CN112813408A - Vapor deposition graphene layer growth preparation device and process - Google Patents
Vapor deposition graphene layer growth preparation device and process Download PDFInfo
- Publication number
- CN112813408A CN112813408A CN202110193070.3A CN202110193070A CN112813408A CN 112813408 A CN112813408 A CN 112813408A CN 202110193070 A CN202110193070 A CN 202110193070A CN 112813408 A CN112813408 A CN 112813408A
- Authority
- CN
- China
- Prior art keywords
- graphite
- vapor deposition
- silicon carbide
- induction coil
- heating element
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000007740 vapor deposition Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 114
- 239000010439 graphite Substances 0.000 claims abstract description 114
- 238000010438 heat treatment Methods 0.000 claims abstract description 65
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 230000006698 induction Effects 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- 150000001721 carbon Chemical group 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 55
- 239000007789 gas Substances 0.000 claims description 53
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 47
- 239000000919 ceramic Substances 0.000 claims description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 238000007789 sealing Methods 0.000 claims description 26
- 238000004321 preservation Methods 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 3
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 230000008021 deposition Effects 0.000 abstract description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C23C16/45559—Diffusion of reactive gas to substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/08—Reaction chambers; Selection of materials therefor
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/10—Heating of the reaction chamber or the substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/02—Elements
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a device and a process for preparing a graphene layer by vapor deposition, wherein the device for preparing the graphene layer by vapor deposition comprises a sealed cavity, a high-vacuum sealed gate valve, a thermal field base, a graphite hard felt heat-insulating layer, a first graphite heating element, a second graphite heating element, a first induction coil and a second induction coil; starting the first induction coil and the second induction coil; heating to reach the target temperature; filling high-purity process gas; the temperature is reduced to the degree centigrade, the substrate slice coated with the coating is taken out, each gas circuit only corresponds to one substrate slice, the problems of uneven inflation pressure and uneven carbon atom deposition caused by the fact that a single gas circuit corresponds to multiple substrate slices are avoided, eight groups of preparation devices are used for simultaneously preparing and producing, wherein each gas circuit independently controls the temperature, controls the flow, and ensures the standardization and controllable reproducibility of the process.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a device and a process for preparing a graphene layer by vapor deposition.
Background
The graphene is a two-dimensional nano material with hexagonal honeycomb lattices formed by arranging carbon atoms, has special physical and chemical properties and has a very wide application prospect. However, since it is a two-dimensional material, it cannot be prepared precisely under the existing processing and preparation technology, and the most promising technology is vapor deposition of graphene coating on a substrate sheet by means of pyrolytic graphite. However, in the metal-based substrate vapor deposition technology, the metal layer needs to be removed by acid cleaning at the later stage to obtain graphene, and the method is high in cost and large in pollution when used for manufacturing a graphene device. And the graphene is directly subjected to vapor deposition on the insulating substrate sheet, so that the steps of acid washing and the like can be omitted, and the graphene and the substrate are directly processed into a device, so that the mainstream technology is formed.
However, how to accurately control the uniformity and consistency of the thickness of the vapor deposition graphene on the single substrate sheet is still difficult; in addition, because the temperature of the pyrolysis hydrocarbon gas is high (about 2000 ℃) in the preparation process, an oxygen-free environment is required, each preparation batch needs to be vacuumized again, a temperature rise and drop process is required, the production cost is very high, the equipment utilization rate is very low, and how to reduce the production cost and improve the production efficiency is important.
