CN105603530B - For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals - Google Patents
For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals Download PDFInfo
- Publication number
- CN105603530B CN105603530B CN201610018942.1A CN201610018942A CN105603530B CN 105603530 B CN105603530 B CN 105603530B CN 201610018942 A CN201610018942 A CN 201610018942A CN 105603530 B CN105603530 B CN 105603530B
- Authority
- CN
- China
- Prior art keywords
- carborundum
- raw material
- particle
- rapid growth
- speed rapid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to the growing method of a kind of raw material for carborundum crystals high-speed rapid growth and carborundum crystals, belong to technical field of semiconductors.In order to solve the problems, such as that existing carborundum crystals life lifting speed difference is low with efficiency, a kind of method of the raw material for carborundum crystals high-speed rapid growth and carborundum crystals high-speed rapid growth is provided, the raw material contains carborundum particle, and the average grain diameter of the carborundum particle is less than 5 μm or the mixed material formed using the mixing of the carborundum particle of at least two different shapes and/or at least two different-grain diameters, and at least it is less than 5 μm of carborundum particle in the raw material containing a kind of average grain diameter.And Silicon carbide crystal growth method includes above-mentioned raw materials being put into crucible, heating crucible makes the raw material in crucible be recrystallized after distilling, and obtains carborundum crystals.The purpose for improving rate of sublimation and efficiency can be reached.
Description
Technical field
The present invention relates to the growing method of the raw material for carborundum crystals high-speed rapid growth and carborundum crystals, belong to and partly lead
Body technique field.
Background technology
Single-crystal silicon carbide has that energy gap is big, breakdown electric field is high, thermal conductivity is big and dielectric constant is small and physics and chemistry
Unique characteristic such as stable performance, it is considered to be the preferable semi-conducting material such as manufacture opto-electronic device, Deep trench termination.
In the past, the manufacture method as carborundum crystals, typically by under the high temperature conditions entering raw material silicon carbide powder
Row distillation recrystallization, grows in silicon carbide seed and forms the monocrystal or polycrystal of carborundum.It is well known that as raw material
Silicon carbide powder have and its consequence for the speed to distil with crystallization.And in order to be maintained under the conditions of crystal growth
Speed fast and stable rate of sublimation and repeatability, it is mostly homogeneous by using micro-particles shapes rule, size, and shape and big
The small micropowder for being distributed concentration is as corresponding raw material.General common mode is in order to obtain bigger specific surface area, mostly
The tiny silicon carbide powder of particle diameter can be used, however, technology prejudice present in prior art be think due to using it is more tiny,
If the carborundum particle of regular shape, the density being packed together will become higher, so that the carborundum below surface
Powder is difficult to distil, and can not inherently improve the speed and efficiency of distillation.Therefore, it is mostly relatively more complete using shape
Carborundum particle is as raw material, the general carborundum particle using 100 μm of more than m, even if from thinner carborundum particle
Need the pre- secondary operation that first passes through to be fired into particle of the particle diameter in 100 μm of more than m, another aspect reason, now also deposit in the art
In certain prejudice, it is believed that the particle diameter of carborundum particle is too small, makes the intensity step-down of silicon carbide powder, is unable to maintain that the shape of particle
State, so as to influence the speed of distillation.Although improving specific surface area to a certain extent using the carborundum particle compared with small particle,
But with the progress of sublimation process, the density being packed together can become higher, so that the carborundum powder below surface
End is difficult to distil, and can not inherently improve the speed and efficiency of distillation.
The content of the invention
The present invention is for defect present in above prior art, there is provided a kind of original for carborundum crystals high-speed rapid growth
Material, solves the problems, such as it is how to improve rate of sublimation and efficiency, enables carborundum crystals high-speed rapid growth using sublimed method.
An object of the present invention technical scheme is that, one kind be used for the high fast-growing of carborundum crystals
Long raw material, the raw material contains carborundum particle, and the average grain diameter of the carborundum particle is less than 5 μm.
The present invention is used for the raw material of carborundum crystals high-speed rapid growth, and 5 μm of carbonization silicon grain is less than by using average grain diameter
Specific item is in order that raw material carborundum particle can be easy to suspend when being passed through gas, so as in overall sublimation process
In, be not in bulk density it is excessive and the problem of reduce rate of sublimation and efficiency, and if particle diameter is excessive, then growing
Cheng Zhongxu is passed through the gas compared with hyperbar or larger flow, and because flow is excessive, easily make the gaseous carbon SiClx on crucible top
Largely taken out of crucible, the speed and efficiency of distillation can be influenceed on the contrary, be unfavorable for the high-speed rapid growth of carborundum crystals.Certainly, on
It can be single-crystal silicon carbide or carborundum polycrystalline form to state described carborundum crystals.
In the above-mentioned carborundum particle raw material for carborundum crystals high-speed rapid growth, preferably, the carborundum
The specific surface area of particle is more than or equal to 0.5m2/g.By making the specific surface area of carborundum particle be more than or equal to 0.5m2/ g, Neng Gouti
The high while heated area with distillation, so as to improve the distillation amount of carborundum, while also ensure that gaseous carbon SiClx in crucible
Concentration so that carborundum crystals can high-speed rapid growth, reached the purpose for improving rate of sublimation and efficiency.Preferably, institute
The average grain diameter of carborundum particle is stated at 1.0 μm~3.0 μm.Preferably it is more than or equal to from the specific surface area of carborundum particle
1.0m2/ g carborundum particle.
In the above-mentioned carborundum particle raw material for carborundum crystals high-speed rapid growth, preferably, the carborundum
The some or all of particle are the carborundum particle with mechanicalness and/or physical injury.In order that raw material carborundum
The integrality damage of particle is fallen, and the crystal boundary of carborundum particle is destroyed by mechanicalness and/or physical method, makes it in part
After distillation, it is easily broken off or ftractures, show new surface, so as to more effectively keeps certain sublimation area.
In the above-mentioned carborundum particle raw material for carborundum crystals high-speed rapid growth, preferably, in the raw material
Also it is mixed with the solid matter for not gasifying under the hot conditions below 2400 DEG C or not melting and forms mixed material.By adding
The solid matter for not gasifying or not melting under less than 2400 DEG C of hot conditions, make its in the sublimation process of carborundum particle not
It can be sublimated, by increasing capacitance it is possible to increase the gap between mixed material, mixed material is had enough in state loosely, guarantee
Sublimation area, the effect for improving rate of sublimation is realized, and the carbonization silicon vapor under raw material surface can be provided and passed through
Gap distils upwards, it is possible to increase the purpose of the concentration of carborundum steam.As it is further preferably, typically make the solids
The average grain diameter of matter is more than the minimum average particle diameters of carborundum in raw material.The average grain diameter of solid matter is preferably set to be more than in raw material
5 times or more of the minimum average particle diameters of carborundum.The further carborundum particle made in mixed material is in loosely
State, it is had enough sublimation areas, realize the effect for improving rate of sublimation and efficiency.
In the above-mentioned carborundum particle raw material for carborundum crystals high-speed rapid growth, preferably, described 2400
The solid matter for not gasifying or not melting under hot conditions below DEG C is selected from tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and oxidation
One or more in magnesium.
