CN214782131U - Two-dimensional material preparation device - Google Patents
Two-dimensional material preparation device Download PDFInfo
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- CN214782131U CN214782131U CN202121176518.2U CN202121176518U CN214782131U CN 214782131 U CN214782131 U CN 214782131U CN 202121176518 U CN202121176518 U CN 202121176518U CN 214782131 U CN214782131 U CN 214782131U
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- 239000000463 material Substances 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 109
- 239000010439 graphite Substances 0.000 claims abstract description 109
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 108
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000010453 quartz Substances 0.000 claims abstract description 87
- 230000007246 mechanism Effects 0.000 claims abstract description 15
- 238000009826 distribution Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims description 21
- 229910052723 transition metal Inorganic materials 0.000 claims description 10
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- 230000000149 penetrating effect Effects 0.000 abstract description 8
- 239000007789 gas Substances 0.000 description 24
- 239000002243 precursor Substances 0.000 description 13
- 239000012159 carrier gas Substances 0.000 description 12
- 229910052961 molybdenite Inorganic materials 0.000 description 10
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 8
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 5
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 5
- 238000010899 nucleation Methods 0.000 description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 4
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
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- 229910002899 Bi2Te3 Inorganic materials 0.000 description 1
- 229910003865 HfCl4 Inorganic materials 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910019029 PtCl4 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
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- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
The utility model provides a two-dimensional material preparation device, belonging to the technical field of two-dimensional material preparation, comprising a quartz tube, wherein the first end and the second end of the quartz tube are provided with openings for air inlet and air outlet respectively; the fixed heating devices are arranged at the upper end and the lower end of the quartz tube and are used for fixing and heating the quartz tube; the graphite workpiece is smaller than the diameter of the quartz tube and is arranged at the bottom of the quartz tube, and a through flat groove is formed in the middle of the graphite workpiece; the exhaust mechanism is arranged at the opening of the second end of the quartz tube and is used for decompressing and exhausting gas in the quartz tube; and the control mechanism controls the first flow speed condition and the first temperature condition, so that the flow field and the temperature field of the graphite workpiece penetrating through the flat groove are more uniform in spatial distribution compared with the graphite workpiece. Through using the utility model provides a two-dimensional material preparation facilities can link up the two-dimensional material that flat inslot obtained large tracts of land and evenly grown at graphite work piece.
Description
Technical Field
The utility model relates to a two-dimensional material preparation field, in particular to two-dimensional material preparation facilities.
Background
The trend in semiconductor materials and device applications is toward miniaturization, which is extremely towards single-atom layers of two-dimensional materials. At present, two-dimensional materials are hot spots of research in the international material field. Two-dimensional materials have atomic-scale thickness, diverse component compositions, layer-number dependence of properties. Single-layer two-dimensional Transition Metal chalcogenides (TMDs), represented by MoS2, have direct band gaps, unlike the semimetal properties of graphene, and are a promising new material for next-generation semiconductor materials. In addition, the two-dimensional materials include non-laminar materials other than the layered materials stacked by van der waals forces, such as MoS2 and WS 2.
In the prior art, a tubular furnace is generally adopted for preparing the two-dimensional material, but in the prior art, the controllability and the stability of the preparation method of the two-dimensional material are poor, and the prepared material is small in area, difficult to grow and thin and easy to grow and thick.
SUMMERY OF THE UTILITY MODEL
The utility model discloses an overcome prior art not enough, provide a two-dimensional material preparation facilities and utilize two-dimensional material preparation method of two-dimensional material preparation facilities to controllable, can grow evenly and thinner two-dimensional material repeatedly.