Disclosure of Invention
The invention aims to provide a device and a process for preparing a graphene layer by vapor deposition, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a vapor deposition graphene layer growth preparation device and a process thereof comprise a sealed cavity body, and are characterized in that: the vacuum heat-insulating plate is characterized in that a high-vacuum sealing gate valve is transversely arranged at a position, close to the top, on the sealing cavity, a thermal field base is fixedly arranged at the bottom of the sealing cavity, a cylindrical graphite hard felt heat-insulating layer is fixedly connected to the top of the thermal field base, a first graphite heating element and a second graphite heating element are fixedly arranged on the inner wall of the graphite hard felt heat-insulating layer, the first graphite heating element and the second graphite heating element are arranged from bottom to top, a through hole for fixedly connecting a silicon carbide ceramic air inlet pipe is formed in the top of the thermal field base, a carbon-carbon sealing ring is arranged around the upper position of the connecting part of the silicon carbide ceramic air inlet pipe and the thermal field base, a process gas nozzle is fixedly connected to the bottom of the silicon carbide ceramic air inlet pipe, a carbon atom vapor deposition position is corresponding to the position right above the process gas nozzle, and a, the position cover that the hard felt heat preservation of graphite is close to the top is equipped with second induction coil, the impartial distance distribution of first induction coil and second induction coil is in the outside of the hard felt heat preservation of graphite, it is equipped with the infrared temperature measuring device of a plurality of to inlay on the hard felt heat preservation lateral wall of graphite, the hard felt heat preservation of graphite is provided with a plurality of along the circumferencial direction, the top of the hard felt heat preservation of graphite is provided with silicon carbide ceramic tray, be provided with the draw-in groove of a plurality of and the hard felt heat preservation top looks adaptation of graphite along the circumferencial direction equidistance on the silicon carbide ceramic tray, the center of draw-in groove is carbon atom.
As a further scheme of the invention: the process gas nozzle is in the shape of an inverted horn.
As a still further scheme of the invention: the carbon atom vapor deposition position is located on the substrate sheet.
As a still further scheme of the invention: the inboard of draw-in groove is provided with the through-hole, the through-hole has seted up a plurality of along the circumferencial direction on carborundum ceramic tray, fixed mounting has the graphite jib in the through-hole.
As a still further scheme of the invention: the substrate sheet may be a silicon carbide wafer, a graphite wafer or a sapphire wafer, preferably a silicon carbide wafer.
According to another aspect of the present invention, there is provided a process for preparing a graphene layer by vapor deposition, comprising the following steps:
s1: placing the silicon carbide ceramic tray and the substrate slice as required, sealing the sealed cavity, vacuumizing to 7 × 10 of vacuum degree in the furnace cavity-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa；
S2: the first induction coil and the second induction coil are started to induce the corresponding first graphite heating element and the second graphite heating element respectively, the first graphite heating element reaches 2000-2150 ℃, the second graphite heating element reaches 1950-2100 ℃, and the temperature is increased to reach the target temperature for 120-180 min.
S3: filling high-purity process gas into the silicon carbide ceramic gas inlet pipe, wherein the proportion of the high-purity process gas is mixed gas of 5-10ml/min methane and 40-80/min argon, and setting filling time as required;
s5: stopping filling the process gas after the process preparation process is finished, and reducing the temperature of the heating elements of the first graphite heating element and the second graphite heating element to 1500 ℃;
s6: in the cooling process, the silicon carbide ceramic tray is pulled up to the position above the high-vacuum sealing gate valve by using the graphite suspender;
s7: taking out the substrate coated with the coating, placing the substrate to be coated, and vacuumizing the sealed cavity to 7 x 10-3Pa, filling argon protective gas to 5 multiplied by 104After Pa, opening the high-vacuum sealing gate valve, descending the graphite suspender, and dropping the silicon carbide ceramic tray to the original process position;
s8: raising the temperature of the heating element to the process temperature within 30-60 min, and restarting a new round of wafer epitaxial preparation process;
s9: after the reciprocating operation is carried out for 20-30 cycles, the power is cut off, the sealed cavity is opened, and the whole cleaning and correction are carried out.
Compared with the prior art, the invention has the beneficial effects that:
1. each gas circuit only corresponds to one substrate slice, so that the problem of uneven carbon atom deposition caused by uneven inflation pressure due to the fact that a single gas circuit corresponds to multiple substrate slices is solved;
2. eight groups of preparation devices comprising a first induction coil, a first graphite heating element, a second induction coil, a second graphite heating element, a graphite hard felt heat-insulating layer, an infrared temperature measuring device and the like are arranged for simultaneous preparation and production, wherein each gas circuit independently controls the temperature, so that the standardization and controllable reproducibility of the process are ensured;
3. according to the invention, by adding the secondary cavity, the temperature is not reduced in the process of replacing the substrate after the preparation period is finished, the atmosphere pressure of the main cavity is kept unchanged, the preparation time is shortened, and the production cost is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a vapor deposition graphene layer growth preparation device.
Fig. 2 is a partially enlarged view of a vapor deposition graphene layer growth preparation apparatus.
