CN107190322B - A kind of growing method of the adjustable silicon carbide polycrystalline ceramics of large scale resistivity - Google Patents
A kind of growing method of the adjustable silicon carbide polycrystalline ceramics of large scale resistivity Download PDFInfo
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- CN107190322B CN107190322B CN201710213529.5A CN201710213529A CN107190322B CN 107190322 B CN107190322 B CN 107190322B CN 201710213529 A CN201710213529 A CN 201710213529A CN 107190322 B CN107190322 B CN 107190322B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
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Abstract
The present invention relates to a kind of growing methods of the adjustable silicon carbide polycrystalline ceramics of large scale resistivity, sic raw material is held using graphite crucible, wherein graphite crucible is made of graphite crucible top cover and graphite crucible body, carbon film layer is provided on the graphite crucible inner surface, sic raw material is placed in graphite crucible body, cover the graphite crucible top cover, it is put into growth furnace, and the bottom of the graphite crucible body and/or lower part is set to be located at heating zone so that the temperature of the bottom of graphite crucible body is higher than the temperature of graphite crucible top cover, silicon carbide polycrystalline ceramic is grown in the carbon film layer surface using physical vapor transport method or high temperature chemical vapor deposition method.Growing method of the present invention is simple, and the silicon carbide polycrystalline ceramics is more more excellent than Conventional silicon carbide ceramic performance, and uniformity is good, and consistency is more preferable, and purity is higher, and thermal conductivity is more preferable.
Description
Technical field
The invention belongs to carbofrax material fields, and in particular to one kind is based on physical vapor transport growth carbonization policrystalline silicon
The method of ceramics.
Background technique
Silicon carbide (SiC) material mainly includes monocrystalline and ceramic 2 major class.Single-crystal silicon carbide big, thermal conductivity with forbidden bandwidth
Rate is high, electronics saturation drift velocity is big, critical breakdown electric field is high, dielectric constant is low, good chemical stability, high frequency,
High-power, high temperature resistant, Flouride-resistani acid phesphatase semiconductor devices and ultraviolet detector and short-wave LED etc., which have, widely answers
With prospect, device made of it can use in 600 DEG C or more of hot environment.Silicon carbide ceramics has elevated temperature strength big,
Inoxidizability is strong, and wear resistance is good, and thermal stability is good, and thermal expansion coefficient is small, and thermal conductivity is big, and hardness is high and anti-thermal shock and resistance to
The characteristics such as chemical attack, thus its aerospace, nuclear energy, national defence, military project and in terms of have a extensive future.At the same time,
Special applying working condition is also to the shape complexity of silicon carbide ceramic product, compactness, intensity, purity, thermal conductivity and reliability
More stringent requirements are proposed.
The problem of consistency, purity and thermal conductivity existing for Conventional silicon carbide ceramics etc. limit its broader applications at present,
And single-crystal silicon carbide is although have excellent performance and prepare comparative maturity, it is expensive, is also difficult to be widely used at present general
Field.The performances such as SiC monocrystal thermal conductivity are more preferable than SiC ceramic performance, but the cost of manufacture of high quality single crystal silicon carbide is high,
Complex process, this is very restricted the application of monocrystalline silicon carbide.In contrast, the preparation of polycrystal carborundum ceramics
At low cost, technique is also relatively simple, but its consistency, purity and resistivity are difficult to meet existing demand.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of replaceable Conventional silicon carbide ceramics and performance and monocrystalline
The growing method of equally excellent silicon carbide polycrystalline ceramic.
On the one hand, the present invention provides a kind of growing method of the adjustable silicon carbide polycrystalline ceramics of large scale resistivity,
Middle graphite crucible is made of graphite crucible top cover and graphite crucible body, is provided with carbon film layer on the graphite crucible inner surface, will
Sic raw material is placed in graphite crucible body, is covered the graphite crucible top cover, is put into growth furnace, and makes the graphite earthenware
The bottom and/or lower part of crucible body are located at heating zone so that the temperature of the bottom of graphite crucible body is higher than the temperature of graphite crucible top cover
Degree grows carbonization policrystalline silicon in the carbon film layer surface using physical vapor transport method or high temperature chemical vapor deposition method
Ceramic material.
