CN109722711A - A kind of the SiC growing method and device of regulation doping concentration - Google Patents
A kind of the SiC growing method and device of regulation doping concentration Download PDFInfo
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- CN109722711A CN109722711A CN201711024669.4A CN201711024669A CN109722711A CN 109722711 A CN109722711 A CN 109722711A CN 201711024669 A CN201711024669 A CN 201711024669A CN 109722711 A CN109722711 A CN 109722711A
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Abstract
The present invention provides the SiC growing method and device of a kind of controllable doping concentration, and wherein growing method is the following steps are included: provide a crucible;The source SiC is put into crucible;SiC seed crystal is fixed on crucible;Heating crucible establishes a main thermal gradient between SiC seed crystal and the source SiC, and the gas for promoting the source SiC to distil is transmitted to SiC seed crystal to grow SiC crystal on SiC seed crystal;It is passed through impurity gas, SiC crystal is doped when growing SiC crystal;The doping concentration for the SiC crystal that system monitoring is growing, and the flow for the impurity gas being passed through according to the doping concentration control monitored are monitored using light wave;When fixed SiC seed crystal, the macroscopic growth surface of SiC seed crystal is made to form an acute angle relative to main thermal gradient.The accurate control adulterated to SiC crystal may be implemented using the method for the present invention and device, obtain high quality, low defect, the accurate SiC crystal of doping concentration.
Description
Technical field
The present invention relates to technical field of semiconductors, a kind of SiC growing method more particularly to controllable doping concentration and
Device.
Background technique
As a kind of novel semiconductor material, silicon carbide (SiC) with its excellent physicochemical characteristics and electrical characteristics at
For manufacture short-wavelength light electronic device, high-temperature device, Flouride-resistani acid phesphatase device and high-power, the most important semiconductor of great number electronic device
Material.In application, the characteristic of SiC device is considerably beyond Si device and GaAs device especially under extreme condition and mal-condition
Part.Therefore, SiC device gradually becomes one of Primary Component, plays increasingly important role.
Under regular industrial working condition, the growing method of SiC crystal usually has chemical vapour deposition technique, liquid phase epitaxial method
And sublimed method.Sublimed method is the current growth a kind of most common method of SiC crystal, and this method is used as guidance using seed crystal, one
In a closed growing system, heating powder is allowed to distil, then recrystallizes at seed crystal.Publication No. P2008-
The Japanese documentation of 509872A proposes a kind of off-axis (off-axis) sublimed method, is tilted using the seed holder of wedge shape
Fixed SiC seed crystal makes seed crystal face and horizontal plane at certain inclination angle, i.e. deviation thermal gradient direction.With seed crystal face perpendicular to heat
The conventional sublimation method of gradient direction is compared, and this method makes surface step of the seed crystal with more highdensity per unit area, this
A little surface steps play nucleation, promote the nucleation and growth of high quality silicon carbide.This method can provide good knot
Structure stability stablizes growth after nucleation, avoids division deficient, and advantageously reduce thermal stress in growth period or cooling procedure and lead
The SiC crystal basal plane dislocation of cause.
For the growth of SiC crystal, powder injection molding is most important.In practical application, N doping is generallyd use to adjust
The resistance of SiC crystal is controlled, however excessive introduce of nitrogen also will lead to crystal defect.It is few due to containing in silicon raw material and graphite crucible
The nitrogen of amount, in SiC growth, the nitrogen in these production backgrounds can be introduced into SiC crystal, in addition carrying out for regulating and controlling resistance
N doping often makes the introducing of nitrogen excessive, causes crystal defect.The Japanese documentation of Publication No. P2015-3850A
It is proposed the depth analysis that impurity is carried out using Secondary Ion Mass Spectrometry (Secondary Ion Mass Spectroscopy, SIMS),
The nitrogen concentration in the SiC crystal for not carrying out N doping is measured, obtains the background nitrogen concentration from raw material and crucible with this.From
And the flow of N doping can be controlled in view of this background nitrogen concentration when SiC crystal is grown.However the back of this method measurement
Although scape nitrogen concentration can be used as the reference of N doping flow control, but do not ensure that the accuracy of nitrogen doped concentration.In order to
Avoid the excessive of nitrogen from introducing, reduce SiC crystal defect, it is really necessary to provide it is a kind of can accuracy controlling doping concentration SiC growth
Method and device.