In order to achieve the above object, an embodiment of the present invention provides a method for preparing a two-dimensional material, including placing a precursor into a quartz tube, and fixing a growth substrate into a through flat slot of a graphite workpiece; leading carrier gas into the quartz tube at a first flow speed condition and passing through the graphite workpiece through flat slot to reach an airflow outlet of the quartz tube at a second flow speed condition, wherein the first flow speed condition is the flow speed of the carrier gas outside the graphite workpiece through flat slot, the second flow speed condition is the flow speed of the carrier gas inside the graphite workpiece through flat slot, and the first flow speed condition is greater than the second flow speed condition; by controlling the first flow speed condition and the first temperature condition, the flow field and the temperature field in the graphite workpiece through flat groove are more uniform in spatial distribution compared with the graphite workpiece, so that a two-dimensional material which is large in area and grows uniformly is obtained in the graphite workpiece through flat groove, and the graphite workpiece through flat groove can be used for preparing two-dimensional materials and two-dimensional non-laminar materials which are difficult to grow.
Optionally, the first flow velocity condition is that the gas flow velocity in a region from the airflow inlet of the quartz tube to the first end of the graphite workpiece is 0.01-0.45 m/s; the first temperature condition is that the temperature outside the graphite workpiece is 0.3 multiplied by 103～1.22×103K。
Optionally, the second flow rate condition is that the flow rate of gas penetrating through the flat groove of the graphite workpiece is 0.01-0.15 m/s; the second temperature condition is that the temperature of the graphite workpiece penetrating through the flat groove is 0.6 multiplied by 103～1.2×103K。
Optionally, the two-dimensional material is a layered transition metal chalcogenide, the precursor is loaded on the front end of the graphite workpiece through flat slot or plated on a growth substrate by a quartz boat, the sulfur source or the selenium source is loaded on the front end of the graphite workpiece through flat slot, and the growth substrate is located in the middle of the graphite workpiece through flat slot.
Optionally, the layered transition metal chalcogenide is MoS2, and the sulfur source and MoO3 as a precursor are respectively loaded on the front end of the interior of the through flat slot of the graphite workpiece by a quartz boat.
Optionally, the layered transition metal chalcogenide is MoS2, the sulfur source is loaded on the front end of the interior of the graphite workpiece through flat slot by using a quartz boat, and MoO3 is plated on the growth substrate as a precursor.
Optionally, the two-dimensional material is a two-dimensional non-layered material, and includes cadmium sulfide, zinc selenide, and two-dimensional iron.
Optionally, the width-height ratio of the through flat slot is 5: 1-20: 1.
optionally, the diameter of the quartz tube is 2.54 cm-11 cm, and the diameter of the graphite workpiece is 1.5 cm-7 cm.
Optionally, the length from the airflow inlet at the first end to the airflow outlet at the second end of the quartz tube is 0.8 m-2 m.
The embodiment of the utility model also provides a two-dimensional material preparation device, which comprises a quartz tube, wherein the first end and the second end of the quartz tube are provided with openings for air inlet and air outlet respectively;
the fixed heating devices are arranged at the upper end and the lower end of the quartz tube and are used for fixing and heating the quartz tube;
the graphite workpiece is smaller than the diameter of the quartz tube and is arranged at the bottom of the quartz tube, a through flat groove is formed in the middle of the graphite workpiece, and a two-dimensional material growth substrate is placed in the through flat groove;
the exhaust mechanism is arranged at the opening of the second end of the quartz tube and is used for decompressing and exhausting gas in the quartz tube;
and the control mechanism controls the first flow speed condition and the first temperature condition to ensure that the flow field and the temperature field in the graphite workpiece through flat slot are more uniform in spatial distribution compared with the graphite workpiece, so that a large-area and uniformly-grown two-dimensional material is obtained in the graphite workpiece through flat slot, and the two-dimensional material comprises a layered transition metal chalcogenide and a two-dimensional non-layered material.
Optionally, the width-height ratio of the through flat slot is 5: 1-20: 1.
optionally, the diameter of the graphite workpiece is 1.5 cm-7 cm.
Optionally, the diameter of the quartz tube is 2.54 cm-11 cm.
Optionally, the graphite workpiece is located in the middle of the quartz tube, and the length of the graphite workpiece is 0.4 m-0.5 m.
Optionally, the length from the airflow inlet at the first end to the airflow outlet at the second end of the quartz tube is 0.8 m-2 m.
Optionally, the graphite workpiece is a cylinder or an elliptical cylinder.
Optionally, the height of the through flat slot is 0.3 cm-2 cm.
