CN107190322A - A kind of growing method of the adjustable carborundum polycrystalline ceramics of large scale resistivity - Google Patents
A kind of growing method of the adjustable carborundum polycrystalline ceramics of large scale resistivity Download PDFInfo
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- CN107190322A CN107190322A CN201710213529.5A CN201710213529A CN107190322A CN 107190322 A CN107190322 A CN 107190322A CN 201710213529 A CN201710213529 A CN 201710213529A CN 107190322 A CN107190322 A CN 107190322A
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- graphite crucible
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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
Abstract
The present invention relates to a kind of growing method of the adjustable carborundum polycrystalline ceramics of large scale resistivity, sic raw material is held using graphite crucible, wherein graphite crucible is made up of graphite crucible top cover and graphite crucible body, carbon film layer is provided with 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 and/or bottom of the graphite crucible body is 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, using physical vapor transport method or high temperature chemical vapor deposition method in the carbon film layer superficial growth carborundum polycrystalline ceramic.Growing method of the present invention is simple, and the carborundum polycrystalline ceramics is more excellent than Conventional silicon carbide ceramic performance, and its uniformity is good, and more preferably, purity is higher, and thermal conductivity is more preferable for consistency.
Description
Technical field
The invention belongs to carbofrax material field, and in particular to one kind is based on physical vapor transport growth carbonization policrystalline silicon
The method of ceramics.
Background technology
Carborundum (SiC) material mainly includes monocrystalline and ceramic 2 major class.Single-crystal silicon carbide has that energy gap is big, thermal conductivity
Rate is high, electronics saturation drift velocity is big, critical breakdown electric field is high, dielectric constant is low, good chemical stability, high frequency,
Have in terms of high-power, high temperature resistant, Flouride-resistani acid phesphatase semiconductor devices and ultraviolet detector and short-wave LED and widely should
With prospect, the device being made of it can be used in more than 600 DEG C hot environments.Silicon carbide ceramics has elevated temperature strength big,
Inoxidizability is strong, and wear resistance is good, and heat endurance is good, and thermal coefficient of expansion 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 Aero-Space, nuclear energy, national defence, military project and it is civilian 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
Propose higher requirement.
The problem of consistency, purity and thermal conductivity that current Conventional silicon carbide ceramics are present etc. limits its broader applications,
Although and single-crystal silicon carbide excellent performance and prepare comparative maturity, its 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 carborundum is high,
Complex process, this causes the application of monocrystalline silicon carbide to be very restricted.By contrast, the preparation of polycrystal carborundum ceramics
Cost is low, and technique is also relatively simple, but its consistency, purity and resistivity are difficult to meet existing demand.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of replaceable Conventional silicon carbide ceramics and performance and monocrystalline
The growing method of equally excellent carborundum polycrystalline ceramic.
On the one hand, the invention provides a kind of growing method of the adjustable carborundum polycrystalline ceramics of large scale resistivity, its
Middle graphite crucible is made up of graphite crucible top cover and graphite crucible body, and carbon film layer is provided with 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 bottom 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, using physical vapor transport method or high temperature chemical vapor deposition method in carbon film layer superficial growth carbonization policrystalline silicon
Ceramic material.
There is certain thickness carbon film layer in the present invention between carborundum polycrystalline ceramics and graphite crucible top cover, not only significantly
Reducing the thermal stress caused by polycrystalline is directly contacted with graphite cover avoids polycrystalline from ftractureing, but also protects polycrystalline and stone
The adhesion destruction of inky cap, drastically increases carborundum polycrystalline quality and yield.
It is preferred that the thickness of the carbon film layer is 0.01~1 millimeter, preferably 10~100 microns.The thickness of the carbon film layer
Degree within this range when, it is ensured that carborundum polycrystalline growth crystallize when one side grow, suppress multiple spot nucleation, it is ensured that preparation it is many
Brilliant fault in material is few, uniformity, and can also avoid polycrystalline from directly being contacted with graphite cover causes the problem of stress is excessive cracking.
It is preferred that the carbon film of the inner surface growth of the crucible top cover can be splashed by chemical vapor deposition, thermal evaporation, magnetic control
Penetrate, 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.