There are certain thickness carbon film layers between silicon carbide polycrystalline ceramics and graphite crucible top cover in the present invention, not only substantially
Reducing thermal stress caused by directly contacting due to polycrystalline with graphite cover avoids polycrystalline from cracking, but also protects polycrystalline and stone
The adhesion of inky cap destroys, and greatly improves silicon carbide polycrystalline quality and yield.
Preferably, the carbon film layer with a thickness of 0.01~1 millimeter, preferably 10~100 microns.The thickness of the carbon film layer
When spending within this range, it is ensured that single side is grown when silicon carbide polycrystalline growth crystallizes, and inhibits multiple spot nucleation, guarantees to prepare more
Brilliant fault in material is few, uniformity, and also avoidable polycrystalline is directly contacted with graphite cover leads to stress excessive the problem of cracking.
Preferably, the carbon film that the inner surface of the crucible top cover is grown can be splashed by chemical vapor deposition, thermal evaporation, magnetic control
It penetrates, uniformly plate hot setting, plasma spraying, molecular beam epitaxy, liquid phase epitaxy or laser deposition legal system after graphite glue or carbohydrate gum
It is standby to obtain.
Preferably, growth pressure is 2~50Torr, growth temperature 1900 in silicon carbide polycrystalline ceramics growth course
~2300 DEG C, be 20 hours or more, preferably 50~150 hours according to different growth rate growth times.
Preferably, growth atmosphere is in argon gas, nitrogen, helium and hydrogen in silicon carbide polycrystalline ceramics growth course
It is at least one.
Preferably, the purity of the sic raw material is not less than 99.8%；Or in the sic raw material doped with vanadium,
At least one of aluminium and nitrogen, doping are 0.1~5wt%.
Preferably, the temperature gradient from graphite crucible top cover to the bottom of graphite crucible body is 1 DEG C/cm~5 DEG C/cm, it is excellent
Select 1.5 DEG C/cm~3 DEG C/cm.
On the other hand, the present invention also provides a kind of silicon carbide polycrystalline ceramic grown according to above-mentioned method, institutes
The boundary dimensions (diameter) of silicon carbide polycrystalline ceramic is stated at 4 inches or more, preferably 4~8 inches.
This is preferably, the silicon carbide polycrystalline ceramic includes conductive silicon carbide polycrystalline ceramic and semi-insulating type
Silicon carbide polycrystalline ceramic, wherein the resistivity of the conductive silicon carbide polycrystalline ceramic 0.015 Ω cm~
0.03 Ω cm range, the resistivity > 10 of the semi-insulating type silicon carbide polycrystalline ceramic5Ω·cm。
Growing method of the present invention is simple, and the silicon carbide polycrystalline ceramics is more more excellent than Conventional silicon carbide ceramic performance,
Even property is good, and consistency is more preferable, and purity is higher, and thermal conductivity is more preferable, adjustable by semi-insulating and conductiving doping resistivity, and passes through
It helps at low cost, can be processed composition element of different shapes, realize the broader applications of silicon carbide polycrystalline ceramics.
Detailed description of the invention
Fig. 1 is growth room's structural schematic diagram of physical vapor transport (PVT) method growth SiC polycrystalline ceramics；
Fig. 2 is that embodiment 1 uses physical vapor transport (PVT) method in growth pressure for 20Torr, growth temperature 2080
DEG C and 4 inches of SiC polycrystalline crystal ingots being grown under the conditions of growth time 100 hours；
Fig. 3 is 4 inches of polycrystalline ceramics pieces of the corresponding cutting of SiC polycrystalline crystal ingot prepared using embodiment 1；
Fig. 4 is that embodiment 2 uses physical vapor transport (PVT) method in growth pressure for 10Torr, growth temperature 2120
DEG C and 5 inches of SiC polycrystalline crystal ingots being grown under the conditions of growth time 100 hours；
Fig. 5 is the polycrystalline ceramics piece of the corresponding cutting of 5 inches of SiC polycrystalline crystal ingots prepared using embodiment 2；
Fig. 6 is embodiment 2 using physical vapor transport (PVT) method and using 5 English of the graphite cover growth for being coated with carbon film layer
The back photo of very little SiC polycrystalline crystal ingot；
Fig. 7 is comparative example 1 using physical vapor transport (PVT) method and not using the 5 of the graphite cover growth for being coated with carbon film layer
The back photo of inch SiC polycrystalline crystal ingot；
Appended drawing reference:
1, graphite crucible top cover；
2, graphite crucible body；
3, SiC raw material；
4, carbon film layer；
5, SiC polycrystalline ceramics.