Summary of the invention
In view of prior art described above, the purpose of the present invention is to provide a kind of growth sides SiC of regulation doping concentration
Method and device lead to SiC crystal defect since doping is excessive in the prior art for solving the problems, such as.
In order to achieve the above objects and other related objects, the present invention provides a kind of SiC growing method of regulation doping concentration,
The following steps are included:
One crucible is provided;
The source SiC is put into the crucible;
SiC seed crystal is fixed on the crucible;
The crucible is heated, a main thermal gradient is established between the SiC seed crystal and the source SiC, is promoted described
The gas of the source SiC distillation is transmitted to the SiC seed crystal to grow SiC crystal on the SiC seed crystal using sublimed method;
It is passed through impurity gas, the SiC crystal is doped when growing the SiC crystal;
Using the doping concentration for the SiC crystal that light wave monitoring system monitoring is growing, and mixed according to what is monitored
The gas flow for the impurity gas that miscellaneous concentration control is passed through;
Wherein, when the fixed SiC seed crystal, make the macroscopic growth surface of the SiC seed crystal relative to the main heat ladder
Degree forms an acute angle θ 1.
Optionally, the crucible uses graphite crucible.
Optionally, the source SiC uses SiC particulate raw material.
Optionally, the impurity gas includes one of gas containing N, gas containing Al and gas containing B.
Optionally, the impurity gas is after the gas mixing of the bottom of the crucible or the distillation of middle part and the source SiC
It is transported to the SiC seed crystal face.
Optionally, the light wave monitoring system is growing described using the monitoring of ftir analysis method
The doping concentration of SiC crystal.
Optionally, the acute angle θ 1 is 70-89 degree.
In order to achieve the above objects and other related objects, the present invention also provides a kind of SiC of regulation doping concentration to grow dress
It sets, comprising:
Crucible;
The source SiC is placed in the crucible;
Seed holder is set to the crucible top;
SiC seed crystal is fixed in the seed holder;
Main thermal gradient is formed in the crucible, is directed toward the crucible top by the crucible bottom, is promoted described
The sublimation gases in the source SiC are transmitted to the SiC seed crystal, and the seed holder makes the macroscopic growth surface of the SiC seed crystal
An acute angle θ 1 is formed relative to the main thermal gradient;
Transparent pipe is set in the seed holder and passes through the seed holder until the SiC seed crystal face;
Light wave monitors system, is set to the top of the crucible top, detects the light wave across the transparent pipe, with monitoring
The doping concentration of SiC crystal is grown on the SiC seed crystal.
Optionally, the crucible is graphite crucible, including a graphite base and is upwardly extended along the graphite base edge
Graphite side wall pipe.
Optionally, the source SiC is SiC particulate raw material.
Optionally, the acute angle θ 1 is 70-89 degree.
Optionally, the seed holder is equipped with a seed crystal stationary plane, and the SiC seed crystal is fixed on the seed crystal stationary plane
On, keep the macroscopic growth surface of the SiC seed crystal parallel with the seed crystal stationary plane, and the seed crystal stationary plane is relative to level
Face forms an acute angle θ 2.
Still optionally further, the acute angle θ 2 is 1-20 degree.
Optionally, the seed holder is set up in the side wall upper limb of the crucible, covers the crucible top.
Optionally, the transparent pipe is sapphire glass pipe.
Optionally, the light wave monitoring system monitors the SiC crystal using ftir analysis method
Doping concentration.
Optionally, gas access is equipped on the side wall of the crucible, for being passed through impurity gas and protective gas.
Still optionally further, the impurity gas includes one of gas containing N, gas containing Al and gas containing B.
