsten filament is heated, it can ensure that temperature reaches the growth temperature of material.And this enclosed heating unit in four sides, can be with
Stable thermal field is effectively formed, flat-temperature zone becomes longer, so as to be advantageous to the homoepitaxial of material.And use square-section
Heater, equivalent to carrying out Material growth in the reaction tube of rectangle, and the reaction tube of square-section is relative to the anti-of circle
Should for pipe its horizontal uniformity it is more excellent.
Catalyst conveyer 7 is also in the reaction cavity 1, for catalyst 8 to be transmitted by tube chamber 6.As
One preferred embodiment, as shown in figure 3, realizing the transmission of volume to volume by two motors for being individually positioned in tube chamber both sides.Use
The sample carrier of tungsten matter carries the catalyst of suspension.Conveyer can be equipped with speed governing power source, with the work(realized crawl, interlocked
Can, the regulation and control of speed speed can also be realized.The distance entirely transmitted is designed as 30cm~40cm.The motor of transmission is placed on pipe
Outside chamber, prevent the lubricant in motor from polluting tube chamber under high temperature high vacuum condition.
In one embodiment, chemical vapor depsotition equipment also includes growth substrate relative position adjusting means.Growth
Substrate relative position adjusting means is used to adjust growth substrate and the relative position of catalyst, so as to promote to deposit.Therefore, grow
Substrate relative position adjusting means can adjust the position of growth substrate, or the position of regulation catalyst, or both regulations simultaneously.
In Fig. 1, growth substrate relative position adjusting means 9, which is portrayed as, is connected on tubular heater 4, by adjusting tubular heater
4 position drives growth substrate 5, so as to adjust the relative position between catalyst 8.It is to be understood that growth substrate is relative
Apparatus for adjusting position 9 can also be connected on catalyst conveyer 7, the first-class suitable position of growth substrate 5.
Preferably, heater height adjusting means is attached on tubular heater, is adjusted as growth substrate relative position
Device 9.One example of heater height adjusting means includes lifting motor and lifting motor axle, and tubular heater can be made whole
Lift, as shown in FIG. 3 body.Pass through tubular heater integral elevating, thus it is possible to vary place growth base on its bottom surface
Relative distance between bottom and suspended catalyst.
The all parts of the equipment of the present invention are described in detail above in association with Fig. 1, but the invention is not restricted to this.This area skill
Art personnel can be modified to all parts without departing from the spirit of the invention.The feature of each part can basis
Need to be combined.
In an especially preferred embodiment,
The tubular heater is horizontal positioned, and cross section is rectangle, and bottom surface is used to place growth substrate,
The chemical vapor depsotition equipment also includes growth substrate relative position adjusting means, and the growth substrate is with respect to position
It is heater height adjusting means to put adjusting means,
The reaction cavity has double-deck double wall water cooled housing,
The source of the source feedway is liquid source and gaseous source,
The source feedway includes the reaction source memory for liquid source and the carrier gas by the reaction memory
Bubbler, the reaction source memory include semiconductor cold-trap,
The catalyst conveyer is volume to volume conveyer belt, for making the one end of catalyst via the tubular heater
The tube chamber is left into the tube chamber, and via the other end of the tubular heater.
The equipment of the present invention can provide high vacuum, while easily can supplement catalyst to reaction zone.It is of the invention special
It is not suitable for the CVD processes required to vacuum and catalyst change, such as two-dimentional hexagonal boron nitride-two-dimensional graphene is folded
It is prepared by the CVD of Rotating fields.
Therefore, it is used to prepare two-dimentional hexagonal boron nitride-two-dimensional graphene lamination knot the invention provides the equipment of the present invention
The purposes of structure.
Heretofore described " two dimension " includes but is not limited to monoatomic layer.
Present invention also offers a kind of chemical gaseous phase depositing process, including：The vacuum in reaction cavity is provided, wherein in institute
State and tubular heater is provided with reaction cavity, the tubular heater has open both ends and for accommodating growth substrate
Tube chamber, wherein the growth substrate has been placed in tube chamber；Reacting gas is passed through into reaction cavity；Catalyst is transmitted and passed through
Tube chamber；And heat the tube chamber with the tubular heater；So that the reacting gas is anti-in the presence of the catalyst
Should and it deposit in the growth substrate.
The chemical gaseous phase depositing process of the present invention individually is used to deposit in vacuum cavity with tubular heater heating tube chamber
Thing grows, and can supplement catalyst to reaction zone at any time, particularly suitable for what is required to vacuum and catalyst change
CVD processes.