In the above-mentioned carborundum particle raw material for carborundum crystals high-speed rapid growth, preferably, described 2400
The solid matter for not gasifying or not melting under hot conditions below DEG C accounts for 1.0wt%~40wt% of raw material gross mass.Pass through
On the one hand controlling the amount of solid matter can make carborundum particle keep enough laxities, improve sublimation area, on the other hand,
Also it can ensure there are enough carborundum particle raw materials, have enough carborundum in guarantee system.
The second object of the present invention technical scheme is that, the raw material is different using at least two
The mixed material that the carborundum particle of shape and/or at least two different-grain diameters is mixed and formed, and at least contain in the raw material
There is the carborundum particle that a kind of average grain diameter is less than 5 μm.
By substantial amounts of research, discovery is existing in order to increase the specific surface area of distillation and operability, general using big
Small homogeneous and small silicon carbide powder.However, although this mode improves specific surface area on the surface, actually adding
During work, with the progress of sublimation process, the bulk density of fine particles can increase, so as to have impact on the speed of distillation,
In real process and it can not embody preferable effect.The present invention is by using the carborundum particle of at least two particle diameters as former
Material, can make raw material overlapping in a manner of a variety of levels during stacking, add between carborundum particle and particle
Space, carborundum particle is set to be stacked in a manner of polynary, and in actual sublimation process, as a result of the carbonization of different-grain diameter
Silicon particle, each interparticle interval is not fully identical, even if with the progress of sublimation process, also will not be because of bulk density mistake
Rate of sublimation is influenceed greatly, so as to realize the effect for improving rate of sublimation；And by using variform carborundum particle, energy
Enough to form three-dimensional space structure, raw material is avoided the occurrence of in sublimation process influences rate of sublimation because bulk density is excessive
Phenomenon；Simultaneously as shape is different, and it is different equivalent to specific surface area of the carborundum particle under same particle size, so that different
Distillation amount of the carborundum particle of shape in sublimation process is different, so as to can also reduce because bulk density is excessive
The phenomenon of rate of sublimation is influenceed, improves the speed of distillation on the whole, and by making the carborundum particle of wherein at least one
The purpose of being less than 5 μm of carborundum particle using average grain diameter is in order that raw material carborundum particle can be passed through by crucible bottom
Gas is blown afloat, and can be easy to suspension, and so as in overall sublimation process, it is excessive and make distillation fast to avoid the occurrence of bulk density
The problem of degree and efficiency reduce.It can be more beneficial for being blown afloat by using carborundum particle of the average grain diameter less than 5 μm and hang
It is floating, so as to greatly improve heated area and the area of distillation, so as to improve the concentration of carborundum gas, reach silicon carbide whisker
The purpose of body high-speed rapid growth.And if particle diameter is excessive, then need to be passed through the gas compared with hyperbar or larger flow in growth course
Body, and if flow is excessive, the gaseous carbon SiClx on crucible top is largely taken out of the external world, the speed of distillation can be influenceed on the contrary
Degree and efficiency, it is unfavorable for the high-speed rapid growth of carborundum crystals.To sum up, the present invention is by using different size and carbon of different shapes
SiClx grain is mixed to form the space structure of solid, and combines and use the average grain diameter of at least one carborundum particle to make less than 5 μm
It is easier to suspended state, so as to reach the effect with the higher speed of growth and efficiency, reaches the high speed of carborundum crystals
The effect of growth.It is of course also possible to it is that the average grain diameter of the carborundum particle of a variety of different average grain diameters is respectively less than 5 μm.
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, in the carborundum particle at least
It is more than or equal to 0.5m containing a kind of specific surface area2/ g carborundum particle.The sublimation area of carborundum particle can be increased, improved
The speed and efficiency of distillation, the average grain diameter of carborundum particle of different shapes is preferably set to be less than 5 μm and be more than specific surface area
Equal to 1.0m2/g。
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, the shape of the mixed material point
Cloth is different.Due to the mixed material of different shape distribution, its distillation amount in sublimation process is different, makes what different shape was distributed
Each particle variable quantity of mixed material is different, increases the gap between particle, and it is not in the excessive phenomenon of bulk density to make,
Rate of sublimation can more effectively be improved.As further preferably, the distribution of shapes of the mixed material is different, and the carbon
The specific surface area of SiClx particle is more than or equal to 0.5m2/g。
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, the carborundum of the different-grain diameter
Particle is the different carborundum particle of particle size distribution, and is shown at least in the particle size distribution curve of the mixed material
2 main particle diameter distribution peak values.Here mixed material is can to include the carborundum particle of different-grain diameter size or shape, may be used also
With including the solid matter for not gasifying or not melting under the mixed hot conditions below 2400 DEG C.Show mixed material
State loosely, guarantee have larger sublimation area and distillation amount, so as to improve rate of sublimation and efficiency, make silicon carbide whisker
Body being capable of high-speed rapid growth.As a kind of simple resolving method：Carborundum particle can be put into particle size analyzer to be divided
Analysis.
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, one in the carborundum particle
Some or all of is using the carborundum particle with mechanicalness and/or physical injury.Equally, in order to make raw material
The integrality damage of carborundum particle is fallen, and the crystal boundary of carborundum particle is destroyed by mechanicalness and/or physical method, makes it
After partial sublimation, it is easily broken off or ftractures, show new surface, so as to keeps certain sublimation area.
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, being also mixed with the mixed material
The solid matter for not gasifying under hot conditions below 2400 DEG C or not melting.The purpose of adding above-mentioned solid matter be in order that
It will not be sublimated in the sublimation process of carborundum particle, so as to increase the gap between mixed material and make mixing
Raw material is in state loosely, realizes the purpose for improving rate of sublimation and efficiency.As it is further preferably, typically make solid
The average grain diameter of material is more than the minimum average particle diameters of carborundum in mixed material.The further carbonization made in mixed material
Silicon particle is in state loosely, makes have enough heating surface area and sublimation area, reaches carborundum crystals high-speed rapid growth
Purpose.
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, the height below 2400 DEG C
The one kind of the solid matter for not gasifying or not melting under the conditions of temperature in tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and magnesia
It is or several.
In the above-mentioned raw material for carborundum crystals high-speed rapid growth, preferably, the height below 2400 DEG C
The solid matter for not gasifying or not melting under the conditions of temperature accounts for 1.0wt%~40wt% of mixed material gross mass.It is solid by controlling
On the one hand the amount of body material can make carborundum particle keep enough laxities, improve sublimation area, on the other hand, also can
Guarantee has enough carborundum particle raw materials, ensures there are enough carborundum gas concentrations in crucible.It is further preferred, institute
State 10wt%~15wt% that solid matter accounts for mixed material gross mass.
The third object of the present invention technical scheme is that, a kind of carborundum crystals high-speed rapid growth
Method, this method include above-mentioned raw materials being put into crucible, and heating crucible makes the raw material in crucible be recrystallized after distilling, and obtains
Carborundum crystals.