Specific embodiment
The present invention is further illustrated below by way of following drawings and embodiments, it should be appreciated that following embodiments are only used for
Illustrate the present invention, is not intended to limit the present invention.
The present invention provides a kind of growers of physical vapor transport (PVT) method growth SiC polycrystalline ceramics.Described device
By crucible body, crucible top cover and the carbon film layer of crucible top cover inner surface is set forms.The thickness of the carbon film layer can be
0.01~1 millimeter, preferably 10~100 microns.The material of the crucible can be graphite.By taking graphite crucible as an example, such as Fig. 1 institute
Show, wherein carbon film layer 4 is set to the inner surface of graphite crucible top cover 1.Carbon film layer can also be coated in crucible body on surface.
Illustrate to following exemplary the growth side of high-purity carborundum polycrystalline ceramics provided by the invention (SiC polycrystalline material)
Method.
Sic raw material is placed in graphite crucible body high-temperature region, the graphite crucible top cover that growth inner surface is coated with carbon film is set
It is heavy on the carbon film surface of graphite cover using physical vapor transport (PVT) method or high temperature chemical vapor deposition method in low-temperature space
Product growth silicon carbide polycrystalline ceramics.Specifically, when work, graphite crucible top cover 1 is placed on bottom and is placed with sic raw material 3
Graphite crucible body 2 on, be integrally put into crystal growing furnace, the bottom of graphite crucible body and/or lower part made to be located at heating zone, with
The raising of temperature, sic raw material 3 gradually distil, be located at low-temperature space carbon film layer 4 on grow into silicon carbide polycrystalline ceramics
5.Due to, there are certain thickness carbon film layer 4, not only being significantly reduced due to polycrystalline between silicon carbide polycrystalline ceramics and graphite cover
Thermal stress caused by directly contacting with graphite cover avoids polycrystalline from cracking, but also the adhesion of polycrystalline and graphite cover is protected to destroy,
Greatly improve silicon carbide polycrystalline quality and yield.
In silicon carbide polycrystalline ceramic growth course, growth pressure can be 2~50Torr, and growth temperature can be 1900
~2300 DEG C.Different growth pressures and growth temperature are selected, the growth rate of silicon carbide polycrystalline ceramic is different.According to not
Same growth rate, growth time are controlled at 20 hours or more, and preferably 50~150 hours.It was grown in silicon carbide polycrystalline ceramics
Cheng Zhong, growth atmosphere can be at least one of argon gas, nitrogen, helium and hydrogen.
As an example, the present invention, which is used, prepares carbon based on physical vapor transport (PVT) method for preparing single-crystal silicon carbide
Sic raw material is placed in graphite crucible high-temperature region first by SiClx polycrystalline ceramic, and growth inner surface is then coated with carbon film
Graphite be placed on low-temperature space, finally growth pressure be 2~50Torr, growth temperature be 1900~2300 DEG C under conditions of
(temperature gradient from graphite crucible top cover to the bottom of graphite crucible body is 1 DEG C/cm~5 DEG C/cm, preferably 1.5 DEG C/cm~3
DEG C/cm) in the carbon film surface deposition growing silicon carbide polycrystalline ceramics of graphite cover.
