CN114436249A - Graphite crucible - Google Patents
Graphite crucible Download PDFInfo
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- CN114436249A CN114436249A CN202210218548.8A CN202210218548A CN114436249A CN 114436249 A CN114436249 A CN 114436249A CN 202210218548 A CN202210218548 A CN 202210218548A CN 114436249 A CN114436249 A CN 114436249A
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- Prior art keywords
- crucible
- graphite crucible
- wall
- supporting platform
- graphite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 132
- 239000010439 graphite Substances 0.000 title claims abstract description 132
- 239000007788 liquid Substances 0.000 abstract description 68
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 64
- 229910052802 copper Inorganic materials 0.000 abstract description 64
- 239000010949 copper Substances 0.000 abstract description 64
- 238000010438 heat treatment Methods 0.000 abstract description 55
- 239000007789 gas Substances 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 229910021389 graphene Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- -1 graphite alkene Chemical class 0.000 description 5
- 230000006698 induction Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 239000011087 paperboard Substances 0.000 description 3
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- 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
- C23C16/003—Coating on a liquid substrate
-
- 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
- C23C16/4418—Methods for making free-standing articles
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a graphite crucible, which comprises a crucible body and a crucible cover, wherein the crucible body comprises a crucible body bottom, an inner wall and an outer wall; the inner wall is provided with a supporting platform, and the supporting platform is used for horizontally placing a crucible cover; the inner wall is provided with a groove, and the groove is connected with the supporting platform; the crucible cover comprises an air inlet and an air outlet. According to the invention, the groove is arranged on the inner wall of the graphite crucible, and is positioned at the position where the supporting platform at the upper opening is connected with the inner wall, so that liquid can be effectively prevented from splashing into the furnace chamber when the graphite crucible is ventilated, and the supporting platform in the graphite crucible is positioned in the heating system, so that the joint surface of the crucible cover and the supporting platform in the graphite crucible is positioned in a high-temperature heating area, and the copper liquid is prevented from being condensed and gathered at the joint position.
Description
Technical Field
The invention belongs to the technical field of crucibles, and relates to a graphite crucible.
Background
The graphene powder grown by the CVD method has the least defects, the thinnest layer number and the largest sheet diameter. CVD growth graphite alkene powder is with copper placement in graphite crucible, under the inert atmosphere protection, high temperature melts into liquid copper, then will let in under liquid copper liquid level with the carbon source gas that inert gas dilutes, along with gaseous continuous letting in, will produce a large amount of bubbles under the copper liquid level, at bubble surface growth graphite alkene, reach the liquid level when the bubble, the bubble is broken, graphite alkene powder and copper film separation, graphite alkene powder is carried away from the blast pipe way by the air current, gets into the collecting box. However, in the process of growing graphene powder, as gas is introduced below the copper liquid level, particularly when large-flow gas is introduced, the copper liquid splashes very seriously and flies out from a gap between a crucible opening and a crucible cover in a large amount, which causes serious potential safety hazard to an induction coil heating system.
CN 213139844U discloses a packaging structure of a graphite crucible, which comprises a honeycomb paperboard box body, wherein the box body is externally tangent to the outer contour line of the graphite crucible, and a layer of polyurethane waterproof paint is coated on the inner surface of the box body; the top surface of the box body is opened and is closed by a box cover; the bottom surface of the box body is formed with a clamping plate and a base plate, the clamping plate and the base plate are matched with the cross section of the box body, the clamping plate is a plywood, a blind groove matched with the bottom surface of the graphite crucible is formed on the upper surface of the clamping plate, and the base plate is a honeycomb paperboard and is arranged at the bottom of the graphite crucible in a penetrating mode; the box body is covered at the outer side of the connecting edge through an L-shaped laminated paperboard; and a polyurethane foam pad which is propped against the side wall of the graphite crucible is formed on the inner side of the vertical connecting edge of the box body. The invention has simple process and convenient processing, and can realize retention protection of the graphite crucible in the package.