Optionally, the two-dimensional material preparation device is a vacuum tube furnace.
To sum up, the beneficial effects of the utility model reside in that:
the embodiment of the utility model provides a two-dimensional material preparation facilities and preparation method thereof, through controlling first flow velocity condition and first temperature condition, it is more even on the outer spatial distribution of graphite work piece to make graphite work piece link up flat inslot flow field and temperature field and compare, thereby it is great, even growth and thinner two-dimensional material to obtain the area in the flat groove to link up at graphite work piece, and can prepare the difficult long thin two-dimensional material or the two-dimensional non-laminar material of ordinary chemical vapor deposition method, controllability in the two-dimensional material preparation process has been promoted greatly, stability. The method can be used for growing the two-dimensional transition metal chalcogenide with uniform thin layer in a controllable and stable manner and is suitable for preparing other two-dimensional materials.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
Fig. 1 is a schematic external structural view of a two-dimensional material preparation apparatus according to an embodiment of the present invention;
fig. 2 is a front view of a two-dimensional material preparation apparatus according to an embodiment of the present invention;
fig. 3 is a cross-sectional view of a two-dimensional material preparation apparatus according to an embodiment of the present invention;
fig. 4 is a schematic diagram illustrating a two-dimensional material manufacturing apparatus according to an embodiment of the present invention;
FIG. 5 is a graph showing the overall gas flow field of a quartz tube without a graphite workpiece during two-dimensional material preparation;
fig. 6 is a gas flow field diagram of a two-dimensional material preparation apparatus according to an embodiment of the present invention during two-dimensional material preparation;
FIG. 7 is a diagram showing the overall temperature field of a quartz tube without a graphite workpiece during two-dimensional material preparation;
fig. 8 is a whole temperature field diagram of the two-dimensional material preparation device according to the embodiment of the present invention when the two-dimensional material is prepared.
In the figure: 1-quartz tube, 2-fixed heating device, 3-graphite workpiece, 4-exhaust mechanism, 5-control mechanism, 6-growth substrate, 7-graphite workpiece external air flow and 8-graphite workpiece through flat slot internal air flow.
Detailed Description
The present invention will be described in further detail below with reference to specific examples for facilitating understanding of those skilled in the art.
The embodiment of the utility model provides a two-dimensional material preparation device, as shown in figure 1, is a vacuum tube furnace, and comprises a quartz tube 1, wherein the first end and the second end of the quartz tube are provided with openings for air inlet and air outlet respectively; the fixed heating devices 2 are arranged at the upper end and the lower end of the quartz tube 1, and the fixed heating devices 2 are used for fixing and heating the quartz tube 1; the diameter of the graphite workpiece 3 is smaller than that of the quartz tube 1, the graphite workpiece is arranged at the bottom 1 of the quartz tube, a through flat groove is formed in the middle of the graphite workpiece 3, and a two-dimensional material growth substrate is placed in the through flat groove; and the exhaust mechanism 4 is arranged at the opening of the second end of the quartz tube 1 and used for decompressing and exhausting in the quartz tube 1.
Please refer to fig. 2, which is a front view of a two-dimensional material preparation apparatus according to an embodiment of the present invention; the two-dimensional material preparation device also comprises a control mechanism 5 which is used for controlling the first flow speed condition and the first temperature condition, so that the flow field and the temperature field in the graphite workpiece 3 penetrating flat groove are more uniform in spatial distribution compared with the graphite workpiece 3, and the two-dimensional material which grows uniformly in a large area is obtained in the graphite workpiece 3 penetrating flat groove.
Please refer to fig. 3, which is a cross-sectional view of a two-dimensional material preparation apparatus according to an embodiment of the present invention. The graphite workpiece 3 is just positioned in the middle of the quartz tube 1, a certain distance is reserved between the front end of the graphite workpiece 3 and the first end of the quartz tube 1, and a certain distance is reserved between the rear end of the graphite workpiece 3 and the first end of the quartz tube 1.
