CN106048713B - A kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height - Google Patents
A kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height Download PDFInfo
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- CN106048713B CN106048713B CN201610482560.4A CN201610482560A CN106048713B CN 106048713 B CN106048713 B CN 106048713B CN 201610482560 A CN201610482560 A CN 201610482560A CN 106048713 B CN106048713 B CN 106048713B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
-
- 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
Abstract
The present invention relates to silicon carbide solwution method fields, more particularly to a kind of method for monitoring liquid level contact height in silicon carbide solwution method in real time, employ high precision galvanometer, judge whether SiC seed crystals contact with the melting liquid level in graphite crucible by the deflection of pointer, the specific height that SiC seed crystals contact with molten liquid is extrapolated according to the exact numerical values recited that galvanometer is shown, ensure the accuracy of crystal growth experiment, contact the real-time controllable of liquid level, intuitively and effectively obtain the purpose that seed crystal contacts liquid level, in addition the controllable growth of SiC crystal has also been advantageously promoted to a certain extent.In addition this process avoids molten liquid and extraneous atmosphere convection current without manually taking observation, avoid observation take long, working hour is long, the lag drawbacks such as not in time, solve this problem present in solwution method, more conducively produce high-quality monocrystal SiC material.
Description
Technical field
The invention belongs to monitor and adjust in real time in silicon carbide solwution method technical field more particularly to a kind of silicon carbide solwution method
The method of solidating liquid interfacial level.
Background technology
Silicon carbide（SiC）Compare silicon（Si）Band gap with bigger, SiC single crystal has excellent physical property, quite high
Thermal stability and chemical stability, radioresistance line is strong, mechanical strength, than Si have higher breakdown voltage and thermal conductivity
Deng.As the semi-conducting material of a new generation, researcher is constantly promoting the desired value of high-quality monocrystal SiC.
For semi-conducting material about all high quality including SiC crystal, there are two basic demands：First, crystal
The defects of containing lacking as far as possible；Second, impurity concentration present in crystal is low as far as possible.
At present it is known that SiC single crystal representative growing method be vapor phase method and solwution method.In vapor phase method,
The method generally used at present is still that sublimed method places SiC raw material powders i.e. in graphite crucible, and SiC seeds are configured in crucible top
Crystalline substance heats crucible under the atmosphere of inert gas the operation for carrying out crystal growth.SiC single crystal is prepared using sublimed method, although
Crystal growth rate is fast, but containing more micro-pipe and has a large amount of crystal defect, while growth course in crystal obtained by growth
In have the interference of many silicon carbide polytypes structures, the above problem directly affects the quality of SiC single crystal.On the contrary, although solwution method is brilliant
Body growth rate is slow, but due to it does not have disadvantages mentioned above and is causing researcher concern.In solwution method, in the future
It is dissolved in melt of si from the C of graphite crucible, forms molten liquid.End is placed on above-mentioned melting liquid level and is fixed with SiC seed crystals
Graphite rod, by with melting liquid level contact, crystallize in the SiC seed crystals Epitaxial Growing of arrangement and to form SiC single crystal.It should
Inevitable micro-pipe problem present in sublimed method does not occur for method, and less generation crystal is many types of, can obtain good crystallinity
High quality SiC single crystal can meet semi-conducting material necessary requirement.
In the process of solution growth SiC crystal, need SiC seed crystals being immersed in above-mentioned molten liquid so that seed crystal
It is nearby subcooled and is in hypersaturated state so that SiC single crystal epitaxial growth on the seed crystal.The crystal is in the growth process phase
Between internal system must not be made to be exposed in air, if at this time seed crystal be detached from melting liquid level interrupt the crystal being growing, interrupt
Crystal growth causes seed crystal to be contacted with molten liquid and unstable crystal is formd on seed crystal, may cause crystal Polytype Transformation
State.
The driving force of crystal growth is from the temperature gradient of the solid liquid interface between crystal and liquid level.Along with crystal
Growth, since solute enters crystal and can volatilize to a certain degree, leads to the reduction of liquid level.If it is unable to real-time monitoring
The height of solid liquid interface can lead to the variation of the temperature gradient of solid liquid interface, and then cause the variation of crystal growth rate.If
Temperature gradient is excessive, it may appear that the problem of plane of crystal is coarse generates inclusion enclave, polycrystalline and the defects of crystal boundary.
Therefore, how to judge whether seed crystal touches the height of melting liquid level and monitoring contact in real time and adjust solid-liquid circle
Face is highly particularly important.