Fig. 3 is a schematic structural diagram of a vapor deposition graphene layer growth preparation device with a silicon carbide ceramic tray lifted.
Fig. 4 is a schematic structural diagram of a silicon carbide ceramic tray in a vapor deposition graphene layer growth preparation device.
Shown in the figure: the device comprises a thermal field base 1, a first induction coil 2, a first graphite heating element 3, a second induction coil 4, a second graphite heating element 5, a carbon-carbon sealing ring 6, a silicon carbide ceramic air inlet pipe 7, a graphite hard felt heat-insulating layer 19, an infrared temperature measuring device 9, a process gas nozzle 10, a carbon atom vapor deposition position 11, a substrate sheet 12, a silicon carbide ceramic tray 13, a clamping groove 14, a through hole 15, a graphite suspender 16, a high-vacuum sealing gate valve 17 and a sealing cavity 18.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-4, in an embodiment of the invention, an apparatus and a process for preparing a graphene layer by vapor deposition, and a packageDraw together thermal field base 1, first induction coil 2, first graphite heat-generating body 3, second induction coil 4, second graphite heat-generating body 5, charcoal carbon seal ring 6, carborundum pottery intake pipe 7, graphite hard felt heat preservation 19, infrared temperature measuring device 9, process gas nozzle 10, carbon atom vapour deposition position 11, substrate piece 12, carborundum pottery tray 13, draw-in groove 14, through-hole 15, graphite jib 16, high vacuum seal push-pull valve 17 and seal chamber 18, seal chamber 18 can guarantee vacuum 10-3Pa magnitude of force, provide required atmosphere environment for epitaxial preparation process, the position that is close to the top on seal chamber 18 transversely is provided with high vacuum seal push-pull valve 17, high vacuum seal push-pull valve 17 can play the encapsulated situation of guaranteeing the cavity after keeping apart the cavity, the bottom fixed mounting of seal chamber 18 has thermal field base 1, the top fixedly connected with cylindric graphite hard felt heat preservation 19 of thermal field base 1, fixed mounting has first graphite heat-generating body 3 and second graphite heat-generating body 5 on the inner wall of graphite hard felt heat preservation 19, first graphite heat-generating body 3 and second graphite heat-generating body 5 are upper-down setting, the through-hole that is used for fixed connection silicon carbide ceramic intake pipe 7 is seted up at the top of thermal field base 1, be provided with charcoal sealing ring 6 around the upper portion position of silicon carbide ceramic intake pipe 7 and thermal field base 1 connecting portion, the bottom fixedly connected with process gas nozzle 10 of carborundum pottery intake pipe 7, carborundum pottery intake pipe 7 is used for the epitaxial in-process to fill process gas, correspond carbon atom vapor deposition position 11 directly over process gas nozzle 10, the position cover that the graphite hard felt heat preservation 19 outside is close to the bottom is equipped with first induction coil 2, the position cover that the graphite hard felt heat preservation 19 is close to the top is equipped with second induction coil 4, first induction coil 2 and the impartial distance distribution of second induction coil 4 are in the outside of graphite hard felt heat preservation 19, inlay on the graphite hard felt heat preservation 19 lateral wall and be equipped with a plurality of infrared temperature measuring device 9, infrared temperature measuring device 9 is used for measuring the temperature of its first graphite heat-generating body 3 that corresponds and second graphite heat-generating body 5 respectively, can control the temperature alone to first graphite heat-generating body 3 and second graphite heat-generating body 5 in the epitaxial technological process, the axial temperature gradient is ensured to meet the requirement of the epitaxial process,the graphite hard felt heat preservation layer 19 is provided with a plurality of along the circumferencial direction, the top of graphite hard felt heat preservation layer 19 is provided with carborundum ceramic tray 13, the carborundum ceramic tray 13 is gone up and is provided with the draw-in groove 14 of a plurality of and the hard felt heat preservation layer 19 top looks adaptation of graphite along the circumferencial direction equidistance, the center of draw-in groove 14 is carbon atom vapor deposition position 11. The silicon carbide ceramic tray 13 plays a role of bearing a substrate sheet 12, the process gas nozzle 10 is in an inverted horn shape, the carbon atom vapor deposition position 11 is located on the substrate sheet 12, the inner side of the clamping groove 14 is provided with a plurality of through holes 15, the through holes 15 are formed in the silicon carbide ceramic tray 13 along the circumferential direction, a graphite hanger rod 16 is fixedly installed in the through holes 15, the silicon carbide ceramic tray 13 can be lifted by pulling the graphite hanger rod 16, the substrate sheet 12 can be a silicon carbide wafer, a graphite wafer or a sapphire wafer, preferably a silicon carbide wafer, the legend 8 is process gas filled in the silicon carbide ceramic air inlet pipe 7, and is generally mixed gas of carbon hydrogen gas and inert gas in a certain proportion; the graphite hard felt heat-insulating layer 19 and the carbon sealing ring 6 both have certain elasticity, so that the carbon sealing ring 6, the graphite hard felt heat-insulating layer 19 and the silicon carbide ceramic air inlet pipe 7 can be tightly combined, air leakage in the extension process is avoided, and an axial temperature gradient of up-cooling and down-heating is formed; the first induction coil 2 and the second induction coil 4 correspond to the first graphite heating body 3 and the second graphite heating body 5 one by one, and the preparation device further comprises a power supply cabinet electrically connected with the first induction coil 2 and the second induction coil 4.