In the method for above-mentioned carborundum crystals high-speed rapid growth, preferably, this method also includes feeding from the bottom of crucible
The mixture of gas or liquid or both, and make the raw material in crucible be in floating state, wherein described liquid can pass through
Heating becomes gas or is decomposed into gas.By making carborundum particle of the average grain diameter less than 5 μm be in floating state,
The quantity for the silicon-carbide particles for greatly adding while being heated, the surface area for also increasing while being heated, due in identical
For pressure with a temperature of, the distillation amount of the carborundum of similar face product is identical, adds heated surface area, that is, adds carbonization
The amount of silicon distillation, so as to improve the concentration of gaseous carbon SiClx in crucible, and then improves the speed of growth of carborundum crystals.And
Carborundum after distillation is blown afloat further up so that the gaseous carbon SiClx of high concentration is formed at the top of crucible, is advantageous to carbon
The high-speed rapid growth of SiClx crystal.If simultaneously using average grain diameter in below 5um raw particles, the gas being easily fed into due to it
Body is blown afloat, and reaches the state of floating, therefore is advantageous to the raising of carborundum vapour concentration.Or it is more than or equal to using specific surface area
0.5m2/ g carborundum particle raw material, it is more than or equal to 1.0m preferably with than surface2/ g carborundum particle raw material, it is same easy
The gas being fed into is blown afloat, and reaches raising of the floating state in favor of carborundum vapour concentration.
In the method for above-mentioned carborundum crystals high-speed rapid growth, the gas can be selected from current-carrying gas, etching gas, carbon source
The mixed gas of gas, silicon source gas or several gases of the above.Gas therein can be by forming after liquid gasification
Gas or it is heated after the gas that decomposites, current-carrying gas can select gas or the mixing such as hydrogen, argon gas, helium, nitrogen
Inert gas, it can be used for driving caused carborundum gas during silicon carbide powder sublimes；Etching gas can select chlorine
Gas, hydrogen chloride, either the mixed gas of the chlorine-containing gas such as trichloroacetic acid, trichloro ethylene or several gases, can be used for corroding
The impurity of a part is removed, corrosion is may also be used for and removes the carborundum being grown on seed crystal, make the carborundum in growth
Plane of crystal keeps smooth, reduces crystal defect, is advantageous to improve the quality of growing silicon carbice crystals；Carbon-source gas can be selected
Such as carbon containing hydrocarbon gas of methane, ethane, ethene, for supplementing carborundum, carbon is not in sublimation process
Foot；Silicon source gas can select alkanes gas of such as silane containing element silicon, for supplementing carborundum silicon member in sublimation process
The deficiency of element.When producing carborundum crystals, sometimes according to the difference of required characteristic of semiconductor, impurity gas is deliberately added into,
Become N-type or P-type semiconductor.Such as the characteristic that nitrogenous gas can make carborundum have N-type semiconductor is added, and
The material of boracic is added, can make carborundum that there is the characteristic of P-type semiconductor.Wherein nitrogen can either be used as current-carrying gas,
It can be used when manufacturing N-type carborundum crystals as impurity gas.And nitrogen is added, carborundum crystals knot can be improved
Brilliant quality.
In the method for above-mentioned carborundum crystals high-speed rapid growth, preferably, the heating crucible is specially：Using 1 or
The multiple heat sources of person carry out heating crucible.The heating effect of crucible different zones can be more effectively controlled, is accurately controlled
Sic raw material swims the temperature of part in crucible, improves heating-up temperature, its is accelerated distillation, and the steam improved near seed crystal is dense
Degree, reach the purpose of carborundum crystals high-speed rapid growth.
In the method for above-mentioned carborundum crystals high-speed rapid growth, as another embodiment, the heating crucible is specially：
The heating-up temperature for making the solid silicon carbide particle raw material of bottom in crucible is 2100 DEG C~2600 DEG C, make in crucible middle part gas and/
Or the heating-up temperature of the sic raw material of solid-state mixing is 2200 DEG C~2800 DEG C, makes the Gaseous carbonization silicon raw material of crucible internal upper part
Heating-up temperature be 1900 DEG C~2400 DEG C.By being heated to the specific aim under each state of sic raw material, and make seed crystal
Surface can keep the temperature of suitable carborundum crystallization, and the speed of growth of carborundum crystals is improved with this.
In summary, there is advantages below compared to prior art, the present invention：
1. the present invention is used for the raw material of carborundum crystals high-speed rapid growth, 5 μm of carborundum is less than by using average grain diameter
Particle enables raw material carborundum particle to be easy to suspension, so as to be not in bulk density mistake in overall sublimation process
The problem of greatly reducing rate of sublimation and efficiency, so as to improve the distillation amount of carborundum, realize and improve rate of sublimation and efficiency
Purpose.
2. the present invention is used for the raw material of carborundum crystals high-speed rapid growth, by using the carborundum particle of at least two particle diameters
With carborundum particle of different shapes as raw material, raw material can be made overlapping in a manner of a variety of levels during stacking,
The way of contact between carborundum particle and particle is added, carborundum particle is stacked in a manner of polynary, and in actual liter
During China, because shape is different, distillation amount of the carborundum particle of different shapes in sublimation process can be made different,
The gap between carborundum particle is ensure that, the phenomenon of rate of sublimation is influenceed because bulk density is excessive so as to avoid, whole
The speed of distillation is improved on body.
3. the present invention is used for the raw material of carborundum crystals high-speed rapid growth, by adding under the hot conditions below 2400 DEG C
Do not gasify or the solid matter that does not melt can increase the gap of mixed material, mixed material is in state loosely, together
When make the steam of sic raw material lower surface in crucible, risen by gap, improve the concentration of carborundum steam, reach carbonization
The purpose of silicon crystal high-speed rapid growth.
4. the method for the carborundum crystals high-speed rapid growth of the present invention, by the way that the silicon carbide powder being deposited on inside crucible is blown
Rise, with reference to the raw material of the present invention, silicon carbide powder is in floating state, gap between silicon carbide powder is increased with this, made
Silicon carbide powder is more dispersedly distributed in crucible so that silicon carbide powder can rapid sublimation, realize raising rise
Magnificent speed and efficiency, reach the purpose of carborundum crystals high-speed rapid growth.
Brief description of the drawings
Fig. 1 is the surface topography map for the carborundum particle that the method for embodiment 1 obtains.
Fig. 2 is the surface topography map for the carborundum particle that the method for embodiment 2 obtains.
Fig. 3 is the surface topography map for the carborundum particle that the method for embodiment 3 obtains.
Fig. 4 is the grading curve figure of another carborundum particle of the present invention.
Fig. 5 is the grading curve figure of another carborundum particle of the present invention.
Wherein, surface topography map is the electron microscope using Keyemce Electron microscopy in Fig. 1-3.
Embodiment
Below by specific embodiments and the drawings, technical scheme is described in further detail, but this
Invention is not limited to these embodiments.