CN 103387416A is a method for prolonging the service life of a graphite crucible in medium smelting. The method comprises the following steps of placing a graphite crucible in a furnace body, and installing induction coils in the graphite crucible and the graphite crucible, wherein the method comprises the following steps: (1) fixing a graphite protection ring on the upper edge of a graphite crucible, and then adding industrial silicon into the graphite crucible; (2) starting an induction coil, heating to melt the industrial silicon into silicon liquid, and vertically placing a graphite column at the central shaft of a graphite crucible to enable the liquid level of the silicon liquid to rise; (3) continuously adding industrial silicon into the graphite crucible, controlling the temperature rise of the induction coil to ensure that the liquid level of the molten silicon liquid is higher than the upper edge of the wall of the graphite crucible but lower than the upper edge of the graphite protection ring, and then adding a slag former to ensure that the surface of the molten silicon liquid is still lower than the upper edge of the graphite protection ring, thereby smelting; (4) after the smelting is finished, the silicon liquid reacts with the graphite crucible to obtain a silicon carbide coating, then the graphite column and the graphite protection ring are taken out, and the silicon liquid is poured out after the temperature is reduced.
Because the crucible opening is inevitably higher than the upper surface of the induction coil in order to prevent the refractory sand filled around from falling into the crucible when the crucible is installed, the butt joint position of the crucible cover and the crucible opening is in a low-temperature region. When the mixed gas lets in liquid copper, especially when letting in large-traffic gas, the copper liquid splashes very seriously, and a large amount of copper liquid splashes away from crucible cover and crucible mouth supporting platform gap, can cause serious potential safety hazard to heating system, still can have a large amount of copper to solidify in gap department, gathers, forms big copper post, not only can block up the gas vent, also can cause the crucible cover can't also separate smoothly with the crucible.
In the technical scheme, the copper liquid splashing is avoided by improving the use method of the graphite crucible package. However, the structure of graphite crucible itself is not improved, and therefore, how to change the structure of graphite crucible through the design for the copper liquid of growing graphite alkene powder can not splash, can not have the copper to condense the gathering phenomenon in crucible lid and crucible mouth supporting platform position, is the technical problem that graphite crucible technical field needs to solve urgently.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a graphite crucible, wherein a buffer region is disposed between the crucible and a heating region, so as to effectively prevent high-temperature liquid in the crucible from splashing, and prevent the splashed high-temperature liquid from condensing and collecting in the heating region.
In order to achieve the purpose, the invention adopts the following technical scheme:
a graphite crucible comprising a crucible body and a crucible cover, the crucible body comprising a bottom portion and a side portion;
a supporting platform is arranged on the inner wall of the side part and used for horizontally placing the crucible cover;
a groove is arranged between the supporting platform and the inner wall;
the crucible cover comprises an air inlet and an air outlet.
According to the invention, the groove is arranged between the inner wall of the graphite crucible and the supporting platform, so that liquid in the graphite crucible is effectively prevented from splashing out during ventilation, the splashed liquid is prevented from entering the furnace chamber, and the normal heating is ensured. The supporting platform in the graphite crucible is positioned in the heating system, so that the joint surface of the crucible cover and the supporting platform in the graphite crucible is positioned in a high-temperature heating area, and the copper liquid at the joint position is prevented from being condensed and gathered.
When large-flow mixed gas is introduced into liquid copper, splashed copper liquid firstly passes through a gap between the supporting platform and the crucible cover to enter the annular groove, and a convex liquid surface is formed at the upper part of the groove due to the non-infiltration and surface tension effects of the copper and the graphite surface, so that the gap between the crucible cover and the supporting surface platform is sealed through the copper liquid, and then splashed copper liquid drops firstly enter the convex copper liquid, thereby playing a buffer role on the splashed copper liquid and avoiding the splashing of the copper liquid. Because the joint surface of the crucible cover and the supporting platform is positioned in the heating system and in the high-temperature heating area, the copper liquid is prevented from being condensed and gathered at the joint position.
The groove is an annular groove.
As one of the preferable technical solutions of the present invention, the shape of the body includes an inverted frustum shape.
Preferably, the inclination angle between the bottom of the body and the inner wall is 110-150 °, and may be, for example, 110 °, 120 °, 130 °, 140 °, 145 ° or 150 °, but is not limited to the recited values, and other values not recited within the numerical range are equally applicable.