It is preferred that in carborundum polycrystalline ceramics growth course, growth pressure is 2~50Torr, and growth temperature is 1900
~2300 DEG C, be more than 20 hours, preferably 50~150 hours according to different growth rate growth times.
It is preferred that in carborundum polycrystalline ceramics growth course, growth atmosphere is in argon gas, nitrogen, helium and hydrogen
It is at least one.
It is preferred that the purity of the sic raw material is to be 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%.
It is preferred that the thermograde 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, present invention also offers a kind of carborundum polycrystalline ceramic grown according to above-mentioned method, institute
State the boundary dimensions (diameter) of carborundum polycrystalline ceramic at 4 inches and more than, preferably 4~8 inches.
This is it is preferred that the carborundum polycrystalline ceramic includes conductive silicon carbide polycrystalline ceramic and semi-insulating type
Carborundum polycrystalline ceramic, wherein the resistivity of the conductive silicon carbide polycrystalline ceramic 0.015 Ω cm~
0.03 Ω cm scopes, the resistivity ＞ 10 of the semi-insulating type carborundum polycrystalline ceramic5Ω·cm。
Growing method of the present invention is simple, and the carborundum polycrystalline ceramics is more excellent than Conventional silicon carbide ceramic performance, and its is equal
Even property is good, and more preferably, purity is higher for consistency, and thermal conductivity is more preferably, adjustable by semi-insulating and conductiving doping resistivity, and passes through
Cost of helping is low, can process composition element of different shapes, realize the broader applications of carborundum polycrystalline ceramics.
Brief description of the drawings
Fig. 1 is growth room's structural representation that physical vapor transport (PVT) method grows SiC polycrystalline ceramics；
Fig. 2 is that embodiment 1 uses physical vapor transport (PVT) method in growth pressure for 20Torr, growth temperature be 2080 DEG C with
And 4 inches of SiC polycrystalline crystal ingots that growth time grows under the conditions of 100 hours；
Fig. 3 is 4 inches of polycrystalline ceramics pieces of the SiC polycrystalline crystal ingot correspondence cutting prepared using embodiment 1；
Fig. 4 is that embodiment 2 uses physical vapor transport (PVT) method in growth pressure for 10Torr, growth temperature be 2120 DEG C with
And 5 inches of SiC polycrystalline crystal ingots that growth time grows under the conditions of 100 hours；
Fig. 5 is the polycrystalline ceramics piece of the 5 inches of SiC polycrystalline crystal ingots correspondence cutting prepared using embodiment 2；
Fig. 6 is embodiment 2 using physical vapor transport (PVT) method and using 5 inches of SiC of the graphite cover growth for being coated with carbon film layer
The back photo of polycrystalline crystal ingot；
Fig. 7 is 5 inches that comparative example 1 is not grown using physical vapor transport (PVT) method using the graphite cover for being coated with carbon film layer
The back photo of SiC polycrystalline crystal ingots；
Reference：
1st, graphite crucible top cover；
2nd, graphite crucible body；
3rd, SiC raw materials；
4th, carbon film layer；
5th, SiC polycrystalline ceramics.
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, be not intended to limit the present invention.
The invention provides the grower that a kind of physical vapor transport (PVT) method grows SiC polycrystalline ceramics.Described device
It is made up of crucible body, crucible top cover and the carbon film layer for being arranged on crucible top cover inner surface.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 institutes
Show, wherein carbon film layer 4 is arranged at the inner surface of graphite crucible top cover 1.Also carbon film layer can be coated with crucible body on surface.
Illustrate to following exemplary the growth side for the high-purity carborundum polycrystalline ceramics (SiC polycrystalline materials) that the present invention is provided
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 into carbon film is put
In low-temperature space, sunk using physical vapor transport (PVT) method or high temperature chemical vapor deposition method on the carbon film surface of graphite cover
Product growth carborundum polycrystalline ceramics.Specifically, during 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, make graphite crucible body bottom and/or bottom be located at heating zone, with
The rise of temperature, sic raw material 3 is gradually distilled, and carborundum polycrystalline ceramics is grown on the carbon film layer 4 positioned at low-temperature space
5.Due to there is certain thickness carbon film layer 4 between carborundum polycrystalline ceramics and graphite cover, not only significantly reduce due to polycrystalline
Thermal stress caused by directly being contacted with graphite cover avoids polycrystalline from ftractureing, but also protects the adhesion of polycrystalline and graphite cover to destroy,
Drastically increase carborundum polycrystalline quality and yield.
