CN108203814A - The device of dual cavity is pollution-free chemical vapor deposition two-dimensional material hetero-junctions - Google Patents
The device of dual cavity is pollution-free chemical vapor deposition two-dimensional material hetero-junctions Download PDFInfo
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- CN108203814A CN108203814A CN201810210266.7A CN201810210266A CN108203814A CN 108203814 A CN108203814 A CN 108203814A CN 201810210266 A CN201810210266 A CN 201810210266A CN 108203814 A CN108203814 A CN 108203814A
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- vacuum
- vapor deposition
- chemical vapor
- junctions
- pollution
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Classifications
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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
-
- 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
Abstract
The invention discloses a kind of devices of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity, including vacuum chamber, vacuum chamber is round horizontal vacuum room, and by middle baffle plate, laterally barrier is two chambers, and each chamber is respectively equipped with a set of Catalyt feeding system；It often covers the Catalyt feeding system and respectively includes round tray, upper heater is respectively equipped with above each round tray, set that there are one shared lower heaters below two round trays；Round tray is connect with rotary drive motor, and each upper heater is connect respectively with vertical lift driving motor, and lower heater is connect respectively with vertical lift driving motor and horizontal direction movement driving motor.The structure design of cold wall dual cavity is employed, the chemical vapor deposition of different two-dimensional materials is separated and carried out in two different chambers, removed the process of transfer from, avoid cross contamination by the kinematic system of matching design.
Description
Technical field
The present invention relates to a kind of preparation of nano material and chemical device more particularly to a kind of pollution-free chemical gaseous phases of dual cavity
Deposit the device of two-dimensional material hetero-junctions.
Background technology
Currently with chemical vapor deposition (Chemical Vapor Deposition) technology large area deposition two dimension material
Material, enters into the industrialized production stage since laboratory stage.It may be said that the development and progress of the technology is two-dimensional material
It is able to the foundation stone of promotion and application.
It is divided into two large families in two-dimensional material at present：Graphite alkenes material and transition metal dichalcogenide material.At this
Most important one of graphite alkenes material is exactly graphene in two major class materials, and graphene has fabulous electric property, calorifics
Performance, optical property and mechanical performance, but its zero band gap seriously hinders its application as electronic device, and by base
Bottom impurity scattering can also reduce its electric property, and if graphene can be grown directly upon silicon chip or other target substrate
On, remove the process of transfer from, then the quality of graphene can improve very much.
For two-dimensional material, the problem of carrying out the growth of hetero-junctions in situ, inevitably have cross contamination, this dirt
Dye can have a great impact to the property of material,
Invention content
The object of the present invention is to provide a kind of device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity, energy
Reduce the cross contamination for even preventing process gas when using chemical vapor deposition method growth two-dimensional material hetero-junctions.
The purpose of the present invention is what is be achieved through the following technical solutions：
The device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity of the present invention, including vacuum chamber, institute
Vacuum chamber is stated as round horizontal vacuum room, the vacuum chamber is laterally obstructed by middle baffle plate as two chambers, each chamber
Room is respectively equipped with a set of Catalyt feeding system；
It often covers the Catalyt feeding system and respectively includes round tray, be respectively equipped with and add above each round tray
Hot device, sets that there are one shared lower heaters below two round trays；
The round tray is connect with rotary drive motor, and each upper heater is respectively with being vertically moved up or down driving motor
Connection, the lower heater are connect respectively with vertical lift driving motor and horizontal direction movement driving motor, the driving electricity
Machine is fixed on by sealing flange on the wall of the vacuum chamber.
As seen from the above technical solution provided by the invention, the pollution-free chemistry of dual cavity provided in an embodiment of the present invention
The device of vapor deposition two-dimensional material hetero-junctions employs the structure design of cold wall dual cavity, and the kinematic system of matching design will
The chemical vapor depositions of different two-dimensional materials separates to be carried out in two different chambers, graphene be grown directly upon silicon chip or
In other target substrate, remove the process of transfer from, avoid cross contamination, while hetero-junctions is grown, substantially increase stone
The quality of black alkene.
Description of the drawings
Fig. 1 is the device knot of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity provided in an embodiment of the present invention
Structure schematic diagram.