Preferably, the inclination angle between the bottom of the body and the outer wall is 110-150 °, such as 110 °, 120 °, 130 °, 140 °, 145 ° or 150 °, but not limited to the recited values, and other values not recited within the numerical range are equally applicable.
As a second preferred technical solution of the present invention, the shape of the body comprises a cylindrical shape.
The cylindrical graphite crucible provided by the invention is changed into a cylinder from an inverted circular truncated cone shape under the condition of not increasing the maximum diameter of the graphite crucible, the diameter of the upper opening end of the crucible is the same as that of the bottom of the crucible, and the inner wall of the side part is vertical to the bottom, so that the space at the lower part of the graphite crucible can be increased. The phenomenon that the quality of the grown graphene is affected because the bubbles only rise from one side close to the crucible wall and then are quickly converged into large bubbles due to slight deviation between the disc-shaped bubble generator connected with the lower part of the air inlet pipe and the center of the bottom of the crucible is prevented; meanwhile, the phenomenon that bubbles rise from one side close to the crucible wall only because of the position deviation of the crucible wall and the bubble generator is avoided, so that a large amount of carbon is deposited on the inner wall of the side part close to the bubble generator.
Preferably, the distance between the support platform and the upper opening of the graphite crucible is 5-20cm, for example, 5cm, 6cm, 10cm, 15cm, 18cm or 20cm, but is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the external height of the body is 280-1000mm, and can be, for example, 280mm, 400mm, 600mm, 800mm or 1000mm, but is not limited to the recited values, and other values not recited within the numerical ranges are equally applicable.
The wall thickness of the body is 15 to 60mm, for example 15mm, 20mm, 30mm, 40mm, 50mm or 60mm, but is not limited to the values recited, and other values not recited within the numerical range are equally applicable.
The outer diameter of the bottom of the body is 80 to 700mm, and may be, for example, 80mm, 100mm, 330mm, 500mm, 600mm or 700mm, but is not limited to the values recited, and other values not recited in the numerical range are also applicable.
The outer diameter of the upper port end of the body is 95 to 750mm, and may be, for example, 95mm, 100mm, 300mm, 500mm, 600mm or 750mm, but is not limited to the values recited, and other values not recited in the range of values are also applicable.
Preferably, the cross-sectional shape of the groove includes any one of a square, a rectangle, a trapezoid, a circle, an ellipse, a cone, or a diamond.
Preferably, the width of the groove cross-section is 1-20mm, and may be, for example, 1mm, 2mm, 5mm, 10mm, 15mm, 18mm or 20mm, but is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The width of the cross section of the groove is the distance of the opening of the groove.
Preferably, the depth of the groove is 1-30mm, and may be, for example, 1mm, 2mm, 5mm, 10mm, 15mm, 18mm, 20mm, 25mm, 28mm or 30mm, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
When the graphite crucible provided by the invention is placed in a heating system for heating, the groove and the supporting platform are positioned in the heating system, wherein the supporting platform of the graphite crucible is 4-19cm lower than the upper surface of the heating system, for example, 4mm, 10mm, 15mm, 18mm or 19mm, but the invention is not limited to the recited values, and other values in the range of the recited values are also applicable.
Because the joint surface of the crucible cover and the supporting platform is positioned in the heating system and in the high-temperature heating area, the copper liquid is prevented from being condensed and gathered at the joint position.
Preferably, the width of the support platform is 2-50mm, for example 2mm, 5mm, 10mm, 15mm, 18mm, 20mm, 25mm, 28mm, 30mm, 35mm, 40mm, 45mm or 50mm, but not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the crucible cover is placed horizontally on the support platform, the distance between the crucible cover and the inner wall is 0.5-35mm, for example 0.5mm, 1mm, 5mm, 10mm, 15mm, 18mm, 20mm, 25mm, 28mm, 30mm or 35mm, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the thickness of the bottom is 10-100mm, for example 10mm, 15mm, 18mm, 30mm, 50mm, 60mm, 90mm or 100mm, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the thickness of the body at the upper end opening is from 5 to 60mm, and may be, for example, 5mm, 10mm, 15mm, 18mm, 30mm, 50mm, 55mm or 60mm, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the gas inlet hole is disposed at the middle position of the crucible cover.