This raw material for being used for carborundum crystals high-speed rapid growth contains carborundum particle, and the average grain diameter of carborundum particle is small
In 5 μm.By make carborundum particle average grain diameter be less than 5 μm, can make in sublimation process feed gas effect under energy
It is enough preferably to suspend, from without bulk density it is excessive the problem of, preferably make, the specific surface area of carborundum particle is big
In equal to 0.5m2/ g, it is more than or equal to 0.5m with reference to the specific surface area of carborundum particle is made2/ g, the area of distillation is improved, so as to
The distillation amount of carborundum is improved, realizes the purpose for improving rate of sublimation and efficiency, ensures the concentration of carborundum in crucible, reaches high
The purpose of the long carborundum crystals of fast-growing.Preferably, the specific surface area of carborundum particle is made to be more than or equal to 1.0m2/g.It is, of course, also possible to
It is the carborundum particle with mechanicalness and/or physical injury to make from some or all of carborundum particle, specifically
Ratio dosage can be adjusted according to actual conditions, usage ratio number have no effect on the present invention essence.Pass through machine
Tool and/or physical method destroy the crystal boundary of carborundum particle, make it after partial sublimation, are easily broken off or ftracture,
New surface is showed, so as to more effectively keep certain sublimation area.Mechanicalness therein and/or physical destruction can
With by grinding, shearing, high velocity impact the methods of realize, it is preferred to use it is paramount that gases at high pressure accelerate opposite sic raw material
Speed, it is set to collide with each other, the method is it is possible to prevente effectively from bring solid impurity into destructive process.It can also add in the feed
The solid matter for not gasifying under hot conditions below 2400 DEG C or not melting forms mixed material, can make carborundum particle
In state loosely, ensure enough sublimation area and heating surface area, realize high rate of sublimation and efficiency.Solid therein
Material can be the one or more in tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and magnesia.It can be adjusted according to being actually needed
The whole dosage for adding solid matter, preferably makes solid matter account for 1.0wt%~40wt% of mixed material gross mass, is preferably
10wt%~15wt%, optimal is 13wt%.Here mixed material refers to the total raw material of carborundum particle and solid matter.One
As make solid matter average grain diameter be more than mixed material in carborundum particle minimum average particle diameters.Make to be carbonized in mixed material
Silicon particle is at state loosely, there is enough sublimation areas.The average grain diameter of solid matter is preferably set to be more than raw material
5 times or more of the minimum average particle diameters of middle carborundum.
As another embodiment, this raw material for being used for carborundum crystals high-speed rapid growth is using at least two not similar shapes
The mixed material that the carborundum particle of shape and/or two kinds of different-grain diameters is mixed and formed, and at least containing a kind of average in raw material
Particle diameter is less than 5 μm of carborundum particle.Carborundum particle of the average grain diameter therein less than 5 μm can be the carbonization of different-grain diameter
Silicon particle or carborundum particle of different shapes.Mixed material overlapping accumulation, shape in a manner of a variety of levels can be made
Into the space structure of solid, so as to improve rate of sublimation and efficiency.Wherein, can be that distribution of shapes is different using mixed material
Form, by making the distribution of shapes of mixed material different, by increasing capacitance it is possible to increase the gap between particle, it is not in bulk density mistake to make
Big phenomenon, can more effectively improve rate of sublimation, preferably make at least containing a kind of specific surface area to be more than in carborundum particle
Equal to 0.5m2/ g carborundum particle, the optimal specific surface area for making carborundum particle of the average grain diameter less than 5 μm are more than or equal to
0.5m2/g.As another embodiment, the carborundum particle of different-grain diameter therein is the different carbonization of particle size distribution
Silicon particle, and the main particle diameter distribution peak value of at least two is shown in the particle size distribution curve of mixed material.Particle size distribution is not
It is same to be represented using grain size distribution.Wherein, the main particle diameter distribution peak value of above-mentioned at least two, actually refer to use at least 2
The mixed material that the carborundum particle of the different average grain diameters of kind is formed after mixing by a certain percentage, mixed material is detected
Afterwards, the form shown in particle size distribution curve.It is preferably, some or all for use in carborundum particle
Carborundum particle with mechanicalness and/or physical injury.Purpose is the integrality damage in order that raw material carborundum particle
Fall, the crystal boundary of carborundum particle is destroyed by mechanicalness and/or physical method, it is easily broken off after partial sublimation
Or cracking, new surface is showed, so as to keep certain sublimation area.It can also be mixed into above-mentioned mixed material
The solid matter for not gasifying or not melting under less than 2400 DEG C of hot conditions makes to form mixed material, can make carborundum particle
In state loosely, ensure enough sublimation area and heating surface area, realize the speed and efficiency for improving distillation.It is therein
Solid matter can be the one or more in tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and magnesia.Can be according to actual need
The dosage for adding solid matter is adjusted, solid matter is accounted for 1.0wt%~40wt% of mixed material gross mass, it is excellent
Elect 10wt%~15wt% as, optimal is 13wt%.Here mixed material refers to total original of carborundum particle and solid matter
Material.The general average grain diameter for making solid matter is more than the minimum average particle diameters of carborundum in mixed material.Make in mixed material
Carborundum particle is in state loosely, there is enough sublimation areas, realizes the purpose for improving rate of sublimation and efficiency.It is best
The average grain diameter of solid matter is set to be more than 5 times or more of minimum average particle diameters of carborundum in raw material.
The method that carborundum particle used can use prior art conventional in following examples is prepared, and such as uses
Acheson's method or CVD synthetic methods are prepared, and the method for following examples can also be used to be prepared.
Embodiment 1
The silicon metal powder that size is 1-10 μm using 200g per minute speed are supplied to temperature as in 2500 DEG C of stove, and
Carbon-source gas and argon gas are similarly supplied in stove with 200L per minute speed, and control furnace pressure to maintain 10000Pa,
Carry out after fully reacting, obtain corresponding silicon carbide powder, the mixing by obtained silicon carbide powder using hydrofluoric acid and nitric acid
Liquid carries out the silicon composition that processing removes residual, after drying, obtains corresponding silicon carbide powder, wherein, the reaction efficiency of carborundum
For 20%, the particle diameter of carborundum can be according to adjustment be actually needed, and the surface topography of silicon carbide powder is as shown in Figure 1.
Embodiment 2
The silicon metal powder that size is 1-10 μm using 5g per minute speed are supplied to temperature as in 2500 DEG C of stove, and will
Carbon-source gas and argon gas are similarly supplied in stove with 10L per minute speed, and control furnace pressure to maintain 1000Pa, are carried out
Fully after reaction, corresponding silicon carbide powder is obtained, obtained silicon carbide powder is entered using the mixed liquor of hydrofluoric acid and nitric acid
Row processing removes the silicon composition of residual, after drying, obtains corresponding silicon carbide powder, wherein, the reaction efficiency of carborundum is
90%, the particle diameter of carborundum can be as shown in Figure 2 according to actual adjustment, the surface topography of silicon carbide powder.
Embodiment 3
The silicon metal powder that size is 1-10 μm using 10g per minute speed are supplied to temperature as in 2500 DEG C of stove, and
Carbon-source gas and argon gas are similarly supplied in stove with 50L per minute speed, and control furnace pressure to maintain 2000Pa, are entered
After row fully reaction, corresponding silicon carbide powder is obtained, by obtained silicon carbide powder using hydrofluoric acid and the mixed liquor of nitric acid
The silicon composition that processing removes residual is carried out, after drying, obtains corresponding silicon carbide powder, wherein, the reaction efficiency of carborundum is
70%, the particle diameter of carborundum can be as shown in Figure 3 according to actual adjustment, the surface topography of silicon carbide powder.