Invention content
The present invention provides for solution existing issue and monitors and adjust solid liquid interface height in a kind of silicon carbide solwution method in real time
The method of degree employs a kind of high precision electro flowmeter and the sensing device of current loop is formed with crystal growth system, thus real
It can now judge whether SiC seed crystals contact with melting liquid level in time, while monitor what SiC seed crystals were contacted with melting liquid level in real time again
Highly, then by PID feedback loop, the height of solid liquid interface is automatically adjusted, whole process is without manually time-consuming observation and manually
Adjusting, avoid molten liquid and extraneous atmosphere convection current, while also avoid the error that manual adjustment is brought, solve solwution method
Present in this problem.
To realize the purpose of foregoing invention, specific technical solution scheme of the present invention is as follows：
A kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height, using a kind of high precision electricity
Flowmeter and the sensing device that current loop is formed with crystal growth system, then automatically adjust solid-liquid by PID feedback loop again
The height at interface；
The sensing device structure is as follows：
Including grower, crucible axis and high precision galvanometer, the grower include accommodating molten liquid
Graphite crucible and the seed shaft inside graphite crucible can be stretched into；The lower end of the seed shaft is SiC seed crystal substrates；Described
Heat-insulating material is enclosed on the outside of graphite crucible；The graphite crucible bottom, which is provided with, is used to support its crucible axis；It is described
Crucible axis and seed shaft between be electrically connected by high precision galvanometer；Wherein conducting wire anode connection seed shaft, conducting wire cathode
Connect crucible axis；The seed shaft is graphite material；
The graphite crucible, for the solution after storing raw material polysilicon and fusing；Graphite crucible is both to hold solution
Container, and provide carbon source for crystal growth.The Si of melting is formed after unmelted polycrystalline silicon, corrodes graphite crucible, it is molten to form SiC
Liquid.
The method for monitoring liquid level contact height in the silicon carbide solwution method in real time, the specific steps are：It can be with during use
Seed shaft is stretched into inside graphite crucible, polysilicon is put into graphite crucible, is passed through inert gas after closing graphite crucible, so
Set device temperature afterwards, and keep heating graphite crucible, the temperature of crucible is risen to more than raw material fusing point, forms melting
Silicon；By corrosion of the solution to graphite crucible, SiC molten liquids are formed, then SiC seed crystals are immersed in the SiC solution,
The solution near seed crystal is at least made to be in supercooled state, the hypersaturated state for the SiC being consequently formed makes SiC single crystal on seed crystal
Growth.The SiC seed crystals are fixed on rotatable seed shaft, SiC seed crystals are driven to rotate by this seed shaft, fixing axle
The seed crystal of end is contacted with by the way that C to be dissolved in the molten liquid surface containing Si, opens current loop switch, in operation seed rod contact
The pointer variation of high precision galvanometer is paid close attention to during liquid level, according to.Before not contacting, pointer is stationary；It is contacted in seed crystal
Melt liquid level moment, galvanometer deflection；As seed crystal contacts with molten liquid contact surface deeper, the reading of galvanometer is higher, therewith
It is directly proportional, seed crystal is extrapolated according to the height and the standard curve of electric current registration that are contacted according to seed crystal with molten liquid and is connect with molten liquid
Tactile height.Then according to the growth demand of crystal, by the backfeed loop of PID, seed is driven by the motor above seed shaft
Crystallographic axis moves up and down, and dynamic adjusts the position of seed shaft, it is ensured that solid liquid interface keeps the numerical value stablized, so that it is guaranteed that crystal
The stationarity of growth.
It is as follows that the standard curve obtains step：
A. seed crystal contact liquid level of solution, writes down high precision galvanometer registration.
B. after growing 1 hour, solution evaporation speed is more than long brilliant speed, liquid level is caused to reduce, solid liquid interface height increases
Greatly, high precision galvanometer registration at this time is write down.
C. after growing 2 hours, solid liquid interface height continues to increase, and writes down high precision galvanometer registration at this time.
D., until crystal growth terminates, the variation of high precision galvanometer registration is recorded always.Grown junction
Shu Hou, the solution height of measurement remnant, obtaining liquid level of solution reduces speed, can obtain the solid-liquid in crystal growth certain time period
Interfacial level, i.e. can obtain galvanometer registration and the correspondence of solid liquid interface height can draw standard curve in this way.
The height that the current loop is contacted with seed crystal with molten liquid can principle existing for correspondence：
Resistance is several by solution and graphite crucible etc. in seed shaft, the solution of solid liquid interface, crucible in the current loop
Sections in series forms, and wherein seed shaft and graphite crucible are fixed resistance, and solution is can power transformation in solid liquid interface solution and crucible
Resistance.
The calculation formula of wherein resistance is：R=ρ L/S wherein R are resistance, S is sectional area, L is length, ρ is resistivity.