Still optionally further, the protective gas is argon gas.
Optionally, the SiC grower of the regulation doping concentration further includes doping concentration control system and gas flow
Controller;The doping concentration control system is connect with light wave monitoring system, obtains the monitoring of the light wave monitoring system
Data, control the gas flow controller according to the doping concentration of the SiC crystal of growth, are passed through the crucible with control
Dopant gas flow;The gas flow controller controls corresponding doping according to the instruction of the doping concentration control system
The flow of gas.
Optionally, the diameter of the SiC seed crystal is 100mm, 150mm or 200mm.
As described above, the SiC growing method and device of regulation doping concentration of the invention, have the advantages that
The present invention tilts fixed SiC seed crystal using seed holder, grows SiC crystal using off-axis sublimation method, can get
Good SiC crystal structural stability stablizes growth after nucleation, avoids division deficient, and advantageously reduce growth period or cold
But SiC crystal basal plane dislocation caused by thermal stress during.Meanwhile the present invention is configured with light wave monitoring system, using Fourier
The doping concentration of transform infrared spectroscopy analytic approach real-time monitoring SiC crystal realizes the accurate control to SiC crystal doping with this
System avoids the problems such as adulterating excess and thus caused crystal defect.Therefore, it can be obtained using the method for the present invention and device
The accurate SiC crystal of high quality, low defect, doping concentration.
Detailed description of the invention
Fig. 1 is shown as the SiC growing method schematic diagram of regulation doping concentration provided in an embodiment of the present invention.
Fig. 2 is shown as the SiC grower schematic diagram of regulation doping concentration provided in an embodiment of the present invention.
Component label instructions
100 crucibles
101 graphite bases
102 graphite side wall pipes
103 protective layers
104 quartz socket tubes
105 load coils
106 gas accesses
200 sources SiC
300 seed holders
301 seed crystal stationary planes
400 SiC seed crystals
401 macroscopic growth surfaces
500 transparent pipes
600 light waves monitor system gas
700 doping concentration control systems
800 gas flow controllers
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.It should be noted that in the absence of conflict, following embodiment and implementation
Feature in example can be combined with each other.
It should be noted that illustrating the basic structure that only the invention is illustrated in a schematic way provided in following embodiment
Think, only shown in schema then with related component in the present invention rather than component count, shape and size when according to actual implementation
Draw, when actual implementation kenel, quantity and the ratio of each component can arbitrarily change for one kind, and its assembly layout kenel
It is likely more complexity.
In order to avoid doping is excessive, SiC crystal defect is reduced, present embodiments provides a kind of SiC of regulation doping concentration
Growing method, comprising the following steps:
S1 provides a crucible.Wherein, the crucible can use graphite crucible.
The source SiC is put into the crucible by S2.Wherein, the source SiC can use SiC particulate raw material, such as SiC powder
Deng.
SiC seed crystal is fixed on the crucible by S3.The SiC seed crystal can select diameter be 100mm, 150mm or
The concrete shape size present invention of 200mm equidimension, the SiC seed crystal is not particularly limited, and can be chosen according to practical application.
S4 heats the crucible, and a main thermal gradient is established between the SiC seed crystal and the source SiC, promotes institute
The gas for stating the distillation of the source SiC is transmitted to the SiC seed crystal to grow SiC crystal on the SiC seed crystal using sublimed method.Its
In, when fixing the SiC seed crystal, keep the macroscopic growth surface of the SiC seed crystal sharp relative to the main thermal gradient formation one
Angle angle theta 1, i.e., the macroscopic growth surface of the described SiC seed crystal does not face and (is not orthogonal to) the main thermal gradient, but is formed
Certain off-axis angle.The mode of this fixed seed crystal of inclination can promote the nucleation and growth of high quality silicon carbide, obtain
Good structural stability is obtained, SiC crystal basal plane dislocation caused by thermal stress in growth period or cooling procedure is advantageously reduced.Tool
Body, the acute angle θ 1 is 70-89 degree.