Embodiment 4
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and 2 μm of the average grain diameter of carborundum particle, carborundum particle
Specific surface area is 2.0m2/g。
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.4mm/h.0.1mm/h~0.2mm/ of carborundum crystals is grown compared to using existing in general sic raw material
The h speed of growth, add at least more than 2 times.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals can use conventional side
Method, carborundum crystals are prepared preferably with following methods：
According to the needs actually to feed intake, above-mentioned raw materials are put into crucible, after heating crucible makes temperature reach 2400 DEG C, led to
Crossing from the bottom of crucible infeed silicon-containing gas (such as silane) makes the raw material in crucible be in floating state, the raw material in crucible is distilled
After recrystallize, obtain carborundum crystals.One or more heat sources can be used to carry out heating crucible, under specifically making in crucible
The heating-up temperature of the solid silicon carbide particle raw material in portion is 2100 DEG C, and the sic raw material of middle part gas-solid state mixing adds in crucible
Hot temperature is 2200 DEG C, and the heating-up temperature of the Gaseous carbonization silicon raw material of crucible internal upper part is 2400 DEG C.The growth of carborundum crystals
Speed can reach more than 0.4mm/h.
Embodiment 5
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and 3.0 μm of the average grain diameter of carborundum particle, carbonization silicon grain
The specific surface area of son is 1.5m2/g。
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.5mm/h.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals can use conventional side
Method, carborundum crystals are prepared preferably with following methods：
According to the needs actually to feed intake, above-mentioned raw materials are put into crucible, after heating crucible makes temperature reach 2400 DEG C, led to
Crossing from the bottom of crucible infeed current-carrying gas (such as argon gas, nitrogen) makes the raw material in crucible be in floating state, further control temperature
Degree makes the raw material in crucible be recrystallized after distilling, and obtains carborundum crystals.It can be added using one or more heat sources
Hot crucible, the heating-up temperature for specifically making the solid silicon carbide particle raw material of bottom in crucible are 2600 DEG C, middle part gas-solid in crucible
The heating-up temperature of the sic raw material of state mixing is 2800 DEG C, and the heating-up temperature of the Gaseous carbonization silicon raw material of crucible internal upper part is
1900℃.The speed of growth of carborundum crystals can reach more than 0.5mm/h.
Embodiment 6
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length uses carborundum particle and the molecular mixed material of ramet grain, and the average grain diameter of carborundum particle
4.0 μm, the specific surface area of carborundum particle is 2.3m2/ g, the average grain diameter of ramet particle is 8.0 μm, and ramet particle
The 40wt% of mixed material gross mass is accounted for, remaining is carborundum particle.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.6mm/h.
The specific preparation method of the carborundum crystals of the present embodiment is consistent with embodiment 4, repeats no more here.
Embodiment 7
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length uses the mixed material of carborundum particle and metal molybdenum powder constituent, and the average grain diameter of carborundum particle
1.0 μm, the specific surface area of carborundum particle is 0.5m2/ g, the average grain diameter of metal molybdenum are 6.0 μm, and ramet particle account for it is mixed
The 10wt% of raw material gross mass is closed, remaining is carborundum particle.
Certainly, the metal molybdenum of the above can use tungsten, metal tantalum or solid carbon to replace, and equally, can reach suitable
Effect.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.52mm/h.
The specific preparation method of the carborundum crystals of the present embodiment is consistent with embodiment 4, repeats no more here.
Embodiment 8
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and 1.5 μm of the average grain diameter of carborundum particle, carborundum particle
Specific surface area be 1.0m2/ g, and all carbonization silicon grains with mechanicalness and physical injury of carborundum particle therein
Son.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.6mm/h.
The specific preparation method of the carborundum crystals of the present embodiment is consistent with embodiment 4, repeats no more here.
Embodiment 9
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and the average grain diameter of carborundum particle is 1.5 μm, and be carbonized silicon grain
The specific surface area of son is 2.0m2/ g, and a part for carborundum particle therein is the carbon with mechanicalness and physical injury
SiClx particle, the specific carborundum particle with mechanicalness and physical injury account for 10wt%.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.53mm/h.
The specific preparation method of the carborundum crystals of the present embodiment is consistent with embodiment 4, repeats no more here.
Embodiment 10
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The mixed material that the raw material of fast-growing length is formed using carborundum particle and Zirconium oxide powder, and the average grain diameter of carborundum particle
3.0 μm, the specific surface area of carborundum particle is 1.5m2/ g, the average grain diameter for making Zirconia particles is 6.0 μm, and zirconium oxide grain
Son accounts for the 15wt% of mixed material gross mass, and remaining is carborundum particle, meanwhile, whole carborundum particles is with mechanicalness
With the carborundum particle of physical injury.
Certainly, the zirconium oxide of the above can use magnesia, metal molybdenum or solid carbon to replace, and equally, can reach suitable
Effect.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.71mm/h.
The specific preparation method of the carborundum crystals of the present embodiment is consistent with embodiment 4, repeats no more here.
Embodiment 11
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The mixed material that the raw material of body high-speed rapid growth is formed using two kinds of carborundum particle mixing of different shapes is specific using as schemed
The mixing that the carborundum particle of the carborundum particle of surface topography shown in 1 and surface topography as shown in Figure 2 is mixed is former
Material, and make a kind of carborundum particle therein average grain diameter be 2.0 μm, the average grain diameter of another carborundum particle can be with small
In 5 μm, 5 μm can also be more than.Wherein, the carborundum particle of surface topography as shown in Figure 1 and surface topography as shown in Figure 2
Carborundum particle mass ratio be 1：1.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of crystal reaches
0.52mm/h。
The method that the carborundum particle raw material of the present embodiment prepares carborundum crystals can use conventional method, preferably adopt
Carborundum crystals are prepared using the following method：
According to the needs actually to feed intake, above-mentioned raw materials are put into crucible, after heating crucible makes temperature reach 2200 DEG C,
Make the carborundum particle raw material in crucible in drift by feeding carbon-source gas (such as methane, ethane, ethene) from the bottom of crucible
Floating state, further control temperature the raw material in crucible is recrystallized after distilling, obtain carborundum crystals.Wherein it is possible to using
One or more heat sources carry out heating crucible, specifically make the heating-up temperature of the solid silicon carbide particle raw material of bottom in crucible
For 2200 DEG C, the heating-up temperature of the sic raw material of the interior middle part gas-solid state mixing of crucible is 2500 DEG C, the gaseous state of crucible internal upper part
The heating-up temperature of sic raw material is 1900 DEG C.The speed of growth of carborundum crystals can reach more than 0.52mm/h.