It is used to prepare two-dimentional hexagonal boron nitride-two-dimensional graphene laminated construction present invention provides the method for the present invention
Purposes.
The present invention is made below in conjunction with the preparation process embodiment of two-dimentional hexagonal boron nitride-two-dimensional graphene laminated construction
Further it is described in detail.
The preparation of embodiment two dimension hexagonal boron nitride-two-dimensional graphene laminated construction
Prepared using the equipment of the present invention.First using as the 25 of growth substrate microns of thick copper foils and as catalysis
50 microns of thick copper foils of agent are loaded into reaction cavity by the work enabling on reaction cavity.Set in reaction cavity just like figure
The tubular heater and volume to volume catalyst conveyer of the square-section of horizontal setting shown in 3.Growth substrate is placed on heating
On the bottom surface of device, catalyst, which is put on the tungsten bracket of catalyst conveyer belt, is used as suspended catalyst.Tubular heater and lifting electricity
Machine is connected.By controlling lifting motor, adjustment the distance between growth substrate and suspended catalyst is within 1 millimeter.Then will
Reaction cavity good seal.The cooling water system of reaction cavity is opened, keeps shell cavity cooling.Open point that vacuum provides device
Sub- pump group, the base vacuum in reaction cavity is waited to reach 10-6Pa.Heater is connected, 1050 DEG C of annealing is carried out to substrate
Processing.After the completion of annealing, temperature is set to 1000 DEG C of target growth temperature, waiting temperature is stable.
Then the growth of two-dimentional hexagonal boron is carried out.For hexagonal boron, liquid source borazine is used.It is logical
The source feedway of mistake is passed through process gas.Specifically, in the reaction source memory of liquid borazine is accommodated, bubbling is opened
Device valve, the carrier gas nitrogen of 0.5sccm flows is passed through by gas mass flow gauge, by the forerunner for growing hexagonal boron nitride
Body is loaded into carrier gas nitrogen from liquid source.By buffering after the mixed gas tank of carrier gas arrival, pass through gas conduit and reach high temperature
Vitellarium.Setting growth air pressure 3Pa, makes the process atmospheric pressures of whole growth course be in a controlled state.During this, hang
Floating catalyst is without mobile, because growth substrate copper foil can be as the catalyst to growth hexagonal boron nitride.At 1000 DEG C by life
After 20 minutes for a long time, two-dimentional hexagonal boron growth finishes.
Then, the air intake valve of liquid source and the gas mass flow gauge on this road are closed, opens inert gas flowmeter
System is purged, in order to make the growth of subsequent graphene not influenceed by residual gas.
After purged, inert gas is closed.Reusing vacuum offer device rises system vacuum until stable.With
Afterwards, start to grow graphene.The growth of graphene uses gaseous source methane, by air intake valve and mass flowmenter, through too slow
Rush area and gas conduit reaches high growth temperature area.During graphene growth, start catalyst conveyer, because in life
After having grown hexagonal boron, the catalytic action of growth substrate is shielded, it is necessary to which continually introducing new catalyst copper can just enter
The growth of row graphene.The pattern of transmission can select gearing or Manual Mode, generally, Manual Mode, and
And the distance of each crawl is determined according to the size of substrate and the speed of growth.In the present embodiment, each crawl away from
From for 1 centimetre.At a temperature of 1000 DEG C, after the growth of 30 minutes, hexagonal boron nitride is completely covered in graphene, obtains two
Tie up hexagonal boron nitride-two-dimensional graphene laminated construction.
Using the apparatus and method of the present invention, good two-dimentional hexagonal boron nitride-two can be made with high repeatability
Graphene laminated construction is tieed up, and cost is not high.
The present invention equipment not only can with chemical vapor deposition prepare two kinds of materials lamination, from autgmentability for,
The lamination for preparing more than three kinds materials, such as hexagonal boron nitride-three layers of graphene-hexagonal boron nitride hetero-junctions knot can also be used for
Structure, on condition that these materials synthesize suitable for CVD method.
Fig. 4 is the configuration diagram of the preparation process of embodiments of the invention, schematically illustrates each portion of the present invention
/ functional relationship.The system of the present invention can be divided into three parts：Source supply system, growth chamber and peripheral system.
