CN110220377A - A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials - Google Patents

A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials Download PDF

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Publication number
CN110220377A
CN110220377A CN201910513539.XA CN201910513539A CN110220377A CN 110220377 A CN110220377 A CN 110220377A CN 201910513539 A CN201910513539 A CN 201910513539A CN 110220377 A CN110220377 A CN 110220377A
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China
Prior art keywords
gas
cooling
distributor disk
simple substance
crucible
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CN201910513539.XA
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Chinese (zh)
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刘建军
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Individual
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Individual
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Priority to CN201910513539.XA priority Critical patent/CN110220377A/en
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Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00Crucible or pot furnaces
    • F27B14/08Details peculiar to crucible or pot furnaces
    • F27B14/10Crucibles
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/02Supplying steam, vapour, gases, or liquids
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00Cooling of furnaces or of charges therein
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00Cooling of furnaces or of charges therein
    • F27D2009/0002Cooling of furnaces
    • F27D2009/0005Cooling of furnaces the cooling medium being a gas

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials, it is related to technical field of new material preparation, the present invention is by being arranged gas distributor disk (9) below crucible body (4), the venthole (7) of crucible body bottom is arranged in gas vent connection on gas distributor disk, it is not at gas distributor disk in metallic solution, it effectively prevents gas from cracking occurring in gas distributor disk and generates graphene or other simple substance carbons etc., further, raising cooling effect is mentioned, gas distributor disk is placed in cooling body, then cooling gas is passed through in cooling body to cool down gas distributor disk, preferably gas distributor disk can be cooled down, it prevents gas from cracking occurring in gas distributor disk and generates graphene or other simple substance carbons etc., the phenomenon that can also preventing blocking venthole simultaneously, the present invention has structure Simply, the features such as using effect is good is suitble to large-scale promotion and application.