Carbon film layer 4 in the present invention is preferentially prepared by chemical vapour deposition technique.Furthermore the carbon film layer 4 can be with
By high after thermal evaporation, physical vapour deposition (PVD), magnetron sputtering, electron beam evaporation, reaction-sintered, uniformly plating graphite glue or carbohydrate gum
Temperature solidify, plasma coating, molecular beam epitaxy, liquid phase epitaxy, laser deposition etc. deposit and extension is in crucible top cover
On inner surface.These methods are all well known technologies in film field, and details are not described herein.
The compact film for being set to crucible top cover inner surface is extremely stable at a temperature of SiC polycrystalline growth, the thickness of film layer
Degree can be 0.01~1mm, preferably 10~100 μm, not only guarantee preparation polycrystalline material uniformity, also can avoid polycrystalline with
Graphite cover, which directly contacts, leads to stress excessive the problem of cracking.
Further, the silicon carbide polycrystalline ceramics, resistivity can by raw material carry out purification or doping way into
Row is adjusted.The purity of the sic raw material is not less than 99.8%.Or doped with vanadium, aluminium and nitrogen in the sic raw material
At least one of, doping can be 0.1~5wt%.It is more that by different element dopings conductive silicon carbide can be obtained in the present invention
Brilliant ceramic material (for example, nitrating element etc.) and semi-insulating type silicon carbide polycrystalline ceramic (for example, non-impurity-doped or doping vanadium,
Aluminium element etc.).Wherein the resistivity of the conductive silicon carbide polycrystalline ceramic is in 0.015 Ω of Ω cm~0.03 cm
Range, the resistivity > 10 of the semi-insulating type silicon carbide polycrystalline ceramic5Ω·cm。
High-purity carborundum polycrystalline ceramics growing method of the present invention comprises the step of: sic raw material is placed in graphite earthenware
The graphite for being coated with carbon film is placed on low-temperature space by crucible high-temperature region, using physical vapor transport method on the carbon film surface of graphite cover
Deposition growing silicon carbide polycrystalline ceramics.Wherein the thickness of silicon carbide polycrystalline ceramic and performance can be grown by growth temperature
Pressure, growth time are adjusted with the growth parameter(s)s such as, growth atmosphere component and raw material doping.The silicon carbide polycrystalline ceramics ratio
Conventional silicon carbide ceramic performance is more excellent, and uniformity is more preferable, and consistency is higher, and purity is higher, and thermal conductivity is more preferable, resistivity
Adjustable and economic cost is low.
The present invention prepares silicon carbide polycrystalline ceramic using physical vapor transport (PVT) method.Using laser conductometer
Measure the thermal conductivity of prepared silicon carbide polycrystalline ceramics.Prepared carbonization policrystalline silicon pottery is measured using Hall effect test equipment
The resistivity of porcelain.The purity of prepared silicon carbide polycrystalline ceramics is measured using ion microprobe.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. be also only an example in OK range, i.e. those skilled in the art can be done by the explanation of this paper
Selection in suitable range, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Top is coated with to the graphite cover (graphite crucible top cover) of carbon film layer first, bottom material area is (pure equipped with sic raw material
The graphite crucible of degree 99.9%) is placed in heat preservation carbon felt, is placed into crystal growth furnace chamber and (sic raw material is placed in graphite
The graphite crucible top cover that growth inner surface is coated with carbon film is placed in low-temperature space, from graphite crucible top cover to stone by crucible body high-temperature region
The temperature gradient of the bottom of black crucible body is 2 DEG C/cm.), vacuum degree is evacuated to 1.0 × 10-2Pa hereinafter, applying argon gas to growth pressure
20Torr, while nitrogen flow is 1sccm in growth course, is started to warm up to 2080 DEG C of growth temperature, after growing 100h, journey
For sequence cooling down to room temperature, blow-on obtains the silicon carbide polycrystalline ceramic with a thickness of 15mm (such as Fig. 2 institute on graphite cover
Show), silicon carbide polycrystalline ceramics piece (as shown in Figure 3) is obtained finally by machining, thickness 1mm, diameter 100mm),
4 inch silicon carbide polycrystalline materials can effectively be prepared using this patent method known to from Fig. 2 and Fig. 3, measuring its resistivity is
0.02Ω·cm.Fig. 3 is the polarisation photo for the SiC polycrystalline ceramics piece that physical vapor transport (PVT) method is grown in embodiment 1, from
Polycrystalline material uniformity known in Fig. 3.Wherein the thickness of silicon carbide polycrystalline ceramic and performance can by growth temperature,
Growth pressure, growth time are adjusted with the growth parameter(s)s such as, growth atmosphere component and raw material doping.