In carborundum 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 carborundum polycrystalline ceramic is different.According to not
Same growth rate, growth time was controlled more than 20 hours, preferably 50~150 hours.Grown in carborundum polycrystalline ceramics
Cheng Zhong, growth atmosphere can be at least one of argon gas, nitrogen, helium and hydrogen.
As an example, the present invention uses and prepares carbon based on physical vapor transport (PVT) method for preparing single-crystal silicon carbide
SiClx polycrystalline ceramic, is placed in graphite crucible high-temperature region by sic raw material first, and growth inner surface then is coated with into carbon film
Graphite cover be placed in low-temperature space, finally growth pressure be 2~50Torr, growth temperature be 1900~2300 DEG C under conditions of
(thermograde 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 carborundum polycrystalline ceramics of graphite cover.
Carbon film layer 4 in the present invention is preferentially prepared by chemical vapour deposition technique.In addition the carbon film layer 4 can be with
By high after thermal evaporation, physical vapour deposition (PVD), magnetron sputtering, electron beam evaporation, reaction-sintered, uniform plating graphite glue or carbohydrate gum
Warm solidification, plasma coating, molecular beam epitaxy, liquid phase epitaxy, laser deposition etc. are deposited and extension is in crucible top cover
On inner surface.These methods are all known technologies in film field, be will not be repeated here.
The compact film for being arranged at crucible top cover inner surface is extremely stable at a temperature of SiC polycrystalline growths, the thickness of film layer
Degree can be 0.01~1mm, preferably 10~100 μm, not only ensure prepare polycrystalline material uniformity, can also avoid polycrystalline with
Graphite cover directly contact causes the problem of stress is excessive cracking.
Further, the carborundum polycrystalline ceramics, its resistivity can be by being purified or doping way enters to raw material
Row regulation.The purity of the sic raw material is to be 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 many that the present invention can obtain conductive silicon carbide by different element dopings
Brilliant ceramic material (for example, nitrating element etc.) and semi-insulating type carborundum polycrystalline ceramic (for example, non-impurity-doped or doping vanadium,
Aluminium element etc.).The resistivity of wherein described conductive silicon carbide polycrystalline ceramic is in the Ω cm of 0.015 Ω cm~0.03
Scope, the resistivity ＞ 10 of the semi-insulating type carborundum polycrystalline ceramic5Ω·cm。
High-purity carborundum polycrystalline ceramics growing method of the present invention is comprised the step of：Sic raw material is placed in graphite earthenware
Crucible high-temperature region, low-temperature space is placed in by the graphite cover for being coated with carbon film, using physical vapor transport method on the carbon film surface of graphite cover
Deposition growing carborundum polycrystalline ceramics.Wherein the thickness and performance of carborundum polycrystalline ceramic can be grown by growth temperature
Pressure, growth time are adjusted with the growth parameter(s) such as, growth atmosphere component and raw material doping.The carborundum polycrystalline ceramics ratio
Conventional silicon carbide ceramic performance is more excellent, and more preferably, consistency is higher, and purity is higher for its uniformity, and thermal conductivity is more preferable, resistivity
It is adjustable and financial cost is low.