Preferably, the diameter of the vent hole is 10-100mm, for example 10mm, 15mm, 18mm, 30mm, 50mm, 60mm, 90mm or 100mm, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the groove is arranged on the inner wall of the graphite crucible, and is positioned at the position where the supporting platform at the upper opening is connected with the inner wall, so that liquid can be effectively prevented from splashing into the furnace chamber when the graphite crucible is ventilated, and the supporting platform in the graphite crucible is positioned in the heating system, so that the joint surface of the crucible cover and the supporting platform in the graphite crucible is positioned in a high-temperature heating area, and the copper liquid is prevented from being condensed and gathered at the joint position.
(2) The cylindrical graphite crucible provided by the invention can increase the space at the lower part of the graphite crucible because the inner wall of the side part is vertical to the bottom part under the condition that the maximum diameter of the graphite crucible is not required to be increased. The phenomenon that the quality of the grown graphene is affected due to the fact that bubbles only rise from one side close to the crucible wall and then are quickly gathered into large bubbles due to slight deviation between the disc-shaped bubble generator connected to the lower portion of the air inlet pipe and the center of the bottom of the crucible; meanwhile, the phenomenon that bubbles rise from one side close to the crucible wall only because of the position deviation of the crucible wall and the bubble generator is avoided, so that a large amount of carbon is deposited on the inner wall of the side part close to the bubble generator.
Drawings
FIG. 1 is a schematic view showing the structure of an inverted circular truncated graphite crucible according to the present invention.
FIG. 2 is a schematic view of the structure of a cylindrical graphite crucible according to the present invention.
Fig. 3 is a schematic view of the structure of the graphite crucible provided in comparative example 1.
Wherein: 1-crucible body, 2-supporting platform, 3-groove, 4-crucible cover, 5-air inlet, 6-air outlet and 7-heating system.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Example 1
The present embodiment provides a graphite crucible (fig. 1) comprising a body 1 and a crucible cover 4, the body 1 including a bottom portion and a side portion; the graphite crucible is in an inverted circular truncated cone shape, the inclination angle between the bottom and the inner wall of the side part is 120 degrees, and the inclination angle between the bottom and the outer wall of the side part is 120 degrees; the external height of the crucible body 1 is 500mm, the wall thickness of the crucible body 1 is 30mm, the outer diameter of the bottom of the crucible body 1 is 300mm, and the outer diameter of the upper port end of the crucible body 1 is 350 mm; the thickness of the bottom is 50mm, and the thickness of the crucible body 1 at the opening of the upper end is 20 mm.
The inner wall is provided with a supporting platform 2, the supporting platform 2 is used for horizontally placing a crucible cover 4, the distance between the supporting platform 2 and the upper end opening of the graphite crucible is 10cm, and a groove 3 is arranged between the supporting platform 2 and the inner wall; the cross-sectional shape of recess 3 is the square, the width in 3 cross-sections of recess is 5mm, the degree of depth of recess 3 in the inner wall is 15mm, the width of supporting platform 2 is 7mm, crucible lid 4 level is placed on supporting platform 2, and the distance of crucible lid 4 and inner wall is 5 mm.
The crucible cover 4 includes an air inlet hole 5 and an air outlet hole 6. The air inlet 5 is arranged in the middle of the crucible cover 4; the diameter of the vent hole 6 is 20 mm.
When the graphite crucible is placed in the heating system 7 for heating, the groove 3 and the supporting platform 2 are positioned in the heating system 7. The support platform 2 of the graphite crucible is 10cm below the upper surface of the heating system 7.
The graphite crucible that this embodiment provided, through set up recess 3 on graphite crucible's inner wall, recess 3 is located the position that meets with the supporting platform 2 and the inner wall of upper port department, and liquid splashes to the furnace chamber in the time of can effectually preventing ventilating in graphite crucible, and supporting platform 2 in the graphite crucible is located heating system 7 inside for crucible cover 4 is in the high temperature zone of heating with the inside supporting platform 2 faying face of graphite crucible, has avoided the gathering that condenses at seam position copper liquid.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the distance between the molten liquid level and the supporting platform is 10cm, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the depth of the gas inlet pipeline bubble generator from the liquid copper liquid level is 8cm, the gas is ventilated and grown for 4h, the temperature is reduced to room temperature, no copper condensation and aggregation phenomenon exists at the joint of the supporting platform and the crucible cover in the crucible, and no copper particles splash in a furnace chamber.