Embodiment 2
Top is coated with to the graphite cover of carbon film layer first, bottom material area is equipped with the graphite of sic raw material (purity 99.9%)
Crucible is placed in heat preservation carbon felt, place into crystal growth furnace chamber (sic raw material is placed in graphite crucible body high-temperature region, it will
The graphite crucible top cover that growth inner surface is coated with carbon film is placed in low-temperature space, from graphite crucible top cover to the bottom of graphite crucible body
Temperature gradient be 2.5 DEG C/cm), vacuum degree is evacuated to 1.0 × 10-2Pa is hereinafter, applying argon gas starts to rise to growth pressure 10Torr
Temperature to 2120 DEG C of growth temperature, grow 100h after, program cooling down to room temperature, blow-on obtained on graphite cover with a thickness of
The silicon carbide polycrystalline ceramic (as shown in Figure 4) of 20mm obtains silicon carbide polycrystalline ceramics piece (such as finally by machining
Shown in Fig. 5), thickness 1mm, diameter 125mm can effectively prepare 5 inches using this patent method known to from Fig. 4 and Fig. 5
Silicon carbide polycrystalline material, measuring its resistivity is 1.5 × 106Ω·cm.The wherein thickness of silicon carbide polycrystalline ceramic and property
Can be by growth temperature, growth pressure, growth time the growth parameter(s)s such as adulterate with, growth atmosphere component and raw material and are adjusted
Section.
Embodiment 3
Top is coated with to the graphite cover of carbon film layer first, bottom material area is equipped with the stone of sic raw material (purity 99.99%)
Black crucible is placed in heat preservation carbon felt, place into crystal growth furnace chamber (sic raw material is placed in graphite crucible body high-temperature region,
The graphite crucible top cover that growth inner surface is coated with carbon film is placed in low-temperature space, from graphite crucible top cover to the bottom of graphite crucible body
The temperature gradient in portion is 1.5 DEG C/cm), vacuum degree is evacuated to 1.0 × 10-2Pa is hereinafter, applying argon gas starts to growth pressure 10Torr
Be warming up to 2120 DEG C of growth temperature, after growing 100h, program cooling down to room temperature, blow-on obtained on graphite cover with a thickness of
The silicon carbide polycrystalline ceramic of 20mm, obtaining silicon carbide polycrystalline ceramics piece finally by machining, (thickness 1mm, diameter are
125mm), measuring its resistivity is 8.2 × 106Ω·cm。
Embodiment 4
Top is coated with to the graphite cover of carbon film layer first, bottom material area is equipped with sic raw material (purity 99.99%, doping
Have vanadium, content 0.5wt%) graphite crucible be placed in heat preservation carbon felt, place into crystal growth furnace chamber (by silicon carbide original
Material is placed in graphite crucible body high-temperature region, the graphite crucible top cover that growth inner surface is coated with carbon film is placed in low-temperature space, from graphite earthenware
The temperature gradient of crucible top cover to the bottom of graphite crucible body is 2.0 DEG C/cm), vacuum degree is evacuated to 1.0 × 10-2Pa is hereinafter, argon filling
Gas is started to warm up to 2120 DEG C of growth temperature, after growing 100h, program cooling down to room temperature is opened to growth pressure 10Torr
It is more to obtain silicon carbide finally by machining for the silicon carbide polycrystalline ceramic that furnace is obtained on graphite cover with a thickness of 20mm
Brilliant potsherd (thickness 1mm, diameter 125mm), measuring its resistivity is 2.4 × 105Ω·cm。
Comparative example 1
In order to carry out Experimental comparison, it is more that silicon carbide is carried out on the graphite cover that inner surface is not coated with carbon film layer using PVT method
Crystal ingot growth, growthing process parameter remove silicon carbide polycrystalline ingot from graphite cover after growth, as shown in Figure 7 with embodiment 2
It can clearly be seen that firm adhesion occurs for silicon carbide polycrystalline ingot back and graphite cover, when removing, silicon carbide polycrystalline ingot is destroyed
To the problem of cracking occur.Fig. 6 is then silicon carbide polycrystalline ingot of the embodiment 2 using the graphite cover growth for being coated with carbon film layer, can
See its back uniformity, is not destroyed.By comparative example, it can illustrate the graphite interior surface plating carbon that this patent is invented
Coating growth silicon carbide polycrystalline ingot can be released effectively silicon carbide polycrystalline ingot internal stress, and polycrystalline ingot is avoided to crack, and improve SiC crystal
Quality yield.