Specifically, the two-dimensional material preparation device of the embodiment of the present invention, the diameter of the graphite workpiece is 1.5cm to 7cm, for example, 5 cm. The diameter of the quartz tube is 2.54 cm-11 cm, for example 10 cm. The length from the airflow inlet at the first end to the airflow outlet at the second end of the quartz tube is 0.8 m-2 m, such as 1.5 m. The width-height ratio of the through flat groove is 5: 1-20: 1, the height of the through flat slot is 0.3 cm-2 cm.
The utility model discloses the width that link up the flat groove is about 4/5 of graphite work piece diameter, can hold growth substrate 6 down. And the width-height ratio of the through flat groove is 5: 1-20: 1, the height of the through flat slot is 0.3 cm-2 cm, and the air flow is limited in a narrow range during the preparation of the two-dimensional material, so that the uniformity of the air flow in the through flat slot is improved, and the air flow rate is reduced. And the gas flow forms a boundary layer on the surface of the growth substrate 6 because the square root of the gas flow rate is inversely proportional to the thickness of the boundary layer, while the mass transport coefficient of the ambient environment and the surface of the growth substrate is proportional to the diffusion coefficient and inversely proportional to the thickness of the boundary layer. The embodiment of the utility model provides an in, boundary layer thickness is great, and surrounding environment and growth substrate surface quality transmission coefficient are less to make the precursor can provide growth substrate 6 surfaces more slowly and uniformly, make the difficult length of two-dimensional material thick, and reduced nucleation density simultaneously, increased two-dimensional material homogeneity, thereby be favorable to growing up of crystal domain, thereby link up the two-dimensional material that the area is great, even growth and comparison is thin at graphite work piece link up the flat inslot.
In other embodiments, the specific width and height of the through flat slot may be determined according to the specific size of the graphite workpiece and the through flat slot, as long as the ratio of the width to the height of the through flat slot is 5: 1-20: the protection scope of the present invention is within the range of 1. The utility model discloses two-dimensional material preparation facilities is at the during operation, through control mechanism 5 controls first flow velocity condition and first temperature condition for the graphite work piece link up flat inslot flow field and temperature field and compare more evenly on the external spatial distribution of graphite work piece, thereby link up the two-dimensional material that the area is great and evenly grow in the flat inslot at the graphite work piece.
The embodiment of the utility model provides a two-dimensional material preparation method uses above-mentioned two-dimensional material preparation facilities to grow two-dimensional material, two-dimensional material includes two-dimentional laminar material and two-dimentional non-laminar material. In this example, the preparation was carried out in MoS2Representative are Transition Metal Dichalcogenides (TMDs).
In other embodiments, for example, graphene, bismuth composite two-dimensional materials, and HfS may also be prepared2,PtS2And the like, which are difficult to grow and thin by a conventional chemical vapor deposition method, or the like, which are difficult to grow and thin, such as cadmium sulfide (CdS), zinc selenide (ZnSe), two-dimensional iron and other metals.
Referring to fig. 4, in order to prepare a two-dimensional material by using the two-dimensional material preparation apparatus of the embodiment of the present invention, a growth substrate 6 is first fixed in a through flat slot of a graphite workpiece 3, and then a precursor is placed in a quartz tube 1, an external airflow 7 of the graphite workpiece is introduced into the quartz tube 1 under a first flow rate condition, an internal airflow 8 of the through flat slot of the graphite workpiece passes through the through flat slot of the graphite workpiece under a second flow rate condition, the first flow rate condition is an external airflow velocity of the through flat slot of the graphite workpiece, the second flow rate condition is an internal airflow velocity of the through flat slot of the graphite workpiece, and the first flow rate condition is greater than the second flow rate condition; by controlling the first flow speed condition and the first temperature condition, the flow field and the temperature field in the graphite workpiece through flat groove are more uniform in spatial distribution than the graphite workpiece, and therefore the two-dimensional material which is large in area, uniformly grows and is thin in thickness is obtained in the graphite workpiece through flat groove.
In an embodiment of the invention, the sulfur source and the MoO as precursor3Quartz boats are respectively loaded at the front ends of the inner parts of the graphite workpiece through flat grooves, and the growth substrate 6 is positioned in the middle of the graphite workpiece through flat grooves.