A growth preparation process of a vapor deposition graphene layer comprises the following steps:
s1: placing the silicon carbide ceramic tray 13 and the substrate slice 12 as required, sealing the sealed cavity 18, vacuumizing to 7 × 10-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa；
S2: the power supply cabinet is started, the first induction coil 2 and the second induction coil 4 are started simultaneously, the corresponding first graphite heating element 3 and the second graphite heating element 5 are induced, the first graphite heating element 3 reaches 2000-2150 ℃, the second graphite heating element 5 reaches 1950-2100 ℃, and the temperature rises to the target temperature for 120-180 min. Forming an axial temperature gradient of lower heating and upper cooling, so that carbon atoms can move and attach to the position of the substrate sheet;
s3: filling high-purity process gas into the silicon carbide ceramic gas inlet pipe 7, wherein the proportion of the high-purity process gas is a mixed gas of 5-10ml/min methane and 40-80/min argon, and setting filling time as required;
s5: after the process preparation process is finished, stopping filling the process gas, reducing the power supply power of the power supply cabinet, and reducing the temperature of the heating elements of the first graphite heating element 3 and the second graphite heating element 5 to 1500 ℃;
s6: in the cooling process, the graphite suspender 16 is utilized to pull the silicon carbide ceramic tray 13 up to the position above the high vacuum sealing gate valve 17;
s7: taking out the substrate 12 coated with the coating, placing the substrate 12 to be coated, and vacuumizing the sealed cavity 18 to 7 x 10-3Pa, filling argon protective gas to 5 multiplied by 104After Pa, opening a high vacuum seal gate valve 17, descending a graphite suspender 16, and dropping the silicon carbide ceramic tray 13 to the original initial process position;
s8: raising the temperature of the heating element to the process temperature within 30-60 min, and restarting a new round of wafer epitaxial preparation process;
s9: after 20-30 cycles of such reciprocation, the sealed chamber 18 is de-energized and opened for overall cleaning and calibration. The hydrocarbon gas (such as methane) is decomposed at high temperature, the decomposed carbon atoms are attached to the surface of the substrate sheet 12, the carbon atoms are combined into a graphene-structured coating according to the lattice structure of the substrate sheet 12, the coating thickness can be controlled according to the hydrocarbon gas flow and the spraying time, the larger the hydrocarbon gas flow is, the longer the spraying time is, the thicker the coating thickness is, and the time is generally 5min-150 min.