Example 2
The present embodiment provides a graphite crucible (fig. 1) comprising a body 1 and a crucible cover 4, the body 1 comprising a body bottom portion and a side portion; the graphite crucible is in an inverted truncated cone shape, the inclination angle between the bottom and the inner wall of the side part is 110 degrees, and the inclination angle between the bottom and the outer wall of the side part is 110 degrees; the external height of the crucible body 1 is 1000mm, the wall thickness of the crucible body 1 is 60mm, the outer diameter of the bottom of the crucible body 1 is 700mm, and the outer diameter of the upper port end of the crucible body 1 is 750 mm; the thickness of the bottom is 60mm, and the thickness of the opening at the upper end of the crucible body 1 is 15 mm.
The inner wall is provided with a supporting platform 2, the supporting platform 2 is used for horizontally placing a crucible cover 4, the distance between the supporting platform 2 and an opening at the upper end of the graphite crucible is 200mm, and a groove 3 is arranged between the supporting platform 2 and the inner wall; the cross sectional shape of recess 3 is the rectangle, the width in 3 cross-sections of recess is 9mm, the degree of depth of recess 3 in the inner wall is 5mm, supporting platform 2's width is 35mm, crucible lid 4 level is placed on supporting platform 2, and the distance of crucible lid 4 and inner wall is 35 mm.
The crucible cover 4 includes an air inlet hole 5 and an air outlet hole 6. The air inlet 5 is arranged in the middle of the crucible cover 4; the diameter of the vent hole 6 is 190 mm.
When the graphite crucible is placed in the heating system 7 for heating, the groove 3 and the supporting platform 2 are positioned in the heating system 7. The supporting platform 2 of the graphite crucible is 4cm lower than the upper surface of the heating system 7.
The graphite crucible that this embodiment provided, through set up recess 3 on graphite crucible's inner wall, recess 3 is located the position that meets with the supporting platform 2 and the inner wall of upper port department, and liquid splashes to the furnace chamber in the time of can effectually preventing ventilating in graphite crucible, and supporting platform 2 in the graphite crucible is located heating system 7 inside for crucible cover 4 is in the high temperature zone of heating with the inside supporting platform 2 faying face of graphite crucible, has avoided the gathering that condenses at seam position copper liquid.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the distance between the molten liquid level and the supporting platform is 10cm, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the depth of the gas inlet pipeline bubble generator from the liquid copper liquid level is 8cm, the gas is ventilated and grown for 4h, the temperature is reduced to room temperature, no copper condensation and aggregation phenomenon exists at the joint of the supporting platform and the crucible cover in the crucible, and no copper particles splash in a furnace chamber.
Example 3
The present example provides a graphite crucible (fig. 1) comprising a body 1 and a crucible cover 4, the body 1 including a bottom portion and a side portion; the graphite crucible is in an inverted circular truncated cone shape, the inclination angle between the bottom and the inner wall of the side part is 150 degrees, and the inclination angle between the bottom and the outer wall of the side part is 150 degrees; the external height of the crucible body 1 is 280mm, the wall thickness of the crucible body 1 is 15mm, the outer diameter of the bottom of the crucible body 1 is 80mm, and the outer diameter of the upper port end of the crucible body 1 is 95 mm; the thickness of the bottom is 30mm, and the thickness of the opening at the upper end of the crucible body 1 is 17 mm.
The inner wall is provided with a supporting platform 2, the supporting platform 2 is used for horizontally placing a crucible cover 4, the distance between the supporting platform 2 and the opening at the upper end of the graphite crucible is 80mm, and a groove 3 is arranged between the supporting platform 2 and the inner wall; the cross-sectional shape of recess 3 is trapezoidal, the width in 3 cross-sections of recess is 2mm, the degree of depth of recess 3 in the inner wall is 30mm, the width of supporting platform 2 is 2mm, crucible lid 4 level is placed on supporting platform 2, and the distance of crucible lid 4 and inner wall is 1 mm.