In another embodiment, a sulfur source is loaded on the front end of the inner part of the graphite workpiece through flat slot by a quartz boat, and MoO3As a precursor, on the growth substrate 6. At the moment, N is introduced from one side of the quartz tube2The carrier gas is used for driving excessive carrier gas to remove air in the tube furnace and heating the carrier gas to ensure that the solid sulfur source and the solid MoO are in contact with each other3Sulfur vapor and MoO converted to vapor state and propelled by carrier gas3The steam reacts in the graphite workpiece through flat groove to generate MoS2Growth is started on the growth substrate 6.
In other embodiments, when the two-dimensional material to be prepared is a transition metal chalcogenide such as PtS2, PtSe2, HfS2, In2Se3, etc., the sulfur source, the selenium source, and PtCl4, HfCl4, In2O3, FeCl3, etc., which are precursors, are respectively loaded on the front end of the interior of the graphite workpiece through flat slot by a quartz boat or the precursors are plated on a growth substrate, and the growth substrate is positioned In the middle of the graphite workpiece through flat slot.
Because the growth of the two-dimensional crystal is determined by the diffusion of the precursor in the boundary layer of the growth substrate 6, the nucleation density is greatly increased by the high-flow-rate reaction gas, and even the gas-phase reaction occurs, so that the obtained two-dimensional material has the defects of small crystal domain, high defect density and larger thickness. And under the conditions of lower second flow rate and more stable second temperature compared with the conditions outside the graphite workpiece in the graphite workpiece through flat groove, sulfur vapor and the MoO3 film serving as the precursor react to grow continuous star-shaped flaky MoS2These star-shaped sheet-like MoS2Can be combined to form continuous single-layer MoS with the size of 2 mm2。
In addition, before the reaction, air inside the device can be extracted through the exhaust mechanism 4 arranged at the second end of the quartz tube, so that the air pressure inside the quartz tube 1 reaches a preset value required by two-dimensional material preparation. Because temperature, atmospheric pressure, reactant concentration isoparametric are different and change according to the two-dimensional material of needs preparation, so accessible when preparing specific two-dimensional material the utility model discloses control mechanism 5 in the embodiment is at certain limit within a definite range dynamic adjustment, as long as make graphite work piece link up the flat inslot flow field and temperature field and compare graphite work piece outer spatial distribution on more even to link up the two-dimensional material that the area is great and evenly grow in the flat groove at graphite work piece, so no longer give unnecessary details here.
In other embodiments, the MoS is removed during preparation2Other two-dimensional materials, e.g. WS2、ReS2、ReSe2、Bi2Se3、Bi2Te3The layered two-dimensional material and the non-layered two-dimensional material such as cadmium sulfide (CdS), lead sulfide (PbS), zinc oxide (ZnO), two-dimensional iron and the like. In addition, mica, gold, sapphire, silicon oxide, or the like can be used as a growth substrate.
Please refer to fig. 5, which is a diagram of an overall gas flow field when a two-dimensional material is prepared for a quartz tube without a graphite workpiece; wherein the coordinate extending along the z-axis direction is the axial length of the quartz tube, and the opening at the first end of the quartz tube is taken as the origin of coordinates; the coordinates extending along the directions of the x axis and the y axis are the radial length of the quartz tube, and the circle center of the quartz tube is taken as the origin of coordinates; the ordinate on the right side of the quartz tube is the flow rate of the carrier gas, wherein the carrier gas flow rate is larger the further upward, the carrier gas flow rate is smaller the further downward. Specifically, the gas flow velocity in the first area in the area with the distance of 0m to 0.4m from the first end pipe orifice of the quartz tube is 0.15 to 0.25 m/s. The gas flow velocity of the second area in the area with the distance of 0.4-0.8 m from the first end pipe orifice of the quartz pipe is 0.05-0.25 m/s. It can be seen that the distribution of gas flow rates is more uniform in the first region than in the second region, but the gas flow rates in the first region have a greater average value than the gas flow rates in the second region.