According to the calculation formula of resistance, resistance is inversely proportional with sectional area, directly proportional with length.When liquid level changes
When, sectional area does not change, and resistivity does not change, the only length of variation.So the height when solid liquid interface changes
When, resistance can change, so as to react in the registration variation of rheometer.When solid liquid interface increases, resistance increases, electric current
Meter registration becomes smaller, and when solid liquid interface reduces, resistance reduces, and galvanometer registration becomes larger.
The present invention also protects a kind of sensing device structure as follows：
Including grower, crucible axis and high precision galvanometer, the grower include accommodating molten liquid
Graphite crucible and the seed shaft inside graphite crucible can be stretched into；The lower end of the seed shaft is SiC seed crystal substrates；Described
Heat-insulating material is enclosed on the outside of graphite crucible；The graphite crucible bottom, which is provided with, is used to support its crucible axis；It is described
Crucible axis and grower between be electrically connected by high precision galvanometer；Wherein conducting wire anode connection seed shaft, conducting wire are born
Pole connects crucible axis；The seed shaft is graphite material.
Using device and method provided by the invention, it can directly adjust and join according to the method for existing solution growth SiC crystal
Number is produced, such as mode of heating, heating time, growth atmosphere, heating rate and cooldown rate, and inventor is no longer superfluous herein
It states.
Heretofore described PID feedback loop is the prior art.
In conclusion using the present invention, without taking time to observe the contact condition of graphite rod and silicon melt constantly, also without
Growing system need to be opened wide or observation window is set in melting ullage, can crystal directly be carried out using closed growing system
Growth using the galvanometer of a set of high precision connection crystal growth system device outside growing system, designs an electric current and returns
Road judges whether seed crystal touches melting liquid level at once by the deflection of galvanometer pointer, then can by the backfeed loop of PID
Primary Calculation goes out the specific height that seed crystal is contacted with melting liquid level and is adjusted solid liquid interface according to the demand of crystal growth
Highly, in this way without open wide growing system it may determine that in crystal growing apparatus seed crystal and silicon melt face contact situation,
Crystal growth defect caused by can reducing and eliminating atmosphere convection current, greatly improves the stability of crystal growth, provides one
The method that kind produces the monocrystal SiC material of high-quality.
Description of the drawings
Fig. 1 is sensing device structure diagram of the present invention；
1 is seed shaft in figure, and 2 be grower, and 3 be SiC seed crystal substrates, and 4 be heat-insulating material, and 5 be graphite crucible, and 6 are
Molten liquid, 7 be crucible axis, and 8 be high precision galvanometer.
Specific embodiment
Embodiment 1
A kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height, using a kind of high precision electricity
Flowmeter and the sensing device realization that current loop is formed with crystal growth system, the sensing device structure are as follows：
1）Including grower 2, crucible axis 7 and high precision galvanometer 8, the grower 2 include accommodating
The graphite crucible 5 of molten liquid 6 and the seed shaft 1 inside graphite crucible 5 can be stretched into；The lower end of the seed shaft 1 is SiC seed crystals
Substrate 3；The outside of the graphite crucible 5 is enclosed with heat-insulating material 4；5 bottom of graphite crucible, which is provided with, to be used to support
Its crucible axis 7；It is electrically connected between the crucible axis 7 and seed shaft 1 by high precision galvanometer 8, wherein conducting wire anode
Connect seed shaft 1, conducting wire cathode connection crucible axis 7；The seed shaft 1 is graphite material.
The method for monitoring in real time in the silicon carbide solwution method and adjusting solid liquid interface height, the specific steps are：
Seed shaft can be stretched into inside graphite crucible during use, polysilicon is put into graphite crucible, close graphite earthenware
Inert gas is passed through after crucible, then set device temperature, and keeps heating graphite crucible, the temperature of crucible is risen into original
Expect more than fusing point, form the silicon of melting；By corrosion of the solution to graphite crucible, SiC molten liquids are formed, then by SiC seed crystals
It is immersed in the SiC solution, the solution near seed crystal is at least made to be in supercooled state, the hypersaturated state for the SiC being consequently formed,
SiC single crystal is made to be grown on seed crystal.The SiC seed crystals are fixed on rotatable seed shaft, are driven by this seed shaft
SiC seed crystals rotate, and the seed crystal of fixed shaft end is contacted with by the way that C to be dissolved in the molten liquid surface containing Si, open current loop and open
It closes, the pointer variation of concern high precision galvanometer when operating seed rod contact liquid level.Before not contacting, pointer is static not
It is dynamic；Melting liquid level moment, galvanometer deflection are contacted in seed crystal；With seed crystal contact with molten liquid contact surface it is deeper, galvanometer
Reading is higher, proportional therewith, and the height and electric current registration contacted according to seed crystal with molten liquid draws standard curve and extrapolate seed
The height that crystalline substance is contacted with molten liquid.Then according to the growth demand of crystal, by the backfeed loop of PID, by above seed shaft
Motor driving seed shaft move up and down, dynamic adjusts the position of seed shaft, it is ensured that solid liquid interface keeps the numerical value stablized,
So that it is guaranteed that the stationarity of crystal growth.