In figure：
1st, the first upper heater, the 2, first round tray, the 3, second round tray, the 4, second upper heater, 5, lower heating
Device, 6, middle baffle plate.
Specific embodiment
The embodiment of the present invention will be described in further detail below.What is be not described in detail in the embodiment of the present invention is interior
Appearance belongs to the prior art well known to professional and technical personnel in the field.
The device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity of the present invention is preferably embodied
Mode is：
Including vacuum chamber, the vacuum chamber is round horizontal vacuum room, and the vacuum chamber passes through middle baffle plate horizontal stroke
It is two chambers to barrier, each chamber is respectively equipped with a set of Catalyt feeding system；
It often covers the Catalyt feeding system and respectively includes round tray, be respectively equipped with and add above each round tray
Hot device, sets that there are one shared lower heaters below two round trays；
The round tray is connect with rotary drive motor, and each upper heater is respectively with being vertically moved up or down driving motor
Connection, the lower heater are connect respectively with vertical lift driving motor and horizontal direction movement driving motor, the driving electricity
Machine is fixed on by sealing flange on the wall of the vacuum chamber.
A diameter of 25 centimetres of the round tray uniformly opens up 6 diameters on the concentric circles position apart from 7 centimetres of the center of circle
For the circular hole of 5cm, suspended catalyst is placed at the circular hole position；
The size of the vacuum chamber be diameter 400x long 800mm, before be provided with art and craft door, using double-deck double wall water cooling knot
Structure, the manufacture of chamber wall stainless steel material, interface position are equipped with metal washer or fluorine rubber ring, and the middle baffle plate is semicircular
Stainless steel plate.
It further includes alignment system, source supply system, vacuum and obtains system, vacuum measurement system.
The alignment system includes：It limits the laser diode of the upper heater, measure the lower heater with suspending
The grating scale of distance between catalyst, the grating scale for measuring the lower heater present position.
The vacuum obtains system and includes two sets of molecular pumps and its component, high vacuum valve.
The vacuum measurement system includes bigness scale vacuum gauge and thin survey vacuum gauge, and bigness scale vacuum gauge is gamut vacuum gauge,
Thin vacuum gauge of surveying is film rule, and the thin survey vacuum gauge links with butterfly valve.
The source supply system includes two parts, and a part is source, and another part is the gentle bottle of gas mass flow gauge,
The source is divided into gaseous source and liquid source, and the gaseous source is carbon source, and the liquid source is borazine source.
The device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity of the present invention, directly grows graphene
On silicon chip or other target substrate, remove the process of transfer from, substantially increase the quality of graphene, and in growth hetero-junctions
While, avoid cross contamination.
The inventive system comprises：
Catalyt feeding system includes：For placing the movement shaft of the round tray of catalyst, connecting trays and motor,
Sealing flange.
Heating system includes：For the upper heater of heatable catalyst, the vertical lift axis with motor is heated in connection, even
Connect the vertical lift axis of lower heater and lower motor, sealing flange, lower heater.
Alignment system includes：Mainly include three positioning devices：(1) for limiting the laser diode of upper heater, (2)
For measuring the grating scale of distance between lower heater and suspended catalyst, (3) are for measuring the light of lower heater present position
Grid ruler.
Vacuum chamber：For providing the place of chemical vapor deposition.
Kinematic system：Main there are three moving, (1) moves for the vertical direction of upper lower heater, (2) placement catalyst
Round tray rotation, the movement of (3) and lower heater horizontal direction.
Source supply system：For controlling the gas mass flow gauge of gas flow and gaseous source and liquid source.
Vacuum obtains system：Two sets of molecular pumps and its component, high vacuum valve.
Vacuum measurement system：Including two vacuum gauges, one is gamut vacuum gauge, and for bigness scale, another is thin
Film is advised, and for carefully surveying, and links with butterfly valve, closed loop regulation and control are realized to pressure in reaction cavity.
The round tray for placing catalyst is ined succession the motor shaft of vertical direction, can be driven by motor in vertical side
To movement.A diameter of 25 centimetres of the round tray, (copper, stainless steel, tungsten etc.) or ceramic material (such as nitrogen are made using metal
Change boron, ceramics, silicon nitride etc.), rigidity can be effectively ensured in preferably boron nitride at high temperature.The round tray is in distance
The circular hole of 6 a diameter of 5cm, the catalyst that circular hole suspends for placement, the catalyst are provided at the concentric circles that 7 centimetres of the center of circle
Can be copper, platinum, preferably copper.