Because the utility model discloses two-dimensional material preparation facilities's 1 bottoms of quartz capsule are equipped with graphite work piece 3. The diameter ratio of this graphite work piece is little than the quartz capsule pipe diameter in the embodiment of the utility model provides an, the pipe diameter of quartz capsule is 2.54cm ~ 11cm, the diameter of graphite work piece is 1.5cm ~ 7 cm. In other embodiments, the diameter of the graphite workpiece may be adjusted within a proper range according to the diameter of the quartz tube, as long as the condition that the diameter of the graphite workpiece is smaller than the diameter of the quartz tube is satisfied, which is not described herein again.
Fig. 6 is a gas flow field diagram of a two-dimensional material preparation device according to an embodiment of the present invention during two-dimensional material preparation. In this example, the first flow rate condition, i.e., the gas flow rate in the region from the first end of the quartz tube to the first end of the graphite workpiece, was 0.15 m/s; the second flow rate condition is that the gas flow rate of the graphite workpiece penetrating through the flat groove is 0.05 m/s; link up the inside gas velocity of flow of flat groove and be less than the outside gas velocity of flow of flat groove and the inside gas velocity of flow of flat groove, and compare in the quartz capsule that does not contain graphite work piece in figure 5 when carrying out two-dimensional material preparation, the utility model discloses a gas velocity of flow is more even in the quartz capsule of two-dimensional material preparation facilities, and the gas flow change is littleer in the different regions. And the graphite workpiece penetrates through the flat slot, so that the flow rate of carrier gas is reduced, the supply amount of a precursor is further reduced, the nucleation density and the growth rate of the two-dimensional material are reduced, and the growth of the two-dimensional material with large area, uniformity and thin layer number is facilitated.
The above flow rate conditions were only for the preparation of MoS2According to the preferred embodiment of the present invention, when other two-dimensional materials are prepared, the first flow rate condition, i.e., the flow rate of the gas outside the graphite workpiece, can be dynamically adjusted within a range of 0.01-0.45 m/s according to the difference of the two-dimensional materials, and the second flow rate condition, i.e., the flow rate of the gas penetrating through the flat slot of the graphite workpiece, also changes within a range of 0.01-0.15 m/s, so that the detailed description is omitted herein.
Referring to fig. 7, the fixed heating device controlled by the control mechanism heats the outside of the quartz tube to 750K, and the temperature variation range in the quartz tube is shown as the ordinate of the right diagram, and it can be seen that the temperature variation of the quartz tube from outside to inside is not uniform and varies within the range of 300K to 750K due to the heat transfer and heat exchange of the low-temperature gas and the lower heat transfer coefficient of the quartz and the carrier gas, and the temperature tends to be higher at the tube wall of the quartz tube and lower at the center of the quartz tube.
Please refer to fig. 8, which is an overall temperature field diagram of the two-dimensional material manufacturing apparatus according to the embodiment of the present invention when manufacturing two-dimensional material, in this embodiment, the quartz tube 1 is heated to the first temperature condition by the control mechanism, because of the good thermal conductivity of the graphite workpiece 3, it can be seen that the temperature distribution on the graphite workpiece is overall uniform and the temperature of the graphite workpiece inside the through flat slot is 1.2 × 103～1.21×103K, the graphite workpiece 1 has a more stable temperature in the whole, especially in the through flat slot of the graphite workpiece than in FIG. 7And (4) conditions.
The above temperature conditions are also only for the preparation of MoS2In a preferred embodiment of the present invention, the first temperature condition, i.e., the temperature outside the graphite workpiece, is 0.3 × 10, depending on the two-dimensional material to be prepared, when preparing the other two-dimensional material3～1.22×103K is dynamically adjusted within the range of 0.4 multiplied by 10, and the second temperature condition, namely the temperature of the graphite workpiece penetrating through the flat slot is also adjusted within the range of 0.4 multiplied by 103～1.48×103K varies within this range and is not described in detail herein.
The embodiment of the utility model provides a two-dimensional material preparation facilities is when carrying out two-dimensional material preparation, through setting up the graphite work piece that has a perfect understanding flat groove in the quartz capsule for the reactant concentration and the velocity of flow in the flat groove of graphite work piece are showing and are reducing, and lower velocity of flow and stable temperature condition nucleation take shape more easily and grow to diffusion all around, thereby make the number of piles of the two-dimensional material of preparation thinner, the nucleation density is littleer, grow more evenly, the area is bigger.