Embodiment 2
A kind of sensing device structure is as follows：
Including grower, crucible axis and high precision galvanometer, the grower include accommodating molten liquid
Graphite crucible and the seed shaft inside graphite crucible can be stretched into；The lower end of the seed shaft is SiC seed crystal substrates；Described
Heat-insulating material is enclosed on the outside of graphite crucible；The graphite crucible bottom, which is provided with, is used to support its crucible axis；It is described
Crucible axis and seed shaft between be electrically connected by high precision galvanometer；Wherein conducting wire anode connection seed shaft, conducting wire cathode
Connect crucible axis；The seed shaft is graphite material.
Claims (1)
1. a kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height, it is characterised in that：Using one kind
High precision galvanometer and the sensing device that current loop is formed with crystal growth system, then again by PID feedback loop, from
The dynamic height for adjusting solid liquid interface is realized；
The sensing device structure is as follows：
Including grower (2), crucible axis (7) and high precision galvanometer (8), the grower (2) hold including being used for
Receive molten liquid (6) graphite crucible (5) and the internal seed shaft (1) of graphite crucible (5) can be stretched into；The seed shaft (1)
Lower end is SiC seed crystals substrate (3)；Heat-insulating material (4) is enclosed on the outside of the graphite crucible (5)；The graphite crucible
(5) bottom, which is provided with, is used to support its crucible axis (7)；Pass through high precision between the crucible axis (7) and seed shaft (1)
Galvanometer (8) is electrically connected, wherein conducting wire anode connection seed shaft (1), conducting wire cathode connection crucible axis (7)；The seed shaft
(1) it is graphite material；
The method for monitoring in real time in the silicon carbide solwution method and adjusting solid liquid interface height, the specific steps are：
(1) before use, the height and electric current registration that are contacted according to seed crystal with molten liquid draw standard curve；
(2) the SiC seed crystals substrate is fixed on rotatable seed shaft, SiC seed crystals is driven to rotate by this seed shaft,
The SiC seed crystals substrate of fixed shaft end is contacted with by the way that C to be dissolved in the molten liquid surface containing Si, opens current loop switch,
The pointer variation of concern high precision galvanometer, extrapolates the height that seed crystal is contacted with molten liquid when operating seed rod contact liquid level
Degree；Then by the backfeed loop of PID, moving up and down for seed shaft is driven by the motor above seed shaft, dynamic adjusts seed
The position of crystallographic axis；
It is as follows that the standard curve obtains step：
A. seed crystal contact liquid level of solution, writes down high precision galvanometer registration；
B. after growing 1 hour, solution evaporation speed is more than long brilliant speed, and liquid level is caused to reduce, and the increase of solid liquid interface height is write down
High precision galvanometer registration at this time；
C. after growing 2 hours, solid liquid interface height continues to increase, and writes down high precision galvanometer registration at this time；
D., until crystal growth terminates, the variation of high precision galvanometer registration is recorded always；
After growth, the solution height of measurement remnant, obtaining liquid level of solution reduces speed, can obtain crystal growth sometime
Solid liquid interface height in section can obtain the standard curve of the correspondence of galvanometer registration and solid liquid interface height in this way.
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| CN110751889A (en) * | 2019-10-30 | 2020-02-04 | 阳皓 | Method for constructing current model |
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| CN114411236B (en) * | 2022-02-10 | 2023-06-27 | 北京青禾晶元半导体科技有限责任公司 | Crystal growth simulating method, crystal growth simulating method and crystal growth simulating device |
| CN115029781A (en) * | 2022-07-29 | 2022-09-09 | 北京晶格领域半导体有限公司 | Method and device for growing silicon carbide single crystal by liquid phase method |
| CN115597682B (en) * | 2022-12-13 | 2023-03-10 | 常州臻晶半导体有限公司 | System and method for measuring liquid level height value in silicon carbide single crystal growth process |
| CN115815544B (en) * | 2022-12-27 | 2024-03-26 | 河南科技大学 | Crystallizer, continuous casting device and method for determining solid-liquid interface position |
| CN116607216B (en) * | 2023-07-20 | 2023-10-13 | 苏州优晶光电科技有限公司 | Method and system for adjusting internal temperature field of resistance silicon carbide growth furnace and growth method |
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