Description

A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials
[technical field]
The present invention relates to technical field of new material preparation, and in particular to one kind is used to prepare simple substance two-dimensional material and other multiple The crucible of condensation material.
[background technique]
Known, the development of simple substance two-dimensional material and composite material to modern science and technology has highly important effect. The depth of investigation and application range and its speed and scale of production development of simple substance two-dimensional material and composite material, it has also become measure The one of the important signs that of the technologically advanced level of one national science.Since the 21th century, global simple substance two-dimensional material and compound Material market rapid growth, Asia especially Chinese market increase very fast.Wherein composite material it is common for silicon packet carbon composite, Carbon packet silicon composite etc., simple substance two-dimensional material are graphene, high quality BN, MOS2Deng, by taking graphene growth as an example, graphene Be one kind by carbon atom with sp2Hybridized orbit forms the two-dimentional carbon nanomaterial that hexangle type is in honeycomb lattice.Graphene has excellent Different optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and in terms of there is weight A kind of application prospect wanted, it is considered to be future revolutionary material.Univ Manchester UK physicist An Delie lid Nurse and Constantine's Nuo Woxiao love isolate graphene, therefore common acquisition with micromechanics stripping method success from graphite Nobel Prize in physics in 2010, the method for the common production of graphene are mechanical stripping method, oxidation-reduction method, the life of SiC extension Regular way and chemical vapour deposition technique (CVD).
Chemical vapour deposition technique is that (CVD) is to carry out the obtained graphene that is vapor-deposited using carbon containing organic gas for raw material Method.This is current production graphene most efficient method.The graphene of this method preparation has area greatly and quality is high Feature, but it is primarily present the major drawbacks such as production cost is higher, and production efficiency is low at this stage, and process conditions also need further complete It is kind, then how to provide a kind of device for being used to prepare simple substance two-dimensional material and other composite materials just at those skilled in the art The long-term technology demand of member, and crucible is one of critical component therein in whole device, is used for then how to provide one kind The crucible for preparing simple substance two-dimensional material and other composite materials is also the long-term technology demand of those skilled in the art.
[summary of the invention]
In order to realize the goal of the invention, the present invention provides one kind to be used to prepare simple substance two-dimensional material and other composite woods The crucible of material, by the way that gas distributor disk is arranged below crucible body, the gas vent connection on gas distributor disk is set the present invention Set the venthole in crucible body bottom, effectively prevent mixed gas occur in gas distributor disk cracking generate graphene or The features such as other simple substance carbons etc., the present invention have structure simple, and using effect is good.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials, including crucible body and gas distribution Box is equipped with gas distributor disk in the lower section of the crucible body, in the upper surface of described gas distributor disk equipped at least one exhaust Hole, each gas vent are respectively connected to the venthole of crucible body bottom, the gas distributor disk connect at least one into Tracheae forms the crucible for being used to prepare simple substance two-dimensional material and other composite materials.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the upper surface of the gas vent and logical Ventilation nozzle is equipped between the lower end surface of stomata.
The periphery of the crucible for being used to prepare simple substance two-dimensional material and other composite materials, the gas distributor disk is set There is cooling body.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the first structure of the cooling body To be equipped with the hollow molded cavity extended downwardly in the lower end surface of the crucible body, cover board is equipped in the open end of hollow molded cavity lower part So that the inside of hollow molded cavity is formed a closed cooling chamber, gas distributor disk, the cooling chamber are equipped in the cooling chamber It is separately connected at least a cooling gas air inlet pipe and at least one cooling gas escape pipe.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, be respectively equipped in the cooling chamber to A few cooling gas air inlet and at least one cooling gas gas outlet, each cooling gas air inlet and cooling gas outlet Mouth is separately connected cooling gas air inlet pipe and cooling gas escape pipe.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the cooling gas escape pipe it is outer Port connects pressure-regulating valve.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, gas distribution outer box wall with it is cold But gas drainage plate is equipped between the inner wall of room.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the second structure of the cooling body There is cooling tube to coil on the outer edge surface of the gas distributor disk, the air inlet of the cooling tube connects cooling gas air inlet The gas outlet of pipe, cooling tube connects cooling gas escape pipe.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the third structure of the cooling body To be equipped with thermal insulation layer on the outer edge surface of the gas distributor disk or in the periphery setting thermal insulation layer of gas distributor disk.