The crucible cover 4 includes an air inlet hole 5 and an air outlet hole 6. The air inlet 5 is arranged in the middle of the crucible cover 4; the diameter of the exhaust hole 6 is 10 mm.
When the graphite crucible is placed in the heating system 7 for heating, the groove 3 and the supporting platform 2 are positioned in the heating system 7. The support platform 2 of the graphite crucible is 50mm below the upper surface of the heating system 7.
The graphite crucible that this embodiment provided, through set up recess 3 on graphite crucible's inner wall, recess 3 is located the position that meets with the supporting platform 2 and the inner wall of upper port department, and liquid splashes to the furnace chamber in the time of can effectually preventing ventilating in graphite crucible, and supporting platform 2 in the graphite crucible is located heating system 7 inside for crucible cover 4 is in the high temperature zone of heating with the inside supporting platform 2 faying face of graphite crucible, has avoided the gathering that condenses at seam position copper liquid.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the distance between the molten liquid level and the supporting platform is 10cm, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the depth of the gas inlet pipeline bubble generator from the liquid copper liquid level is 8cm, the gas is ventilated and grown for 4h, the temperature is reduced to room temperature, no copper condensation and aggregation phenomenon exists at the joint of the supporting platform and the crucible cover in the crucible, and no copper particles splash in a furnace chamber.
Example 4
The present embodiment provides a graphite crucible (fig. 2) comprising a body 1 and a crucible cover 4, the body 1 including a bottom portion and a side portion; the graphite crucible is cylindrical; the external height of the crucible body 1 is 500mm, the wall thickness of the crucible body 1 is 30mm, the outer diameter of the bottom of the crucible body 1 is 350mm, and the outer diameter of the upper port end of the crucible body 1 is 350 mm; the thickness of the bottom is 50mm, and the thickness of the crucible body 1 at the opening of the upper end is 20 mm.
The inner wall is provided with a supporting platform 2, the supporting platform 2 is used for horizontally placing a crucible cover 4, the distance between the supporting platform 4 and the opening at the upper end of the graphite crucible is 10cm, and a groove 3 is arranged between the supporting platform 2 and the inner wall; the cross-sectional shape of recess 3 is the square, the width in recess 3 cross-section is 5mm, the degree of depth of recess 3 in the inner wall is 5mm, the width of supporting platform 2 is 5mm, crucible lid 4 level is placed on supporting platform 2, and the distance of crucible lid 4 and inner wall is 10 mm.
The crucible cover 4 includes an air inlet hole 5 and an air outlet hole 6. The air inlet 5 is arranged in the middle of the crucible cover 4; the diameter of the vent hole 6 is 20 mm.
When the graphite crucible is placed in the heating system 7 for heating, the groove 3 and the supporting platform 2 are positioned in the heating system 7. The support platform 2 of the graphite crucible is 10cm below the upper surface of the heating system 7.
The graphite crucible that this embodiment provided, through set up recess 3 on graphite crucible's inner wall, recess 3 is located the position that meets with the supporting platform 2 and the inner wall of upper port department, and liquid splashes to the furnace chamber in the time of can effectually preventing ventilating in graphite crucible, and supporting platform 2 in the graphite crucible is located heating system 7 inside for crucible cover 4 is in the high temperature zone of heating with the inside supporting platform 2 faying face of graphite crucible, has avoided the gathering that condenses at seam position copper liquid. The cylindrical graphite crucible is used without increasing the maximum diameter of the graphite crucible. The space at the lower part of the graphite crucible can be increased because the inner wall of the side part is vertical to the bottom part. The phenomenon that the quality of the grown graphene is affected because the bubbles only rise from one side close to the crucible wall and then are quickly converged into large bubbles due to slight deviation between the disc-shaped bubble generator connected with the lower part of the air inlet pipe and the center of the bottom of the crucible is prevented; meanwhile, the phenomenon that bubbles rise from one side close to the crucible wall only because of the position deviation of the crucible wall and the bubble generator is avoided, so that a large amount of carbon is deposited on the inner wall of the side part close to the bubble generator.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the distance between the molten liquid level and the supporting platform is 10cm, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the depth of the gas inlet pipeline bubble generator from the liquid copper liquid level is 8cm, the gas is ventilated and grown for 4h, the temperature is reduced to room temperature, no copper condensation and aggregation phenomenon exists at the joint of the supporting platform and the crucible cover in the crucible, and no copper particles splash in a furnace chamber.