Detailed description of the preferred embodiment
Firstly, the silicon carbide ceramic tray 13 and the substrate slice 12 are put well according to the requirement, the sealed cavity 18 is sealed, the vacuum is pumped, the vacuum degree of the furnace chamber is 7 multiplied by 10-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa, starting upAnd the source cabinet is used for simultaneously starting the first induction coil 2 and the second induction coil 4 to induce the corresponding first graphite heating element 3 and the second graphite heating element 5, wherein the first graphite heating element 3 reaches 2000 ℃, the second graphite heating element 5 reaches 1950 ℃, and the time for heating to reach the target temperature is 120-180 min. Forming an axial temperature gradient of lower heat and upper cold, facilitating the movement and attachment of carbon atoms to the position of a substrate sheet, filling high-purity process gas through a silicon carbide ceramic air inlet pipe 7, wherein the high-purity process gas is a mixed gas of 5ml/min methane and 40/min argon for 5min, stopping filling the process gas after the process preparation process is finished, reducing the power supply of a power supply cabinet, reducing the temperature of the heating elements of the first graphite heating element 3 and the second graphite heating element 5 to 1500 ℃, pulling up a silicon carbide ceramic tray 13 to be above a high-vacuum sealing gate valve 17 by using a graphite suspender 16 in the temperature reduction process, taking out the substrate sheet 12 plated with the coating, and obtaining the coating with a uniform graphene structure.
Detailed description of the invention
Placing the silicon carbide ceramic tray 13 and the substrate slice 12 as required, sealing the sealed cavity 18, vacuumizing to 7 × 10-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa, starting a power supply cabinet to enable a first induction coil 2 and a second induction coil 4 to be started simultaneously to induce a first graphite heating element 3 and a second graphite heating element 5 which correspond to each other, wherein the first graphite heating element 3 reaches 2090 ℃, the second graphite heating element 5 reaches 2000 ℃, 150min is used when the temperature is raised to the target temperature, high-purity process gas is filled through a silicon carbide ceramic air inlet pipe 7, the filling time is 50min, the process gas is stopped to be filled, the power supply power of the power supply cabinet is reduced, the heating element temperatures of the first graphite heating element 3 and the second graphite heating element 5 are reduced to 1500 ℃, a graphite suspender 16 is used for pulling up a silicon carbide ceramic tray 13 to be above a high-vacuum sealing gate valve 17 in the cooling process, and a substrate slice 12 coated with a coating is taken out, and obtaining a smooth and uniform graphite coating.
Detailed description of the preferred embodiment
Placing the silicon carbide ceramic tray 13 and the substrate slice 12 as required, sealing the sealed cavity 18, vacuumizing to 7 × 10-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa, starting a power supply cabinet to enable a first induction coil 2 and a second induction coil 4 to be started simultaneously to induce a first graphite heating element 3 and a second graphite heating element 5 which correspond to each other, wherein the first graphite heating element 3 reaches 2030 ℃, the second graphite heating element 5 reaches 2000 ℃, 170min is taken for heating to reach a target temperature, high-purity process gas is filled through a silicon carbide ceramic air inlet pipe 7, the filling time is 130min, the filling of the process gas is stopped, the power supply power of the power supply cabinet is reduced, the heating element temperatures of the first graphite heating element 3 and the second graphite heating element 5 are reduced to 1500 ℃, a silicon carbide ceramic tray 13 is pulled up to be above a high-vacuum sealed gate valve 17 by a graphite suspender 16 in the cooling process, and a substrate sheet 12 coated with a coating is taken out, and obtaining a smooth and uniform graphite coating.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (6)
1. A vapor deposition graphene layer growth preparation device comprises a sealed cavity (18), and is characterized in that: the vacuum heat-insulation device is characterized in that a high-vacuum sealing gate valve (17) is transversely arranged at a position, close to the top, on the sealing cavity (18), a thermal field base (1) is fixedly arranged at the bottom of the sealing cavity (18), a cylindrical graphite hard felt heat-insulation layer (19) is fixedly connected to the top of the thermal field base (1), a first graphite heating body (3) and a second graphite heating body (5) are fixedly arranged on the inner wall of the graphite hard felt heat-insulation layer (19), the first graphite heating body (3) and the second graphite heating body (5) are arranged from bottom to top, a through hole for fixedly connecting a silicon carbide ceramic air inlet pipe (7) is formed in the top of the thermal field base (1), a carbon sealing ring (6) is arranged around the upper position of the connecting part of the silicon carbide ceramic air inlet pipe (7) and the thermal field base (1), and a process gas nozzle (10) is fixedly connected to the bottom of the silicon, the carbon atom vapor deposition device is characterized in that a carbon atom vapor deposition position (11) corresponds to the position right above the process gas nozzle (10), a first induction coil (2) is sleeved at a position, close to the bottom, of the outer side of the graphite hard felt heat preservation layer (19), a second induction coil (4) is sleeved at a position, close to the top, of the graphite hard felt heat preservation layer (19), the first induction coil (2) and the second induction coil (4) are distributed at the outer side of the graphite hard felt heat preservation layer (19) at equal distances, a plurality of infrared temperature measuring devices (9) are embedded on the side wall of the graphite hard felt heat preservation layer (19), a plurality of graphite hard felt heat preservation layers (19) are arranged along the circumferential direction, a silicon carbide ceramic tray (13) is arranged above the graphite hard felt heat preservation layer (19), a plurality of clamping grooves (14) matched with the top of the graphite hard felt heat preservation layer (19) are equidistantly arranged on the silicon carbide ceramic tray, the center of the clamping groove (14) is a carbon atom vapor deposition position (11).