Embodiment 12
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The raw material of body high-speed rapid growth, raw material mix the mixed material formed for the carborundum particle being distributed using two kinds of different-grain diameters,
The specifically shape using the carborundum particle of particle diameter distribution as shown in Figure 4 and the carborundum particle mixing of particle diameter distribution as shown in Figure 5
Into mixed material.Wherein, the carborundum particle of particle diameter distribution as shown in Figure 4 and the carbonization silicon grain of particle diameter distribution as shown in Figure 5
The mass ratio of son is 1：1.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of crystal is 0.55mm/
h。
The method that the carborundum particle raw material of the present embodiment prepares carborundum crystals can use conventional method, preferably adopt
Carborundum crystals are prepared using the following method：
According to the needs actually to feed intake, above-mentioned raw materials are put into crucible, and by feeding etching gas from the bottom of crucible
Body (such as chlorine, trichloroacetic acid, trichloro ethylene) makes the raw material carborundum particle in crucible be in floating state, and heating crucible makes earthenware
Recrystallized after raw material distillation in crucible, obtain carborundum crystals, make the heating of the solid silicon carbide particle raw material of bottom in crucible
Temperature is 2300 DEG C, and the heating-up temperature of the sic raw material of middle part gas-solid state mixing is 2500 DEG C in crucible, crucible internal upper part
The heating-up temperature of Gaseous carbonization silicon raw material is 2260 DEG C.The speed of growth of carborundum crystals can reach more than 0.55mm/h.
Embodiment 13
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for carborundum
The raw material of crystal high-speed rapid growth, raw material is mixing is formed jointly using two kinds of different-grain diameters and carborundum particle of different shapes
Mixed material, it is specific to be mixed and shape with carborundum particle as shown in Figure 3 and Figure 5 using carborundum particle as shown in Figure 2 and Figure 4
Into mixed material, make in mixed material carborundum particle as shown in Figure 2 and Figure 4 and carborundum particle as shown in Figure 3 and Figure 5
Mass ratio is 1：0.8.
The raw material of the present embodiment is prepared into carborundum crystals with sublimed method, the speed of growth of crystal is 0.60mm/h.
The method that the raw material of the present embodiment prepares carborundum crystals with the sublimed method of routine is consistent with embodiment 12, here not
Repeat again.
Embodiment 14
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The mixed material that the raw material of body high-speed rapid growth is formed using two kinds of carborundum particle mixing of different shapes, and one of which shape
The average grain diameter of the carborundum particle of shape is 2.0 μm, specially uses specific surface area as 2.0m2/ g and average grain diameter are 2.0 μm
Carborundum particle and specific surface area be 3.0m2The mixed material that/g and particle diameter are formed for 2.5 μm of carborundum particle mixing,
Wherein, specific surface area 2.0m2/ g and average grain diameter are 2.0 μm of carborundum particle and specific surface area is 3.0m2/ g and particle diameter is
The mass ratio of 2.5 μm of carborundum particle is 1：0.5, and both carborundum particles are all using with mechanicalness and physical
The carborundum particle of damage, specifically making carborundum particle, mutually impact forms damage under 250MPa pressure condition.
The raw material of the present embodiment is prepared into carborundum crystals with sublimed method, the speed of growth of crystal is 0.68mm/h.
The method that the raw material of the present embodiment prepares carborundum crystals with the sublimed method of routine is consistent with embodiment 12, here not
Repeat again.
Embodiment 15
The raw material for carborundum crystals high-speed rapid growth of the present embodiment is substantially consistent with embodiment 10, and difference is, mixes
Close in raw material and be also mixed with ramet, and ramet accounts for the 10% of mixed material gross mass.
The raw material of the present embodiment is prepared into carborundum crystals, the speed of growth 0.60mm/h of crystal with the sublimed method of routine.
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 11, no longer superfluous here
State.
Embodiment 16
The raw material for carborundum crystals high-speed rapid growth of the present embodiment is substantially consistent with embodiment 11, and difference is, former
Also it is mixed with magnesia in material, and magnesia accounts for the 5.0% of mixed material gross mass, meanwhile, the particle diameter for making magnesia is 10 μm.
The raw material of the present embodiment is prepared into carborundum crystals, the speed of growth 0.59mm/h of crystal with the sublimed method of routine.
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 12, no longer superfluous here
State.
Embodiment 17
The raw material for carborundum crystals high-speed rapid growth of the present embodiment is substantially consistent with embodiment 12, and difference is, former
Carbon is also mixed with material, and carbon accounts for the 40% of raw material gross mass, and makes the particle diameter of carbon be 15 μm.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of crystal is 0.62mm/
h。
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 5, repeats no more here.
Embodiment 18
The raw material for carborundum crystals high-speed rapid growth of the present embodiment is substantially consistent with embodiment 13, and difference is, former
The mixture of mixed metal powder tungsten and ramet is gone back in material, and the mixture of metal dust tungsten and ramet accounts for raw material gross mass
20%, metal dust tungsten：The mass ratio of ramet is 1：0.5.
The raw material of the present embodiment is prepared into carborundum crystals, the speed of growth 0.72mm/h of crystal with sublimed method.
Embodiment 19
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The mixed material that the raw material of body high-speed rapid growth is formed using three kinds of carborundum particle mixing of different shapes, and wherein three kinds of shapes
The average grain diameter of the carborundum particle of shape is respectively 2.0 μm, 3.0 μm and 10 μm, and average grain diameter is 2.0 μm of carborundum particle
Specific surface area be 2.0m2/ g, average grain diameter are that the specific surface area of 3.0 μm of carborundum particle is 1.5m2/ g, average grain diameter are
The specific surface area of 10 μm of carborundum particle is 0.5m2/ g, wherein, average grain diameter is respectively 2.0 μm, 3.0 μm and 10 μm of carbon
The mass ratio of SiClx particle is 1：0.5：0.2, and both carborundum particles are all using carrying mechanicalness and physical injury
Carborundum particle, specifically make carborundum particle under 250MPa pressure condition mutually impact formed damage.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of crystal is 0.72mm/
h。
It is, of course, also possible to using the carborundum particle mixing of four kinds or more kind different shapes and/different average grain diameters and
The mixed material of formation, it can reach suitable level.
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 14, no longer superfluous here
State.
Embodiment 20
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The mixed material that the raw material of body high-speed rapid growth is formed using the carborundum particle mixing of three kinds of different average grain diameters, and wherein three
The average grain diameter of kind carborundum particle is respectively 1.0 μm, 2.0 μm and 4.0 μm, and average grain diameter is respectively 1.0 μm, 2.0 μm and 4.0
μm carborundum particle mass ratio be 0.3：1：0.1, and carborundum particle is all using carrying mechanicalness and physical injury
Carborundum particle, specifically make carborundum particle under 250MPa pressure condition mutually impact formed damage.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of crystal is 0.67mm/
h。
It is, of course, also possible to using the carborundum particle mixing of four kinds or more kind different shapes and/different average grain diameters and
The mixed material of formation, it can reach suitable level.
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 12, no longer superfluous here
State.
Embodiment 21
Average grain diameter and specific surface area for carborundum particle can be according to selection be actually needed, and this is used for silicon carbide whisker
The mixed material that the raw material of body high-speed rapid growth is formed using two kinds of carborundum particle mixing of different shapes is specific using as schemed
The carborundum particle of the carborundum particle of surface topography shown in 2 and surface topography as shown in Figure 3 is mixed mixed
Close raw material, and make a kind of carborundum particle therein average grain diameter be 3.0 μm, the average grain diameter of another carborundum particle can
So that less than 5 μm, 5 μm can also be more than.Wherein, the carborundum particle of surface topography as shown in Figure 2 and surface as shown in Figure 3
The mass ratio of the carborundum particle of pattern is 1：0.8.