Example 5
This example provides a graphite crucible (FIG. 1) which is the same as example 4 except that the gas inlet hole 5 is not disposed at the center of the crucible cover 4, but is disposed on the opposite side of the crucible cover 4 from the gas outlet hole 6.
Although the air inlet hole is not positioned in the center of the crucible cover, the disc-shaped bubble generator connected with the lower part of the air inlet pipe is necessarily deviated from the center of the crucible, the space at the lower part of the graphite crucible is increased because the inner wall of the side part of the crucible is vertical to the bottom, and the problem that the quality of the grown graphene is influenced because bubbles rise from one side close to the crucible wall and then are quickly converged into large bubbles is solved; and meanwhile, a large amount of carbon is not deposited on the inner wall of the side part close to the side close to the bubble generator.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the distance between the molten liquid level and the supporting platform is 10cm, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the depth of the gas inlet pipeline bubble generator from the liquid copper liquid level is 8cm, the gas is ventilated and grown for 4h, the temperature is reduced to room temperature, no copper condensation and aggregation phenomenon exists at the joint of the supporting platform and the crucible cover in the crucible, and no copper particles splash in a furnace chamber.
Comparative example 1
This comparative example provides a conventional graphite crucible (fig. 3) comprising a body 1 and a crucible cover 4, the body 1 comprising a body bottom and side portions; the inclination angle between the bottom and the inner wall is 120 degrees, and the inclination angle between the bottom and the outer wall is 120 degrees; the thickness of bottom is 50mm, the thickness of inner wall at the upper end opening is 20 mm.
Be provided with supporting platform 2 on the inner wall, supporting platform 2 is used for the level to place crucible cover 4, supporting platform 2 is 20mm with graphite crucible upper end open-ended distance, no recess 3 on the inner wall. The width of the supporting platform 2 is 10mm, the crucible cover 4 is horizontally placed on the supporting platform 2, and the distance between the crucible cover 4 and the inner wall is 2 mm.
The crucible cover 4 includes an air inlet hole 5 and an air outlet hole 6. The air inlet 5 is a through hole and is arranged in the middle of the crucible cover 4; the exhaust hole 6 is a through hole, and the diameter of the exhaust hole 6 is 20 mm.
When the graphite crucible is placed in the heating system 7 for heating, the supporting platform 2 is positioned outside the heating system 7.
According to the graphite crucible provided by the comparative example, when the graphite crucible is heated, the internal liquid is easy to splash and enter a heating system, so that equipment is influenced, and the efficiency is reduced.
By utilizing the graphite crucible and the crucible cover, copper is added, heating is carried out under the protection of nitrogen, so that the copper is in a molten state, the liquid level is 10cm away from the supporting platform after melting, mixed gas with the flow of methane and nitrogen being 5/25L is introduced at the growth temperature of 1250 ℃ under normal pressure, the air inlet pipeline bubble generator is 8cm away from the liquid level of the liquid copper, the air inlet pipeline bubble generator is ventilated and grown for 4h, the temperature is reduced to room temperature, a large amount of copper is condensed and accumulated at the joint of the supporting platform and the crucible cover in the crucible through observation, the mass is 630g, and a great amount of copper particles which are splashed out and solidified are also exist in the furnace chamber, and the mass is 750 g.
Therefore, the graphite crucible can avoid the phenomenon of copper liquid drops condensing and gathering at the joint of the supporting platform in the crucible and the crucible cover, and meanwhile, the copper liquid drops can not splash into the furnace chamber.