The crucible for being used to prepare simple substance two-dimensional material and other composite materials, the external port connection of the air inlet pipe Gas mixing valve, the Gas mixing valve connect gas source.
Due to the adoption of the technical scheme as described above, the invention has the following beneficial effects:
For the present invention by the way that gas distributor disk is arranged below crucible body, the gas vent on gas distributor disk connects setting Venthole in crucible body bottom, is not at gas distributor disk in metallic solution, effectively prevents gas from distributing in gas Cracking generation graphene or other simple substance carbons etc. occur in box and has further mentioned raising cooling effect, gas distributor disk is placed in In cooling body, it is then passed through cooling gas in cooling body, gas distributor disk is cooled down, it can be preferably to gas Distributor disk is cooled down, and is prevented gas from cracking occurring in gas distributor disk and is generated graphene or other simple substance carbons etc., simultaneously also The features such as the phenomenon that can preventing blocking venthole, the present invention has structure simple, and using effect is good, is suitble to promote on a large scale And application.
[Detailed description of the invention]
Fig. 1 is structural schematic diagram of the invention;
Fig. 2 is the second structural schematic diagram of the invention;
Fig. 3 is third structural schematic diagram of the invention;
Fig. 4 is the 4th structural schematic diagram of the invention;
Fig. 5 is the structural schematic diagram of gas distributor disk in the present invention;
Fig. 6 is application schematic diagram of the invention;
In figure: 1, shell;2, insulating layer;3, heater;4, crucible body;5, metallic solution;6, hollow molded cavity;7, it ventilates Hole;8, ventilation nozzle;9, gas distributor disk;10, air inlet pipe;11, cooling gas air inlet pipe;12, cover board;13, cooling gas outlet Pipe;14, cooling chamber;15, gas drainage plate;16, thermal insulation layer.
[specific embodiment]
The present invention can be explained in more detail by the following examples, the open purpose of the present invention is intended to protect the present invention All changes and improvements in range, the invention is not limited to the following examples;
Firstly the need of explanation, "upper" that the present invention is used in description scheme, "lower", "front", "rear", " left side ", The orientation or positional relationship of the instructions such as " right side ", "top", "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, It is merely for convenience of description and simplification description, rather than the device or element of indication or suggestion meaning there must be specific side Position is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
A kind of crucible for being used to prepare simple substance two-dimensional material and other composite materials in conjunction with described in attached drawing 1~6, including earthenware Crucible ontology 4 and gas distributor disk 9 are equipped with gas distributor disk 9 in the lower section of the crucible body 4, in the gas distributor disk 9 It is equipped at least one gas vent above, each gas vent is respectively connected to the venthole 7 of 4 bottom of crucible body, the gas Body distributor disk 9 connects at least one air inlet pipe 10, when it is implemented, can be in the upper surface of gas vent and the lower end of venthole 7 It is equipped with ventilation nozzle 8 between face, is equipped with cooling body, the first structure of the cooling body in the periphery of the gas distributor disk 9 To be equipped with the hollow molded cavity 6 extended downwardly in the lower end surface of the crucible body 4, it is equipped in the open end of 6 lower part of hollow molded cavity Cover board 12 makes the inside of hollow molded cavity 6 form a closed cooling chamber 14, and gas distributor disk is equipped in the cooling chamber 14 9, the shape of the gas distributor disk 9 is square hollow structure or tubular type structure or serpentine configuration (being detailed in attached drawing 5) or other Anisotropic approach is equipped at least one gas vent in the upper surface of described gas distributor disk 9, and each gas vent is respectively connected to earthenware The diameter of the venthole 7 of 4 bottom of crucible ontology, the venthole 7 is 0.1~1.5mm, in the specific implementation, in order to make crucible sheet Certain distance is kept between body 4 and gas distributor disk 9, the gas that is transmitted to for keeping the heat of 4 bottom of crucible body as few as possible divides With on box 9, while the distance between crucible body 4 and gas distributor disk 9 can be such that cooling gas passes through, and make 9 quilt of gas distributor disk Be fully cooled, between the upper surface of the gas vent and the lower end surface of venthole 7 be equipped with ventilation nozzle 8, the two of the ventilation nozzle 8 End can choose the upper end of the lower end and gas vent that are respectively welded at venthole 7;The gas distributor disk 9 connect at least one into Tracheae 10, the cooling chamber 14 are separately connected at least a cooling gas air inlet pipe 11 and at least one cooling gas escape pipe 13 Form the crucible for being used to prepare simple substance two-dimensional material and other composite materials.
In the specific implementation, the cooling chamber 14 is perforated equipped at least one air inlet pipe, in the perforation of each air inlet pipe It is respectively equipped with air inlet pipe 10.Further, in order to ensure cooling chamber 14 forms a closed chamber, in air inlet pipe perforation Sealing mechanism is equipped between inner edge surface and the outer edge surface of air inlet pipe 10, the sealing mechanism is o-ring or high-temperature resistant seal ring.