To sum up, the embodiment of the utility model provides a two-dimensional material preparation method is through controlling first flow velocity condition and first temperature condition for the graphite work piece link up flat inslot flow field and temperature field and compare more evenly on the external spatial distribution of graphite work piece, thereby link up the flat inslot at the graphite work piece and obtain the two-dimensional material that the area is great, even growth, the number of piles is thin. The controllability and the stability of the two-dimensional material in the preparation process are greatly improved. The method can be used for controllably and stably growing the two-dimensional transition metal chalcogenide with large area, uniformity and thin layer number and is suitable for preparing other two-dimensional layered materials or two-dimensional non-layered materials.
Finally, any modification or equivalent replacement of some or all technical features, carried out by means of the device structure of the present invention and the technical solutions of the embodiments, and the obtained essence does not depart from the corresponding technical solutions of the present invention, all belonging to the device structure of the present invention and the patent scope of the embodiments.
Claims (9)
1. A two-dimensional material preparation device is characterized by comprising a quartz tube, wherein the first end and the second end of the quartz tube are provided with openings for air inlet and air outlet respectively; the fixed heating devices are arranged at the upper end and the lower end of the quartz tube and are used for fixing and heating the quartz tube; the graphite workpiece is smaller than the diameter of the quartz tube and is arranged at the bottom of the quartz tube, a through flat groove is formed in the middle of the graphite workpiece, and a two-dimensional material growth substrate is placed in the through flat groove; the exhaust mechanism is arranged at the opening of the second end of the quartz tube and is used for decompressing and exhausting gas in the quartz tube; and the control mechanism controls the first flow speed condition and the first temperature condition to ensure that the flow field and the temperature field in the graphite workpiece through flat slot are more uniform in spatial distribution compared with the graphite workpiece, so that a large-area and uniformly-grown two-dimensional material is obtained in the graphite workpiece through flat slot, and the two-dimensional material comprises a layered transition metal chalcogenide and a two-dimensional non-layered material.
2. The apparatus for preparing a two-dimensional material according to claim 1, wherein the cross-section of the through flat groove is rectangular, and the width-to-height ratio is 5: 1-20: 1.
3. the apparatus of claim 1, wherein the graphite workpiece has a diameter of 1.5cm to 7 cm.
4. The apparatus for preparing a two-dimensional material according to claim 1, wherein the tube diameter of the quartz tube is 2.54cm to 11 cm.
5. The apparatus according to claim 1, wherein the graphite workpiece is located at a central portion of the quartz tube, and the graphite workpiece has a length of 0.4m to 0.5 m.
6. The apparatus according to claim 1, wherein the quartz tube has a length from a first end gas flow inlet to a second end gas flow outlet of 0.8m to 2 m.
7. A two-dimensional material preparation apparatus as defined in claim 1 wherein said graphite workpiece is cylindrical or ellipsoidal.
8. The apparatus for preparing a two-dimensional material according to claim 1, wherein the height of the through flat groove is 0.3cm to 2 cm.
9. The apparatus according to claim 1, wherein the apparatus is a vacuum tube furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114212824A (en) * | 2022-02-23 | 2022-03-22 | 浙江大学杭州国际科创中心 | Method for controllable growth of hexagram single-layer MoS2 |
| CN117488281A (en) * | 2023-12-29 | 2024-02-02 | 琥崧智能装备(太仓)有限公司 | Chemical vapor deposition film preparation device |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114212824A (en) * | 2022-02-23 | 2022-03-22 | 浙江大学杭州国际科创中心 | Method for controllable growth of hexagram single-layer MoS2 |
| CN117488281A (en) * | 2023-12-29 | 2024-02-02 | 琥崧智能装备(太仓)有限公司 | Chemical vapor deposition film preparation device |
| CN117488281B (en) * | 2023-12-29 | 2024-03-19 | 琥崧智能装备(太仓)有限公司 | Chemical vapor deposition film preparation device |
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