The vacuum chamber be round horizontal vacuum room, size about diameter 400x 800mm (length), before be provided with art and craft door,
Side opening structure, both ends are opened the door and cavity, using double-deck double wall water-cooling structure, stainless steel material are selected to manufacture, argon arc welding,
Surface carries out special polishing treatment, and interface is sealed using metal washer or fluorine rubber ring sealing.There is one piece of centre in chamber center
Baffle, middle baffle plate refer to one piece of semicircular stainless steel plate in vacuum chamber centre, for obstructing between two chambers
Gas cross pollutes.
The kinematic system includes three independent movements.First kinematic system is upper lower heater in vertical direction
On kinematic system, it is therefore an objective to be respectively：1) control between upper heater and round tray upper surface in the vertical direction
Distance, 2) distance in the vertical direction between control lower heater and round tray lower surface.Second kinematic system be
The rotary motion system of round tray when growing two-dimensional material, is placed with metallic catalyst in the hole of round tray, but raw
After long a period of time, catalyst will fail, so new catalyst is needed to enter high-temperature region.By the rotation of round tray,
New catalyst is brought into high-temperature region, so as to which reactive deposition be maintained to continue in substrate.Third kinematic system is control
The movement of lower heater processed horizontal direction on guide rail.By two motors being fixed at left and right sides of vacuum chamber, add to lower
Hot device carries out differential motion, stretches a contracting for one during movement, can more be accurately controlled mobile distance.Lower heater moves
It is in order to make to be placed on the growth substrate in lower heater to move back and forth between two chambers, so as to contamination-freely grow different
Matter knot.
The source supply system is made of two parts, first, source, another part is the gaseous mass for controlling gas flow
Flowmeter and gas cylinder.Source is divided into gaseous source and liquid source, and the gaseous source is carbon source, as the forerunner needed for growth graphene
Body can select methane, ethylene, acetylene etc., preferably methane；The liquid source is borazine, as growth six sides nitridation
Presoma needed for boron by the way that carrier gas (e.g., argon gas, preferably nitrogen, nitrogen) is passed through in the hermetically sealed can for filling liquid source, carries
Gas will take a part of liquid source out of and enter high temperature reaction zone, so as to provide sufficient presoma for growth.
In device provided by the invention design, the structure design of cold wall dual cavity, the kinetic system of matching design are employed
The chemical vapor deposition of different two-dimensional materials is separated and is carried out in two different chambers, can be significantly reduced material in this way by system
Mutual pollution problem between material, then coordinate and close on catalysis process, deposit the two-dimensional material of one layer of last layer.
Specific embodiment：
As shown in Figure 1, using copper as growth substrate, routing motion system and the method for closing on catalysis, in two chambers
Between move back and forth lifting, a kind of each material of chamber deposition growing finally deposits the side of hexagonal boron nitride/graphene/six
Boron nitride two-dimensional material hetero-junctions.
Upper heater is moved up first, lower heater moves down so that it is easy to operation to reserve enough spaces, then by copper sheet
It is placed on the sample stage of lower heater.The catalyst copper of rounded cap shape is placed in the circular hole of top support plate.Fall upper heater,
The spacing place for reaching photodiode is stopped, and the upper surface of positional distance support plate is 1mm herein.Lower heater is risen, is passed through
The reading of grating scale and the thickness of copper sheet, the lower surface distance for setting copper sheet and rounded cap shape catalyst copper is 30 microns.