Table 1 is the performance data of silicon carbide polycrystalline ceramic prepared by the present invention；
It is noted that only the present invention is described in detail for above-mentioned specific embodiment, it should not be to the present invention
Limitation.It for a person skilled in the art, can be there are many shape when without departing from the objective and range of claim
The variation of formula and details.
Claims (6)
1. a kind of growing method of the adjustable silicon carbide polycrystalline ceramic of large scale resistivity, which is characterized in that use graphite
Crucible holds sic raw material, and wherein graphite crucible is made of graphite crucible top cover and graphite crucible body, the graphite crucible top
It is provided with carbon film layer on interior surface, sic raw material is placed in graphite crucible body, covers the graphite crucible top cover, is put into
In growth furnace, and so that the bottom of the graphite crucible body and/or lower part is located at heating zone so that the bottom of graphite crucible body temperature
Degree is higher than the temperature of graphite crucible top cover, using physical vapor transport method or high temperature chemical vapor deposition method in the carbon film
Layer surface grows silicon carbide polycrystalline ceramic；
Wherein, the carbon film layer with a thickness of 0.01~1 millimeter, in silicon carbide polycrystalline ceramics growth course, growth atmosphere pressure
It is by force 2~50Torr, growth temperature is 1900~2300 DEG C, and growth time is 20 hours or more, from graphite crucible top cover to stone
The temperature gradient of the bottom of black crucible body is 1 DEG C/cm~5 DEG C/cm.
2. growing method according to claim 1, which is characterized in that the carbon film layer with a thickness of 10~100 microns.
3. growing method according to claim 1, which is characterized in that the growth time is 50~150 hours.
4. growing method according to claim 3, which is characterized in that in silicon carbide polycrystalline ceramics growth course, growth
Atmosphere is at least one of argon gas, nitrogen, helium and hydrogen.
5. growing method according to claim 1, which is characterized in that the purity of the sic raw material be not less than
99.8%；Or doped at least one of vanadium, aluminium and nitrogen in the sic raw material, doping is 0.1~5wt%.
6. growing method according to any one of claims 1-5, which is characterized in that from graphite crucible top cover to graphite earthenware
The temperature gradient of the bottom of crucible body is 1.5 DEG C/cm~3 DEG C/cm.
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| CN108048911A (en) * | 2017-12-20 | 2018-05-18 | 中国科学院上海硅酸盐研究所 | A kind of method using physical gas phase deposition technology growing large-size carborundum crystals |
| CN110331438B (en) * | 2019-07-30 | 2021-07-13 | 河北普兴电子科技股份有限公司 | Method for inhibiting defect generation of carbon inclusion in growth of conductive silicon carbide crystal |
| CN114395799A (en) * | 2022-01-29 | 2022-04-26 | 北京青禾晶元半导体科技有限责任公司 | Device and method for simultaneously manufacturing silicon carbide single crystal and silicon carbide polycrystal |
| CN114481325A (en) * | 2022-01-29 | 2022-05-13 | 北京青禾晶元半导体科技有限责任公司 | Device and method for manufacturing silicon carbide polycrystal |
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