2. The vapor deposition graphene layer growth preparation apparatus according to claim 1, wherein: the process gas nozzle (10) is shaped as an inverted trumpet.
3. A vapor deposition graphene layer growth preparation apparatus according to claim 1 or 2, wherein: the carbon atom vapor deposition locations (11) are located on a substrate sheet (12).
4. The vapor deposition graphene layer growth preparation apparatus according to claim 1, wherein: the inboard of draw-in groove (14) is provided with through-hole (15), a plurality of has been seted up along the circumferencial direction on carborundum ceramic tray (13) through-hole (15), fixed mounting has graphite jib (16) in through-hole (15).
5. The vapor deposition graphene layer growth preparation apparatus according to claim 1, wherein: the substrate sheet (12) is a silicon carbide wafer, a graphite wafer or a sapphire wafer, preferably a silicon carbide wafer.
6. A growth preparation process of a vapor deposition graphene layer is characterized by comprising the following steps: the method comprises the following steps:
s1: placing the silicon carbide ceramic tray (13) and the substrate slice (12) as required, sealing the sealed cavity (18), vacuumizing to 7 x 10 of vacuum degree in the furnace chamber-3When Pa, stopping the vacuum pumping action, and introducing argon protective gas to 5 × 104Pa；
S2: starting the first induction coil (2) and the second induction coil (4) to induce the corresponding first graphite heating element (3) and the second graphite heating element (5), wherein the first graphite heating element (3) reaches 2000-;
s3: filling high-purity process gas into the silicon carbide ceramic gas inlet pipe (7), wherein the proportion of the high-purity process gas is a mixed gas of 5-10ml/min methane and 40-80/min argon, and setting filling time according to needs;
s5: stopping filling the process gas after the process preparation process is finished, and reducing the temperature of the heating elements of the first graphite heating element (3) and the second graphite heating element (5) to 1500 ℃;
s6: in the cooling process, the silicon carbide ceramic tray (13) is pulled up to the position above the high-vacuum sealing gate valve (17) by using the graphite suspender (16);
s7: taking out the substrate slice (12) coated with the coating, placing the substrate slice (12) to be coated, and vacuumizing the sealed cavity 18 to 7 x 10-3Pa, filling argon protective gas to 5 multiplied by 104After Pa, opening a high-vacuum sealing gate valve (17), descending a graphite suspender (16), and dropping the silicon carbide ceramic tray (13) to the original process position;
s8: raising the temperature of the heating element to the process temperature within 30-60 min, and restarting a new round of wafer epitaxial preparation process;
s9: after the reciprocating operation for 20-30 cycles, the power is cut off, the sealed cavity (18) is opened, and the whole cleaning and correction are carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110193070.3A CN112813408A (en) | 2021-02-20 | 2021-02-20 | Vapor deposition graphene layer growth preparation device and process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110193070.3A CN112813408A (en) | 2021-02-20 | 2021-02-20 | Vapor deposition graphene layer growth preparation device and process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112813408A true CN112813408A (en) | 2021-05-18 |
Family
ID=75864404
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110193070.3A Pending CN112813408A (en) | 2021-02-20 | 2021-02-20 | Vapor deposition graphene layer growth preparation device and process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112813408A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012028446A (en) * | 2010-07-21 | 2012-02-09 | Kwansei Gakuin | HEAT TREATMENT APPARATUS FOR SiC SEMICONDUCTOR WAFER |
| CN102465333A (en) * | 2010-11-18 | 2012-05-23 | 南京大学 | Vertical hydride vapor phase epitaxy growth system |
| CN103184514A (en) * | 2013-04-11 | 2013-07-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Crystal growing furnace |