The present invention prepares carborundum polycrystalline ceramic using physical vapor transport (PVT) method.Using laser conductometer
Measure the thermal conductivity of prepared carborundum polycrystalline ceramics.Prepared carbonization policrystalline silicon pottery is measured using Hall effect tester
The resistivity of porcelain.The purity of prepared carborundum polycrystalline ceramics is measured using ion microprobe.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope 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 this paper explanation
Selected in suitable scope, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Top is coated with to the graphite cover (graphite crucible top cover) of carbon film layer first, bottom material area is equipped with sic raw material (purity
99.9%) graphite crucible is placed in heat preservation carbon felt, is placed into crystal growth furnace chamber and (sic raw material is placed in into graphite crucible
Body high-temperature region, the graphite crucible top cover that growth inner surface is coated with into carbon film is placed in low-temperature space, from graphite crucible top cover to graphite earthenware
The thermograde of the bottom of crucible body is 2 DEG C/cm.), vacuum is evacuated to 1.0 × 10-2Below Pa, 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 growth 100h, journey
Sequence cooling down is to room temperature, and blow-on obtains carborundum polycrystalline ceramic of the thickness for 15mm (such as Fig. 2 institutes on graphite cover
Show), obtain carborundum polycrystalline ceramics piece (as shown in Figure 3), its thickness 1mm, a diameter of 100mm finally by machining),
Understand effectively prepare 4 inch silicon carbide polycrystalline materials using this patent method from Fig. 2 and Fig. 3, measuring its resistivity is
0.02Ω·cm.Fig. 3 is the polarisation photo of the SiC polycrystalline ceramics pieces of physical vapor transport (PVT) method growth in embodiment 1, from
Polycrystalline material uniformity is understood in Fig. 3.Wherein the thickness and performance of carborundum polycrystalline ceramic can by growth temperature,
Growth pressure, growth time are adjusted with the growth parameter(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 crucible of sic raw material (purity 99.9%)
It is placed in heat preservation carbon felt, places into crystal growth furnace chamber and (sic raw material is placed in graphite crucible body high-temperature region, will be grown
The graphite crucible top cover that inner surface is coated with carbon film is placed in low-temperature space, from graphite crucible top cover to the temperature of the bottom of graphite crucible body
Degree gradient is 2.5 DEG C/cm), vacuum is evacuated to 1.0 × 10-2Below Pa, applying argon gas to growth pressure 10Torr, start to warm up to
After 2120 DEG C of growth temperature, growth 100h, program cooling down to room temperature, it is 20mm's that blow-on obtains thickness on graphite cover
Carborundum polycrystalline ceramic (as shown in Figure 4), carborundum polycrystalline ceramics piece is obtained (such as Fig. 5 institutes finally by machining
Show), its thickness 1mm, a diameter of 125mm understand effectively prepare 5 inch silicon carbides using this patent method from Fig. 4 and Fig. 5
Policrystalline silicon material, it is 1.5 × 10 to measure its resistivity6Ω·cm.The thickness and performance of wherein carborundum polycrystalline ceramic can
By growth temperature, growth pressure, growth time are adjusted with, growth atmosphere component and the raw material growth parameter(s) such as adulterate.
Embodiment 3
Top is coated with to the graphite cover of carbon film layer first, bottom material area is equipped with the graphite earthenware of sic raw material (purity 99.99%)
Crucible is placed in heat preservation carbon felt, is placed into crystal growth furnace chamber and (sic raw material is placed in into graphite crucible body high-temperature region, by life
The graphite crucible top cover that long 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
Thermograde is 1.5 DEG C/cm), vacuum is evacuated to 1.0 × 10-2Below Pa, applying argon gas are started to warm up to growth pressure 10Torr
To 2120 DEG C of growth temperature, after growth 100h, program cooling down to room temperature, it is 20mm that blow-on obtains thickness on graphite cover
Carborundum polycrystalline ceramic, finally by machining obtain carborundum polycrystalline ceramics piece (thickness 1mm, it is a diameter of
125mm), it is 8.2 × 10 to measure its resistivity6Ω·cm。
Embodiment 4
Top is coated with to the graphite cover of carbon film layer first, bottom material area equipped with sic raw material (purity 99.99%, doped with vanadium,
Content is 0.5wt%) graphite crucible be placed in heat preservation carbon felt, place into and (be placed in sic raw material in crystal growth furnace chamber
Graphite crucible body high-temperature region, the graphite crucible top cover that growth inner surface is coated with into carbon film is placed in low-temperature space, from graphite crucible top cover
Thermograde to the bottom of graphite crucible body is 2.0 DEG C/cm), vacuum is evacuated to 1.0 × 10-2Below Pa, applying argon gas to life
Long pressure 10Torr, is started to warm up to 2120 DEG C of growth temperature, after growth 100h, program cooling down to room temperature, and blow-on is in stone
The carborundum polycrystalline ceramic that thickness is 20mm is obtained on inky cap, carborundum polycrystalline ceramics is obtained finally by machining
Piece (thickness 1mm, a diameter of 125mm), it is 2.4 × 10 to measure its resistivity5Ω·cm。
Comparative example 1
In order to carry out Experimental comparison, progress carborundum polycrystalline ingot on the graphite cover of carbon film layer is not coated with inner surface using PVT methods
Growth, growthing process parameter be the same as Example 2, growth removes carborundum polycrystalline ingot after terminating from graphite cover, as shown in Figure 7 can be with
Be clearly visible carborundum polycrystalline ingot back and graphite cover and occur firm adhesion, when removing, carborundum polycrystalline ingot it is destroyed so as to
Cracking the problem of.Fig. 6 is then carborundum polycrystalline ingot of the embodiment 2 using the graphite cover growth for being coated with carbon film layer, it can be seen that
Its back uniformity, is not destroyed.By comparative example, the graphite interior surface plating carbon film layer that explainable this patent is invented
Growth carborundum polycrystalline ingot can effectively discharge carborundum polycrystalline ingot internal stress, it is to avoid polycrystalline ingot ftractures, and improve the matter of SiC crystal
The yield of amount.