Specifically, heating crucible can be conducive to control the thermal field and the SiC in crucible by the way of induction heating
Thermal gradient between seed crystal and the source SiC.
S5 is passed through impurity gas, is doped when growing the SiC crystal to the SiC crystal.Preferably, gas is adulterated
Body is transported to SiC seed crystal face after the bottom of the crucible or middle part mix with the sublimation gases in the source SiC, to can be obtained
The SiC crystal of even doping.Specifically, according to the needs actually adulterated, the impurity gas can be gas containing N, gas containing Al
Or gas containing B, for example, it may be NH3、N2、N2H2, TMA (trimethyl aluminium), B2H6Deng.It needs to carry out N in the present embodiment to mix
Miscellaneous, then the impurity gas can select NH3、N2、N2H2。
The doping concentration of the SiC crystal that S6 is growing using light wave monitoring system monitoring, and according to monitoring
The gas flow for the impurity gas that doping concentration control is passed through.Specifically, the light wave monitoring system is become using Fourier
Change the doping concentration for the SiC crystal that infrared spectroscopy (FT-IR) monitoring is growing.According to the doping of real-time monitoring
Concentration adjusts the flow for the impurity gas being passed through to control, so as to accurately obtain required doping concentration.
For the ease of realizing above-mentioned manufacture craft, the present embodiment additionally provides a kind of SiC growth dress of regulation doping concentration
It sets, referring to Fig. 2, the device mainly includes: crucible 100, the source SiC 200, seed holder 300, SiC seed crystal 400, transparent pipe
500 and light wave monitor system 600.
Wherein, the crucible 100 uses graphite crucible, for example, the crucible 100 can using it is high-purity, high-densit, respectively to
The graphite material of the same sex is made.Specifically, the crucible 100 may include a graphite base 101 and along the graphite base 101
The graphite side wall pipe 102 that edge upwardly extends.For the ease of the thermal field and temperature gradient in control crucible 100, crucible 100 is heated
It can be by the way of induction heating.In the present embodiment, protective layer 103 is provided with outside the crucible 100, outside protective layer 103
It is provided with quartz socket tube 104,104 outer wall of quartz socket tube is coupled with load coil 105.In addition, can be on crucible 100
Temperature controller (not shown) is set in order to carry out the therm-param method of crucible 100.
The source SiC 200 is placed in the crucible 100.The source SiC 200 can use SiC particulate raw material, such as SiC
Powder etc..As shown in Fig. 2, the source SiC 200 is mainly placed in 100 bottom of crucible, in the present embodiment, the crucible
Also some sources SiC 200 are attached on 100 side wall.
The seed holder 300 is set to 100 top of crucible.The SiC seed crystal 400, is fixed on the seed crystal
On fixator 300.A main thermal gradient is formed in the crucible 100, as shown in the solid arrow in Fig. 2.It is described main
Thermal gradient is directed toward 100 top of the crucible by 100 bottom of crucible, promotes the sublimation gases in the source SiC 200 to described
SiC seed crystal 400 transmits, and the seed holder 300 makes the macroscopic growth surface 401 of the SiC seed crystal 400 relative to described
Main thermal gradient forms an acute angle θ 1.Specifically, the acute angle θ 1 is 70-89 degree.
Wherein, the main thermal gradient is formed by heating the crucible 100.And use the seed holder 300
The fixed SiC seed crystal 400 of inclination, may be implemented to grow SiC crystal on the SiC seed crystal 400 with off-axis sublimation method.
As a preferred embodiment, the seed holder 300 is wedge shaped, and is equipped with an inclined seed crystal stationary plane
301, the SiC seed crystal 400 is fixed on the seed crystal stationary plane 301, makes the macroscopic growth surface 401 of the SiC seed crystal 400
It is parallel with the seed crystal stationary plane 301, and the seed crystal stationary plane 301 with respect to the horizontal plane forms an acute angle θ 2, such as Fig. 2
Shown in.Specifically, the acute angle θ 2 is 1-20 degree.