The raw material of the present embodiment is prepared into carborundum crystals, the speed of growth 0.55mm/h of crystal with the sublimed method of routine.
The method that the raw material of the present embodiment prepares carborundum crystals with sublimed method is consistent with embodiment 12, no longer superfluous here
State.
Embodiment 22
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and 2 μm of the average grain diameter of carborundum particle.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.38mm/h.Compared to using existing in general sic raw material come grow the 0.1mm/h of carborundum crystals~
The 0.2mm/h speed of growth, add at least more than 2 times.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals is consistent with embodiment 4, this
In repeat no more.
Embodiment 23
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is all using carborundum particle as raw material, and 3.0 μm of the average grain diameter of carborundum particle, and whole carbon
SiClx particle is the carborundum particle with mechanicalness and/or physical injury.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.42mm/h.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals is consistent with embodiment 4, this
In repeat no more.
Embodiment 24
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is the mixed material of carborundum particle and metal molybdenum, and 2.5 μm of the average grain diameter of carborundum particle and all
Carborundum particle is the carborundum particle with mechanicalness and/or physical injury, and metal molybdenum accounts for the quality percentage of mixed material
Than for 20wt%, and the average grain diameter of metal molybdenum is 10 μm.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.50mm/h.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals is consistent with embodiment 4, this
In repeat no more.
Embodiment 25
The average grain diameter and specific surface area of carborundum particle can be according to selection be actually needed, and it is high that this is used for carborundum crystals
The raw material of fast-growing length is the mixed material of carborundum particle and magnesia, and 4.0 μm of the average grain diameter of carborundum particle, magnesia
The mass percent for accounting for mixed material is 1.0wt%, and the average grain diameter of metal molybdenum is 12 μm.
The raw material of the present embodiment is prepared into carborundum crystals with the sublimed method of routine, the speed of growth of carborundum crystals can
Reach 0.48mm/h.
Certainly, above-mentioned magnesium oxygen can use ramet, charcoal, tantalum, tungsten or zirconium oxide to replace, and be equally reached quite
Effect.
The high-speed rapid growth method that the carborundum particle raw material of the present embodiment prepares carborundum crystals is consistent with embodiment 4, this
In repeat no more.
Specific embodiment described in the present invention is only to spirit explanation for example of the invention.Technology belonging to the present invention
The technical staff in field can make various modifications or supplement to described specific embodiment or using similar mode
Substitute, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.
It is skilled to this area although having been made a detailed description to the present invention and being cited some specific embodiments
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (24)
1. a kind of raw material for carborundum crystals high-speed rapid growth, it is characterised in that the raw material contains carborundum particle, and described
The average grain diameter of carborundum particle is less than 5 μm.
2. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 1, it is characterised in that the carborundum particle
Specific surface area be more than or equal to 0.5m2/g。
3. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 1, it is characterised in that the carborundum particle
In it is some or all be the carborundum particle with mechanicalness and/or physical injury.
4. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 1 or 2 or 3, it is characterised in that the raw material
In be also mixed with the solid matter for not gasifying under the hot conditions below 2400 DEG C or not melting and make to form mixed material；It is described
The solid matter for not gasifying or not melting under less than 2400 DEG C of hot conditions in the sublimation process of the carborundum particle not
It can be sublimated.
5. according to claim 4 be used for carborundum crystals high-speed rapid growth raw material, it is characterised in that it is described 2400 DEG C with
Under hot conditions under do not gasify or the solid matter that does not melt is in tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and magnesia
One or more.
6. according to claim 4 be used for carborundum crystals high-speed rapid growth raw material, it is characterised in that it is described 2400 DEG C with
Under hot conditions under do not gasify or the solid matter that does not melt accounts for 1.0wt%~40wt% of raw material gross mass.
7. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 4, it is characterised in that the solid matter
Average grain diameter is more than the minimum average particle diameters of carborundum particle in raw material.
8. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 6, it is characterised in that the solid matter
Average grain diameter is more than the minimum average particle diameters of carborundum particle in raw material.
9. a kind of raw material for carborundum crystals high-speed rapid growth, it is characterised in that the raw material is using at least two not similar shapes
The mixed material that the carborundum particle of shape and/or at least two different-grain diameters is mixed and formed, and at least contain in the raw material
A kind of average grain diameter is less than 5 μm of carborundum particle.
10. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 9, it is characterised in that the carbonization silicon grain
At least it is more than or equal to 0.5m containing a kind of specific surface area in son2/ g carborundum particle.
11. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 9 or 10, it is characterised in that the mixing
The distribution of shapes of raw material is different.
12. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 9 or 10, it is characterised in that the difference
The carborundum particle of particle diameter is the different carborundum particle of particle size distribution, and in the grading curve of the mixed material
Show the main particle diameter distribution peak value of at least two.
13. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 9 or 10, it is characterised in that the carbonization
It is some or all for using the carborundum particle with mechanicalness and/or physical injury in silicon particle.
14. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 12, it is characterised in that the carbonization silicon grain
Some or all in son are the carborundum particle with mechanicalness and/or physical injury.
15. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 9, it is characterised in that the mixed material
In be also mixed with the solid matter for not gasifying under the hot conditions below 2400 DEG C or not melting；The height below 2400 DEG C
The solid matter for not gasifying or not melting under the conditions of temperature will not be sublimated in the sublimation process of the carborundum particle.
16. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 15, it is characterised in that described at 2400 DEG C
The solid matter for not gasifying or not melting under following hot conditions is selected from tungsten, molybdenum, carbon, tantalum, ramet, zirconium oxide and magnesia
In one or more.
17. it is used for the raw material of carborundum crystals high-speed rapid growth according to claim 15, it is characterised in that described at 2400 DEG C
The solid matter for not gasifying or not melting under following hot conditions accounts for 1.0wt%~40wt% of mixed material gross mass.
18. according to claim 15 or 17 be used for carborundum crystals high-speed rapid growth raw material, it is characterised in that it is described
The solid matter for not gasifying or not melting under less than 2400 DEG C of hot conditions, and the average grain diameter of the solid matter is more than mixed
Close the minimum average particle diameters of carborundum particle in raw material.
A kind of 19. method of carborundum crystals high-speed rapid growth, it is characterised in that this method includes claim 1-18 is any one
The item raw material is put into crucible, and heating crucible makes the raw material in crucible be recrystallized after distilling, and obtains carborundum crystals.
20. the method for carborundum crystals high-speed rapid growth according to claim 19, it is characterised in that also include from the bottom of crucible
Portion feeds the mixture of gas or liquid or both, and it is in floating state to make the raw material in crucible.
21. the method for carborundum crystals high-speed rapid growth according to claim 20, it is characterised in that the gas is selected from current-carrying
One or more of mixing in gas, etching gas, carbon-source gas and silicon source gas.
22. according to the method for carborundum crystals high-speed rapid growth described in claim 19-21 any one, it is characterised in that described
Heating crucible is specially：Heating crucible is carried out using one or more heat sources.