The performance data for the carborundum polycrystalline ceramic that table 1 is prepared for the present invention；
It is noted that above-mentioned embodiment is that the present invention is described in detail, it should not be to the present invention
Limitation.For a person skilled in the art, in the objective and scope without departing from claim, there can be a variety of shapes
The change of formula and details.
Claims (8)
1. a kind of growing method of the adjustable carborundum polycrystalline ceramic of large scale resistivity, it is characterised in that use graphite
Crucible holds sic raw material, and wherein graphite crucible is made up of graphite crucible top cover and graphite crucible body, in the graphite crucible
Carbon film layer is provided with surface, sic raw material is placed in graphite crucible body, the graphite crucible top cover is covered, is put into growth
In stove, and the bottom and/or bottom of the graphite crucible body is set to be located at heating zone so that the temperature of the bottom of graphite crucible body is high
In the temperature of graphite crucible top cover, using physical vapor transport method or high temperature chemical vapor deposition method in the carbon film layer table
Look unfamiliar long carborundum polycrystalline ceramic.
2. growing method according to claim 1, it is characterised in that the thickness of the carbon film layer is 0.01~1 millimeter, excellent
Elect 10~100 microns as.
3. growing method according to claim 1 or 2, it is characterised in that in carborundum polycrystalline ceramics growth course, raw
Long atmosphere pressure is 2~50Torr, and growth temperature is 1900~2300 DEG C, and growth time is more than 20 hours, preferably 50~150
Hour.
4. growing method according to claim 3, it is characterised in that in carborundum polycrystalline ceramics growth course, growth
Atmosphere is at least one of argon gas, nitrogen, helium and hydrogen.
5. the growing method according to any one of claim 1-4, it is characterised in that the purity of the sic raw material is
It is not less than 99.8%；Or doped with least one of vanadium, aluminium and nitrogen in the sic raw material, doping is 0.1~5wt%.
6. the growing method according to any one of claim 1-5, it is characterised in that from graphite crucible top cover to graphite earthenware
The thermograde of the bottom of crucible body is 1 DEG C/cm~5 DEG C/cm, preferably 1.5 DEG C/cm~3 DEG C/cm.
7. a kind of carborundum polycrystalline ceramic of method growth according to any one of claim 1-6, its feature exists
In, the carborundum polycrystalline ceramic boundary dimensions at 4 inches and more than, preferably 4~8 inches.
8. carborundum polycrystalline ceramic according to claim 7, it is characterised in that the carborundum polycrystalline ceramic
Including conductive silicon carbide polycrystalline ceramic and semi-insulating type carborundum polycrystalline ceramic, wherein the conductive silicon carbide
The resistivity of polycrystalline ceramic is in the Ω cm scopes of 0.015 Ω cm~0.03, the semi-insulating type carbonization policrystalline silicon pottery
The resistivity ＞ 10 of ceramic material5 Ω·cm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110331438A (en) * | 2019-07-30 | 2019-10-15 | 河北普兴电子科技股份有限公司 | A method of inhibit carbon package volume defect in conductive silicon carbide crystal growth to generate |
| 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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| 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 |
| WO2023143297A1 (en) * | 2022-01-29 | 2023-08-03 | 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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