Preferably, the seed holder 300 can be set up in the side wall upper limb of the crucible 100 to the present embodiment, similar
One crucible lid covers 100 top of crucible.
Specifically, it is 100mm, 150mm or 200mm equidimension, the SiC seed that the SiC seed crystal 400, which can select diameter,
The concrete shape size present invention of crystalline substance 400 is not particularly limited, and can be chosen according to practical application.
The transparent pipe 500 is set in the seed holder 300 and passes through the seed holder 300 until described
400 surface of SiC seed crystal.Described 500 one end of transparent pipe is directed at the detection window of the light wave monitoring system 600, other end alignment
400 surface of SiC seed crystal.In the present embodiment, the transparent pipe 500 can use sapphire glass pipe.
The light wave monitoring system 600 is set to the top at 100 top of crucible, detects across the transparent pipe 500
Light wave, with monitor on the SiC seed crystal 400 grow SiC crystal doping concentration.Specifically, the light wave monitors system 600
The doping concentration of the SiC crystal is monitored using ftir analysis method.
In the present embodiment, gas access 106 is equipped on the side wall of the crucible 100, for being passed through impurity gas and guarantor
Gas is protected, as indicated by arrows with dashed lines in figure 2.Sublimation gases with the source SiC after impurity gas is passed through crucible from gas access 106
It in crucible bottom or intermediate mixing, then is transported at SiC seed crystal, so that the SiC crystal of Uniform Doped can be obtained.Wherein, root
The factually needs of border doping, the impurity gas can be gas containing N, gas containing Al or gas containing B, for example, it may be NH3、
N2、N2H2, TMA (trimethyl aluminium), B2H6Deng.It needs to carry out N doping in the present embodiment, then the impurity gas can be selected
NH3、N2、N2H2.The protective gas can use argon gas.Argon gas can be used to regulate and control the air pressure in crucible 100, also can be used as
Carrier gas promotes the transport of the source SiC sublimation gases.
As a preferred embodiment, the SiC grower of the regulation doping concentration can also include doping concentration
Control system 700 and gas flow controller 800.The doping concentration control system 700 connects with light wave monitoring system 600
It connects, the monitoring data of the light wave monitoring system 600 is obtained, according to the control of the doping concentration of the SiC crystal of growth
Gas flow controller 800, to control the flow for the impurity gas for being passed through the crucible 100.The gas flow controller 800
According to the instruction of the doping concentration control system 700, the uninterrupted of corresponding impurity gas is adjusted.The present embodiment passes through described
The doping concentration of SiC crystal that light wave monitoring 600 real-time monitoring of system is grown, and by doping concentration control system 700 and
Gas flow controller 800 can realize the automatic control to SiC crystal doping.
In conclusion the present invention tilts fixed SiC seed crystal using seed holder, it is brilliant using off-axis sublimation method growth SiC
Body can get good SiC crystal structural stability, stablize growth after nucleation, avoid division deficient, and advantageously reduce life
SiC crystal basal plane dislocation caused by thermal stress in long-term or cooling procedure.Meanwhile the present invention is configured with light wave monitoring system, adopts
With the doping concentration of ftir analysis method monitoring SiC crystal, realized with this to the accurate of SiC crystal doping
Control avoids the problems such as adulterating excess and thus caused crystal defect.Therefore, it can be obtained using the method for the present invention and device
Obtain high quality, low defect, the accurate SiC crystal of doping concentration.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (20)
1. a kind of SiC growing method of regulation doping concentration, which is characterized in that the described method comprises the following steps:
One crucible is provided;
The source SiC is put into the crucible;
SiC seed crystal is fixed on the crucible;
The crucible is heated, a main thermal gradient is established between the SiC seed crystal and the source SiC, promotes the source SiC
The gas of distillation is transmitted to the SiC seed crystal to grow SiC crystal on the SiC seed crystal using sublimed method;
It is passed through impurity gas, the SiC crystal is doped when growing the SiC crystal;
The doping concentration for the SiC crystal that system monitoring is growing is monitored using light wave, and dense according to the doping monitored
The gas flow for the impurity gas that degree control is passed through;
Wherein, when the fixed SiC seed crystal, make the macroscopic growth surface of the SiC seed crystal relative to the main thermal gradient shape
Angle theta 1 in an acute angle.
2. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: the crucible uses stone
Black crucible.
3. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: the source SiC uses
SiC particulate raw material.
4. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: the impurity gas packet
Include one of gas containing N, gas containing Al and gas containing B.
5. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: the impurity gas exists
The SiC seed crystal face is transported to after the gas mixing of the bottom or middle part of the crucible and the source SiC distillation.
6. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: light wave monitoring system
The doping concentration for the SiC crystal that system is growing using the monitoring of ftir analysis method.
7. the SiC growing method of regulation doping concentration according to claim 1, it is characterised in that: the acute angle θ 1
For 70-89 degree.
8. a kind of SiC grower of regulation doping concentration characterized by comprising
Crucible;
The source SiC is placed in the crucible;
Seed holder is set to the crucible top;
SiC seed crystal is fixed in the seed holder;
Main thermal gradient is formed in the crucible, is directed toward the crucible top by the crucible bottom, is promoted the source SiC
Sublimation gases transmitted to the SiC seed crystal, and the seed holder make the macroscopic growth surface of the SiC seed crystal relative to
The main thermal gradient forms an acute angle θ 1;
Transparent pipe is set in the seed holder and passes through the seed holder until the SiC seed crystal face;
Light wave monitors system, is set to the top of the crucible top, detects the light wave across the transparent pipe, described in monitoring
The doping concentration of SiC crystal is grown on SiC seed crystal.
9. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the crucible is graphite
Crucible, including a graphite base and the graphite side wall pipe upwardly extended along the graphite base edge.
10. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the source SiC is SiC
Particulate material.
11. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the acute angle θ 1
For 70-89 degree.
12. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the seed holder
Equipped with a seed crystal stationary plane, the SiC seed crystal is fixed on the seed crystal stationary plane, makes the macroscopic growth table of the SiC seed crystal
Face is parallel with the seed crystal stationary plane, and the seed crystal stationary plane with respect to the horizontal plane forms an acute angle θ 2.
13. the SiC grower of regulation doping concentration according to claim 12, it is characterised in that: the acute angle θ
2 be 1-20 degree.
14. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the seed holder
It is set up in the side wall upper limb of the crucible, covers the crucible top.
15. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the transparent pipe is indigo plant
Cameo glass pipe.
16. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: light wave monitoring system
System monitors the doping concentration of the SiC crystal using ftir analysis method.
17. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: in the side of the crucible
Wall is equipped with gas access, for being passed through impurity gas and protective gas.
18. the SiC grower of regulation doping concentration according to claim 17, it is characterised in that: the impurity gas
Including one of gas containing N, gas containing Al and gas containing B, the protective gas is argon gas.
19. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the regulation doping is dense
The SiC grower of degree further includes doping concentration control system and gas flow controller;The doping concentration control system with
The light wave monitoring system connection, obtains the monitoring data of the light wave monitoring system, according to mixing for the SiC crystal of growth
Miscellaneous concentration controls the gas flow controller, to control the dopant gas flow for being passed through the crucible;The gas flow control
Device processed controls the flow of corresponding impurity gas according to the instruction of the doping concentration control system.
20. the SiC grower of regulation doping concentration according to claim 8, it is characterised in that: the SiC seed crystal
Diameter is 100mm, 150mm or 200mm.
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CN111270305A (en) * | 2020-03-30 | 2020-06-12 | 山东天岳先进材料科技有限公司 | High-quality n-type silicon carbide and preparation method thereof |
CN117166044A (en) * | 2022-06-02 | 2023-12-05 | 株式会社力森诺科 | SiC substrate and SiC ingot |
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