23. according to the method for carborundum crystals high-speed rapid growth described in claim 19-21 any one, it is characterised in that described
Heating crucible is specially：The heating-up temperature for making the solid silicon carbide particle raw material of bottom in crucible is 2100 DEG C~2600 DEG C, is made
The heating-up temperature of middle part gas and/or the sic raw material of solid-state mixing is 2200 DEG C~2800 DEG C in crucible, makes crucible internal upper part
Gaseous carbonization silicon raw material heating-up temperature be 1900 DEG C~2400 DEG C.
24. the method for carborundum crystals high-speed rapid growth according to claim 21, it is characterised in that the current-carrying gas is selected from
One or more in hydrogen, helium and nitrogen；The etching gas is a kind of or several in chlorine, hydrogen chloride and trichloro ethylene
Kind；One or more of the carbon-source gas in methane, ethane and ethene；The silicon source gas is selected from silane gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610018942.1A CN105603530B (en) | 2016-01-12 | 2016-01-12 | For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610018942.1A CN105603530B (en) | 2016-01-12 | 2016-01-12 | For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105603530A CN105603530A (en) | 2016-05-25 |
| CN105603530B true CN105603530B (en) | 2018-02-27 |
Family
ID=55983856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610018942.1A Expired - Fee Related CN105603530B (en) | 2016-01-12 | 2016-01-12 | For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105603530B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108193282B (en) * | 2017-11-14 | 2019-06-25 | 山东天岳先进材料科技有限公司 | A kind of synthetic method and its application of high-purity silicon carbide raw material |
| CN108179470B (en) * | 2017-12-29 | 2021-04-27 | 北京华进创威电子有限公司 | Low-cost aluminum nitride crystal growth method |
| CN113026095A (en) * | 2021-03-15 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309729A (en) * | 1998-07-13 | 2001-08-22 | 西门子公司 | Method for growing SiC monocrystals |
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| JP4048606B2 (en) * | 1998-06-25 | 2008-02-20 | 株式会社デンソー | Single crystal manufacturing method |
| CN102596804A (en) * | 2009-09-15 | 2012-07-18 | Ii-Vi有限公司 | Sublimation growth of sic single crystals |
| CN102597339A (en) * | 2010-04-26 | 2012-07-18 | 住友电气工业株式会社 | Silicon carbide crystal and method for producing silicon carbide crystal |
| CN102958834A (en) * | 2011-05-18 | 2013-03-06 | 住友电气工业株式会社 | Silicon carbide powder and method for producing silicon carbide powder |
| CN103209923A (en) * | 2010-11-15 | 2013-07-17 | 独立行政法人产业技术综合研究所 | Silicon carbide powder for production of silicon carbide single crystal, and method for producing same |
| CN103508454A (en) * | 2012-06-19 | 2014-01-15 | 上海硅酸盐研究所中试基地 | Preparation method of highly pure silicon carbide raw material |
| CN104837767A (en) * | 2012-10-18 | 2015-08-12 | Lg伊诺特有限公司 | Silicon carbide powder, and preparation method therefor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130085841A (en) * | 2012-01-20 | 2013-07-30 | 엘지이노텍 주식회사 | Silicon carbide powder and method for manufacturing the same |
-
2016
- 2016-01-12 CN CN201610018942.1A patent/CN105603530B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4048606B2 (en) * | 1998-06-25 | 2008-02-20 | 株式会社デンソー | Single crystal manufacturing method |
| CN1309729A (en) * | 1998-07-13 | 2001-08-22 | 西门子公司 | Method for growing SiC monocrystals |
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| CN102596804A (en) * | 2009-09-15 | 2012-07-18 | Ii-Vi有限公司 | Sublimation growth of sic single crystals |
| CN102597339A (en) * | 2010-04-26 | 2012-07-18 | 住友电气工业株式会社 | Silicon carbide crystal and method for producing silicon carbide crystal |
| CN103209923A (en) * | 2010-11-15 | 2013-07-17 | 独立行政法人产业技术综合研究所 | Silicon carbide powder for production of silicon carbide single crystal, and method for producing same |
| CN102958834A (en) * | 2011-05-18 | 2013-03-06 | 住友电气工业株式会社 | Silicon carbide powder and method for producing silicon carbide powder |
| CN103508454A (en) * | 2012-06-19 | 2014-01-15 | 上海硅酸盐研究所中试基地 | Preparation method of highly pure silicon carbide raw material |
| CN104837767A (en) * | 2012-10-18 | 2015-08-12 | Lg伊诺特有限公司 | Silicon carbide powder, and preparation method therefor |
Non-Patent Citations (1)
| Title |
|---|
| 原料对碳化硅单晶生长的影响;陈之战,等;《无机材料学报》;20030731;第18卷(第4期);第737-743页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105603530A (en) | 2016-05-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TW552325B (en) | Method and apparatus for growing silicon carbide crystals | |
| CN1324168C (en) | Method for preparing sic crystal and SiC crystal | |
| CN1284887C (en) | Method of making sic single crystal and apparatus for making sic single crystal | |
| CN105603530B (en) | For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals | |
| JP5657109B2 (en) | Semi-insulating silicon carbide single crystal and growth method thereof | |
| CN105209671B (en) | Vanadium doping SiC single crystal and its method | |
| CN102732953B (en) | Technology and apparatus for growing single silicon carbide crystals through double seed crystal-assisted vapor transport method | |
| JP2650064B2 (en) | Polycrystalline silicon capable of producing long-lived single-crystal silicon | |
| US9328413B2 (en) | Method for preparing graphene nanoribbon on insulating substrate | |
| CN105525352A (en) | Device and method for high-speed production of silicon carbide crystals by adopting sublimation method | |
| CN110983434B (en) | Growth method for effectively reducing defects of silicon carbide single crystal and high-quality silicon carbide single crystal | |
| CN1663911A (en) | Dust-free and pore-free, high-purity granulated polysilicon | |
| KR20150123114A (en) | Preparing method of silicon carbide powder | |
| CN1227395C (en) | Silicom wafer and method for producing silicon wafer crystal | |
| JP4819069B2 (en) | Method for producing silicon carbide single crystal | |
| CN101040068A (en) | Single-crystal production apparatus | |
| US6797060B2 (en) | Method and apparatus for producing silicon carbide single crystal | |
| CN103403231B (en) | The manufacture method of n type single crystal silicon and mix phosphorus n type single crystal silicon | |
| CN112010311B (en) | Method for treating prefabricated material for high-purity silicon carbide powder | |
| US20220144711A1 (en) | High purity ingot for wafer production | |
| JP2005320203A (en) | Method for manufacturing silicon single crystal, and silicon single crystal | |
| JPH02164711A (en) | Manufacture of high-purity boron | |
| CN111575801B (en) | Preparation method and wafer growth raw material | |
| JPS62501497A (en) | Single crystal silicon ingot drawn continuously | |
| CN1207448C (en) | Method of increasing oxygen content in vertical pulling silicon single crystal rod and automatic aerator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200122 Address after: West of 4th floor, building 3, No. 818, east section of development avenue, Taizhou City, Zhejiang Province Patentee after: Taizhou Yineng Science & Technology Co., Ltd. Address before: 318000, Zhejiang, Taizhou Province, 818 Eastern Road Development Avenue, 3, west side of the 4 Co-patentee before: Hoshino Masahiro Patentee before: Taizhou Yineng Science & Technology Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180227 Termination date: 20210112 |