The present invention is described in detail with reference to the above embodiments, but the present invention is not limited to the above detailed structural features, that is, the present invention is not meant to be implemented only by relying on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A graphite crucible, characterized in that the graphite crucible comprises a body and a crucible cover, the body comprising a bottom portion and a side portion;
a supporting platform is arranged on the inner wall of the side part and used for horizontally placing the crucible cover;
a groove is arranged between the supporting platform and the inner wall;
the crucible cover comprises an air inlet and an air outlet.
2. The graphite crucible of claim 1, wherein the shape of the body comprises an inverted frustum shape;
preferably, the inclination angle between the inner walls of the bottom and side portions is 110-;
preferably, the angle of inclination between the outer walls of the bottom and side portions is 110-.
3. The graphite crucible of claim 1, wherein the body comprises a cylindrical shape.
4. The graphite crucible as claimed in any one of claims 1 to 3, wherein the distance between the support platform and the upper end opening of the graphite crucible is 5 to 20 cm;
preferably, the external height of the crucible body is 280-1000 mm;
preferably, the wall thickness of the crucible body is 15-60 mm;
preferably, the external diameter of the bottom of the crucible body is 80-700 mm;
preferably, the outer diameter of the upper opening end of the crucible body is 95-750 mm.
5. The graphite crucible as claimed in any one of claims 1 to 4, wherein the cross-sectional shape of the groove comprises any one of a square, a rectangle, a trapezoid, a circle, an ellipse, a cone or a rhombus.
6. The graphite crucible as claimed in any one of claims 1 to 5, wherein the groove has a cross section with a width of 1 to 20mm and a depth of 1 to 30 mm.
7. The graphite crucible as claimed in any one of claims 1 to 6, wherein the width of the support platform is 2 to 50 mm.
8. The graphite crucible as claimed in any one of claims 1 to 7, wherein the crucible cover is horizontally placed on the support platform, and the distance between the crucible cover and the inner wall of the side part is 0.5 to 35 mm.
9. The graphite crucible as claimed in any one of claims 1 to 8, wherein the bottom has a thickness of 10 to 100 mm;
preferably, the thickness of the crucible body at the opening is 5 to 60 mm.
10. The graphite crucible as claimed in any one of claims 1 to 9, wherein the gas inlet hole is disposed at a middle position of the crucible cover;
preferably, the diameter of the vent hole is 10-100 mm.
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| CN202210218548.8A CN114436249A (en) | 2022-03-04 | 2022-03-04 | Graphite crucible |
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| CN202210218548.8A CN114436249A (en) | 2022-03-04 | 2022-03-04 | Graphite crucible |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071398A (en) * | 2009-11-20 | 2011-05-25 | 上海广电电子股份有限公司 | Metal evaporation crucible |
| CN103387416A (en) * | 2013-07-31 | 2013-11-13 | 青岛隆盛晶硅科技有限公司 | Method for prolonging service life of graphite crucible in medium smelting |
| CN209655801U (en) * | 2019-01-22 | 2019-11-19 | 吉林科工碳业有限公司 | Graphite crucible is used in a kind of purification of cathode of lithium battery |
| CN214422782U (en) * | 2021-03-12 | 2021-10-19 | 哈尔滨晶彩材料科技有限公司 | Protection type abnormal shape graphite crucible |
| CN217600381U (en) * | 2022-03-04 | 2022-10-18 | 常州二维碳素科技股份有限公司 | Graphite crucible |
-
2022
- 2022-03-04 CN CN202210218548.8A patent/CN114436249A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071398A (en) * | 2009-11-20 | 2011-05-25 | 上海广电电子股份有限公司 | Metal evaporation crucible |
| CN103387416A (en) * | 2013-07-31 | 2013-11-13 | 青岛隆盛晶硅科技有限公司 | Method for prolonging service life of graphite crucible in medium smelting |
| CN209655801U (en) * | 2019-01-22 | 2019-11-19 | 吉林科工碳业有限公司 | Graphite crucible is used in a kind of purification of cathode of lithium battery |
| CN214422782U (en) * | 2021-03-12 | 2021-10-19 | 哈尔滨晶彩材料科技有限公司 | Protection type abnormal shape graphite crucible |
| CN217600381U (en) * | 2022-03-04 | 2022-10-18 | 常州二维碳素科技股份有限公司 | Graphite crucible |
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