| CN104695012A (en) * | 2015-03-24 | 2015-06-10 | 山东大学 | Device and method for preparing large-size high-quality graphene single crystal |
| TW202003377A (en) * | 2018-06-05 | 2020-01-16 | 天主教聖母大學 | SP3-bonded carbon materials, methods of manufacturing and uses thereof |
| US20200373464A1 (en) * | 2018-01-11 | 2020-11-26 | Paragraf Limited | Graphene based contact layers for electronic devices |
| CN215481249U (en) * | 2021-02-20 | 2022-01-11 | 上海岚玥新材料科技有限公司 | Vapor deposition graphene layer growth preparation device |
-
2021
- 2021-02-20 CN CN202110193070.3A patent/CN112813408A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012028446A (en) * | 2010-07-21 | 2012-02-09 | Kwansei Gakuin | HEAT TREATMENT APPARATUS FOR SiC SEMICONDUCTOR WAFER |
| CN102465333A (en) * | 2010-11-18 | 2012-05-23 | 南京大学 | Vertical hydride vapor phase epitaxy growth system |
| CN103184514A (en) * | 2013-04-11 | 2013-07-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Crystal growing furnace |
| CN104695012A (en) * | 2015-03-24 | 2015-06-10 | 山东大学 | Device and method for preparing large-size high-quality graphene single crystal |
| US20200373464A1 (en) * | 2018-01-11 | 2020-11-26 | Paragraf Limited | Graphene based contact layers for electronic devices |
| TW202003377A (en) * | 2018-06-05 | 2020-01-16 | 天主教聖母大學 | SP3-bonded carbon materials, methods of manufacturing and uses thereof |
| CN215481249U (en) * | 2021-02-20 | 2022-01-11 | 上海岚玥新材料科技有限公司 | Vapor deposition graphene layer growth preparation device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103097283B (en) | Process for growth of graphene | |
| CN109280976B (en) | Large-size high-purity silicon carbide single crystal, single crystal substrate and preparation method thereof | |
| CN1555424B (en) | For controlling technique and the product produced thereby of uniformity of film | |
| TWI723579B (en) | Large-size and high-purity silicon carbide single crystal, base material, and preparation method and device for preparation thereof | |
| JP3984820B2 (en) | Vertical vacuum CVD equipment | |
| JP2003086518A (en) | Cvd method of silicon carbide film, cvd unit and susceptor for cvd unit | |
| WO2023082913A1 (en) | Synchronous growth method and device for multi-crucible silicon carbide crystal | |
| KR101719909B1 (en) | Film forming apparatus, susceptor and film forming method | |
| CN215481249U (en) | Vapor deposition graphene layer growth preparation device | |
| CN111074348A (en) | Annealing treatment method and device for reducing internal stress of crystal | |
| CN201740384U (en) | High-temperature vacuum baking oven | |
| CN102703966A (en) | Device for growing carbonization silicon single crystal by using seed crystal temperature gradient method | |
| KR101447663B1 (en) | Film-forming method and film-forming apparatus | |
| CN112553694A (en) | Method and device for high-temperature annealing of silicon carbide single crystal | |
| CN105442038A (en) | Crucible rotating-type silicon carbide single crystal growth method | |
| TWM581766U (en) | MOCVD reactor | |
| CN105556655A (en) | Carbon fiber ring susceptor | |
| CN104233460B (en) | Reaction chamber and MOCVD equipment provided with reaction chamber | |
| CN103603048B (en) | A kind of chemical vapor depsotition equipment for producing silicon carbide epitaxial wafer | |
| CN114561698A (en) | Method for batch production of diamond single crystals by MPCVD (multi-phase chemical vapor deposition) method and molybdenum substrate table | |
| CN112813408A (en) | Vapor deposition graphene layer growth preparation device and process | |
| CN205313716U (en) | Independent rotary mechanism of crucible in siC growth of single crystal equipment | |
| CN116463728B (en) | Apparatus and method for growing high quality silicon carbide crystals | |
| CN106517163B (en) | A kind of cold hearth and continuous producing method preparing graphene for CVD method | |
| CN218175203U (en) | Eight-inch PVT growth furnace with adjustable thermal field |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210518 |