Further, in the specific implementation, at least one cooling gas air inlet and extremely is respectively equipped in the cooling chamber 14 A few cooling gas gas outlet, each cooling gas air inlet and cooling gas gas outlet are separately connected cooling gas air inlet pipe 11 and cooling gas escape pipe 13.At this point, reaching expected cooling effect in order to ensure the pressure of cooling gas in cooling chamber 14 Fruit connects pressure-regulating valve in the external port of the cooling gas escape pipe 13.
Further, in the specific implementation, the external port of the air inlet pipe 10 connects Gas mixing valve, and the Gas mixing valve connects gas Source, the present invention in the specific implementation, gas source can be single methane gas, silane gas, acetylene gas or other gases, It can be the mixed gas of methane or acetylene with nitrogen or other inert gases, or the Combination gas of methane and silane Body, when implementation, the type and combination of gas should be selected according to specifically product is prepared, and such as be passed through methane and silane Mixed gas can prepare Si-C composite material etc..
Further, in the specific implementation, in order to ensure cooling effect, in 9 outer wall of gas distributor disk and cooling chamber 14 Inner wall between be equipped with gas drainage plate 15.
Further, in the specific implementation, the second structure of the cooling body is the outer edge surface in the gas distributor disk 9 Upper coiling has cooling tube, and the air inlet of the cooling tube connects cooling gas air inlet pipe 11, and the gas outlet of cooling tube connects cooling Gas escape pipe 13.The purpose of coiling cooling tube is can be passed through cooling air in cooling tube to cool down to gas distributor disk 9 Body can also be passed through cooling liquid.
Further, in the specific implementation, the third structure of the cooling body is the outer edge surface in the gas distributor disk 9 It is equipped with thermal insulation layer 16 or the periphery setting thermal insulation layer 16 in gas distributor disk 9.Thermal insulation layer 16 can isolate heater 3 or shell Temperature in 1 radiates the heat of gas distributor disk 9, and then realizes the purpose for reducing by 9 temperature of gas distributor disk.
Application Example of the invention is as follows:
By taking prepared by graphene as an example, as shown in Fig. 2, the present invention is when implementing, crucible body 4 is in shell 1, is then existed The periphery setting heater 3 of crucible body 4 is equipped on the inner wall of shell 1 and protects at this time in order to increase the heat insulation effect of shell 1 Warm layer 2, is then arranged metal block in crucible body 4, the preferred copper of metal block, the purity of copper preferably 99.9% or more, When it is implemented, the catalyst such as nickel, iron, cobalt can be added in copper melt, it is therefore an objective to accelerate reaction rate;
Then startup power supply, is passed through argon gas in shell 1, pressure 0.1mpa, by heater 3 to crucible body 4 into Row heating, open gas source after the metal molten in crucible body 4 is at molten metal, the gas in gas source by air inlet pipe 10 into Enter gas distributor disk 9, gas distributor disk 9 is placed in cooling chamber 14 at this time, and cooling gas enters cold by cooling gas inlet pipe 11 But in room 14, then flowed out by cooling gas escape pipe 13, play and carry out cooling effect to gas distributor disk 9, avoid methane or Acetylene is cracked into carbon because temperature is excessively high with the mixed gas of nitrogen or inert gas in gas distributor disk 9 and in turn results in blocking, Cause methane or acetylene cannot be by the ventilation of 4 bottom of ventilation nozzle 8 and crucible body with the mixed gas of nitrogen or inert gas Hole 7 enters in crucible;
It takes the next step, be drained into metallic solution 5 through the gas vent on gas distributor disk 9 into the mixed gas of metallic solution 5 Middle to form multiple bubbles, gas is decomposed into carbon atom in bubble surface, and carbon atom is re-assemblied in bubble surface as graphene, and Molten surface is reached with bubble afterwards and is flocked together;Gas in the gas source be hydrocarbon gas and inert gas or hydrogen or The mixed gas obtained after any one gas mixing in nitrogen;Hydrocarbon gas accounts for mixed gas gross weight in the mixed gas The 2%~5% of amount;The hydrocarbon gas is methane, acetylene, any one in natural gas;The pressure of the gas source be 0.1~ 1mpa。
The purpose that cooling chamber 14 is arranged in the present invention is methane, acetylene or other in order to avoid entering in gas distributor disk 9 After mixed gas enters gas distributor disk 9, since the temperature height in gas distributor disk 9 leads to methane, acetylene or other mixing Type gas Direct Pyrolysis in gas distributor disk 9 generates graphene, and the graphene generated in gas distributor disk 9 deposits to centainly Latter degree is to block gas vent, and gas distributor disk 9 is also resulted in when serious and is scrapped, and causes unnecessary loss etc..
The present invention is applicable not only to the preparation of graphene, is further adapted to the preparation of other simple substance two-dimensional material materials, such as high Quality BN, MOS2Deng, while the present disclosure additionally applies for the preparations of composite material, such as silicon packet carbon composite, carbon packet silicon composite wood The preparation etc. of material.
Not stating part in the above content carefully is the prior art, therefore does not run business into particular one and state.
The embodiment selected herein to disclose goal of the invention of the invention, is presently considered to be suitable, still, It is to be understood that the present invention is intended to include all changes and improvement that all belong to the embodiment in this design and invention scope.