Source supply system includes liquid source and gaseous source, controls gas flow with flowmeter respectively.Reacting gas is through slow
Enter reaction cavity after punching.There are tubular heater and temperature measuring equipment in reaction cavity, there is provided middle part constant high temperature and both ends open
Vitellarium.Catalyst transmission system transports catalyst to vitellarium.As growth substrate relative position adjusting means, reaction chamber
There can be heater lowering or hoisting gear in body.Also include vacuum measurement instrument in reaction cavity, its group such as vavuum pump with periphery
Vacuum into closed loop feedback provides device.Also include water-cooling system in reaction cavity, keep reaction cavity cold wall.In peripheral system
Also include necessary power supply and control system, it can include such as hardware, software, human-computer interaction interface etc..
The apparatus and method structure of the present invention is concise, can keep high vacuum environment, can continue supplement catalyst, can be with
The position of flexible modulation catalyst and growth substrate, and it is applied to different types of reactant source.
The present invention is illustrated above by drawings and examples.It should be appreciated that the scope of the present invention not limited to this.This area
Technical staff can modify and change in the case where not departing from the precursor of spirit of the present invention to embodiments herein.
Claims (10)
1. a kind of chemical vapor depsotition equipment, the chemical vapor depsotition equipment includes：
Reaction cavity；
Vacuum provides device, and the vacuum provides the vacuum in the device offer reaction cavity；
Reacting gas is supplied in the reaction cavity by source feedway, the source feedway；
Tubular heater, the tubular heater are in the reaction cavity, are had open both ends and are grown for accommodating
The tube chamber of substrate；
Catalyst conveyer, the catalyst conveyer are in the reaction cavity, are passed through for catalyst to be transmitted
Tube chamber.
2. chemical vapor depsotition equipment according to claim 1, wherein,
The cross section of the tubular heater is rectangle.
3. chemical vapor depsotition equipment according to claim 1, the chemical vapor depsotition equipment also includes growth substrate
Relative position adjusting means.
4. chemical vapor depsotition equipment according to claim 1, wherein,
The reaction cavity has double-deck double wall water cooled housing.
5. chemical vapor depsotition equipment according to claim 1, wherein,
The source feedway includes reaction source memory.
6. chemical vapor depsotition equipment according to claim 1, wherein,
The source of the source feedway is liquid source and/or gaseous source.
7. chemical vapor depsotition equipment according to claim 1, wherein,
The catalyst conveyer is volume to volume conveyer belt, for making catalyst enter via one end of the tubular heater
The tube chamber, and leave the tube chamber via the other end of the tubular heater.
8. chemical vapor depsotition equipment according to claim 1, wherein,
The cross section of the tubular heater is rectangle, and bottom surface is used to place growth substrate,
The chemical vapor depsotition equipment also includes growth substrate relative position adjusting means, and the growth substrate relative position is adjusted
Regulating device is heater height adjusting means,
The reaction cavity has double-deck double wall water cooled housing,
The source of the source feedway is liquid source and gaseous source,
The source feedway includes rousing for the reaction source memory of liquid source and by the carrier gas of the reaction source memory
Bubbler, the reaction source memory include semiconductor cold-trap,
The catalyst conveyer is volume to volume conveyer belt, for making catalyst enter via one end of the tubular heater
The tube chamber, and leave the tube chamber via the other end of the tubular heater.
9. the chemical vapor deposition unit according to claim 1-8 is used to prepare two-dimentional hexagonal boron nitride-two-dimensional graphene
The purposes of laminated construction.
10. a kind of chemical gaseous phase depositing process, the described method comprises the following steps：
A) vacuum in reaction cavity is provided, wherein tubular heater is provided with the reaction cavity, the tubulose heating
Utensil has open both ends and the tube chamber for accommodating growth substrate, wherein the growth substrate has been placed in tube chamber；
B) reacting gas is passed through into reaction cavity；
C) tube chamber is passed through into catalyst transmission；And
D) tube chamber is heated with the tubular heater；
So that the reacting gas reacts in the presence of the catalyst and deposited in the growth substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711005202.5A CN107815664A (en) | 2017-10-24 | 2017-10-24 | Chemical vapor depsotition equipment, method and purposes |
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| CN109402605A (en) * | 2018-11-15 | 2019-03-01 | 中国人民大学 | A kind of preparation method of the graphene that the large area number of plies is controllable and hexagonal boron nitride hetero-junctions |
| CN110047912A (en) * | 2019-05-24 | 2019-07-23 | 合肥本源量子计算科技有限责任公司 | A kind of vertical heterojunction material and chemical vapor deposition unit |
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