Sealing system starts to vacuumize whole system, is extracted into 1 × below 10^-5Pa always.Lower heater in connection
Power supply is heated to 1000 DEG C to system.After reaching 1000 DEG C, kept for 30 minutes, copper sheet is made annealing treatment.Pass through gas
The nitrogen that mass flowmenter is passed through 0.5sccm enters in the jar of storage liquid source (borazine), and liquid source is brought into the
The high temperature reaction zone of one chamber deposits first layer hexagonal boron nitride on copper sheet.After the completion of deposition, stop hexagonal boron nitride forerunner
The supply of body falls lower heater, and heater is moved in second chamber, after reaching precalculated position, slowly rises lower add
Hot device so that growth substrate arrival can close on the distance (being usually tens microns) of catalysis reaction.It will be placed on pallet
Suspended catalyst rotate to the high-temperature region of the second cavity the growth of the second layer material be catalyzed.It is passed through the second layer material institute
The presoma needed, is methane herein, and after a period of time is grown (generally 60 minutes), the second layer material, which can cover with, to be covered
Lid first layer hexagonal boron nitride.After growth, stop the supply of methane, fall lower heater, and heater is moved to
In one chamber, after reaching precalculated position, lower heater is slowly risen so that growth substrate arrival can close on catalysis reaction
Distance.The suspended catalyst pallet of the first cavity is rotated, catalyst is rotated to the high-temperature region of the first cavity, is passed through six side's nitrogen
The presoma for changing boron enters high-temperature region, carries out the deposition of third layer material.By the deposition of 45 minutes, hexagonal boron nitride film meeting
The full graphene of covering.Heater power source is then shut off, waits for the gas that hexagonal boron nitride presoma is turned off after being cooled to room temperature
Mass flowmenter.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (7)
1. a kind of device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity, which is characterized in that including vacuum chamber
Room, the vacuum chamber are round horizontal vacuum room, and by middle baffle plate, laterally barrier is two chambers to the vacuum chamber, often
A chamber is respectively equipped with a set of Catalyt feeding system；
It often covers the Catalyt feeding system and respectively includes round tray, heating is respectively equipped with above each round tray
Device, sets that there are one shared lower heaters below two round trays；
The round tray is connect with rotary drive motor, and each upper heater connects respectively with vertical lift driving motor
It connects, the lower heater is connect respectively with vertical lift driving motor and horizontal direction movement driving motor, the driving motor
It is fixed on by sealing flange on the wall of the vacuum chamber.
2. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 1, feature
Be, a diameter of 25 centimetres of the round tray, uniformly opened up on the concentric circles position apart from 7 centimetres of the center of circle 6 it is a diameter of
Suspended catalyst is placed at the circular hole of 5cm, the circular hole position；
The size of the vacuum chamber is diameter 400x long 800mm, before be provided with art and craft door, using double-deck double wall water-cooling structure,
Chamber wall stainless steel material manufacture, interface position be equipped with metal washer or fluorine rubber ring, the middle baffle plate for it is semicircular not
Become rusty steel plate.
3. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 2, feature
It is, further includes alignment system, source supply system, vacuum and obtain system, vacuum measurement system.
4. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 3, feature
It is, the alignment system includes：It limits the laser diode of the upper heater, measure the lower heater and the catalysis that suspends
The grating scale of distance between agent, the grating scale for measuring the lower heater present position.
5. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 3, feature
It is, the vacuum obtains system and includes two sets of molecular pumps and its component, high vacuum valve.
6. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 3, feature
It is, the vacuum measurement system includes bigness scale vacuum gauge and thin survey vacuum gauge, and bigness scale vacuum gauge is gamut vacuum gauge, thin to survey
Vacuum gauge is film rule, and the thin survey vacuum gauge links with butterfly valve.
7. the device of the pollution-free chemical vapor deposition two-dimensional material hetero-junctions of dual cavity according to claim 3, feature
It is, the source supply system includes two parts, and a part is source, and another part is the gentle bottle of gas mass flow gauge, institute
The source of stating is divided into gaseous source and liquid source, and the gaseous source is carbon source, and the liquid source is borazine source.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810210266.7A CN108203814A (en) | 2018-03-14 | 2018-03-14 | The device of dual cavity is pollution-free chemical vapor deposition two-dimensional material hetero-junctions |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810210266.7A CN108203814A (en) | 2018-03-14 | 2018-03-14 | The device of dual cavity is pollution-free chemical vapor deposition two-dimensional material hetero-junctions |
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| CN108203814A true CN108203814A (en) | 2018-06-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110079792A (en) * | 2019-05-29 | 2019-08-02 | 无锡盈芯半导体科技有限公司 | Bilateral symmetry formula CVD system |
| CN114457424A (en) * | 2022-03-18 | 2022-05-10 | 广州志橙半导体有限公司 | Induction heating epitaxial equipment |
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