Claims (10)

1. a kind of crucible for being used to prepare simple substance two-dimensional material and other composite materials, including crucible body (4) and gas distribution Box (9), it is characterized in that: gas distributor disk (9) are equipped in the lower section of the crucible body (4), in the gas distributor disk (9) It is equipped at least one gas vent above, each gas vent is respectively connected to the venthole (7) of crucible body (4) bottom, institute It states gas distributor disk (9) and connects at least one air inlet pipe (10) and form the described simple substance two-dimensional material and other compound of being used to prepare The crucible of material.
2. the crucible according to claim 1 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute It states and is equipped with ventilation nozzle (8) between the upper surface of gas vent and the lower end surface of venthole (7).
3. the crucible according to claim 1 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute The periphery for stating gas distributor disk (9) is equipped with cooling body.
4. the crucible according to claim 1 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute The first structure for stating cooling body is to be equipped with the hollow molded cavity (6) extended downwardly in the lower end surface of the crucible body (4), in The open end of casement chamber (6) lower part, which is equipped with cover board (12), makes the inside of hollow molded cavity (6) form a closed cooling chamber (14), Gas distributor disk (9) are equipped in the cooling chamber (14), the cooling chamber (14) be separately connected an at least cooling gas into Tracheae (11) and at least one cooling gas escape pipe (13).
5. the crucible according to claim 4 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute It states and is respectively equipped at least one cooling gas air inlet and at least one cooling gas gas outlet, each cooling on cooling chamber (14) Gas inlet and cooling gas gas outlet are separately connected cooling gas air inlet pipe (11) and cooling gas escape pipe (13).
6. the crucible according to claim 4 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute State the external port connection pressure-regulating valve of cooling gas escape pipe (13).
7. the crucible according to claim 4 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute It states and is equipped with gas drainage plate (15) between gas distributor disk (9) outer wall and the inner wall of cooling chamber (14).
8. the crucible according to claim 3 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute The second structure for stating cooling body is that coiling has cooling tube on the outer edge surface of the gas distributor disk (9), the cooling tube Air inlet connects cooling gas air inlet pipe (11), and the gas outlet of cooling tube connects cooling gas escape pipe (13).
9. the crucible according to claim 3 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: institute The third structure for stating cooling body is to be equipped with thermal insulation layer (16) on the outer edge surface of the gas distributor disk (9) or distribute in gas Periphery setting thermal insulation layer (16) of box (9).
10. the crucible according to claim 1 for being used to prepare simple substance two-dimensional material and other composite materials, it is characterized in that: The external port of the air inlet pipe (10) connects Gas mixing valve, and the Gas mixing valve connects gas source.
CN201910513539.XA 2019-06-08 2019-06-08 A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials Withdrawn CN110220377A (en)

Priority Applications (1)

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CN201910513539.XA CN110220377A (en) 2019-06-08 2019-06-08 A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910513539.XA CN110220377A (en) 2019-06-08 2019-06-08 A kind of crucible being used to prepare simple substance two-dimensional material and other composite materials

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CN110220377A true CN110220377A (en) 2019-09-10

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804083A (en) * 2022-04-11 2022-07-29 常州二维碳素科技股份有限公司 Graphite crucible cover and CVD method graphene powder system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804083A (en) * 2022-04-11 2022-07-29 常州二维碳素科技股份有限公司 Graphite crucible cover and CVD method graphene powder system

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Application publication date: 20190910

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