CN106048713A - Method for monitoring and regulating solid-liquid interface height in silicon carbide solution process in real time - Google Patents
Method for monitoring and regulating solid-liquid interface height in silicon carbide solution process in real time Download PDFInfo
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- CN106048713A CN106048713A CN201610482560.4A CN201610482560A CN106048713A CN 106048713 A CN106048713 A CN 106048713A CN 201610482560 A CN201610482560 A CN 201610482560A CN 106048713 A CN106048713 A CN 106048713A
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- seed
- crucible
- height
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- galvanometer
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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
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
Abstract
The invention relates to the field of a silicon carbide solution process, particularly a method for monitoring and regulating solid-liquid interface height in a silicon carbide solution process in real time. By adopting a high-precision galvanometer, the deflection of the pointer is utilized to judge whether SiC seed crystals contact the molten liquid surface in the graphite crucible, and the definite value displayed on the galvanometer is utilized to estimate the specific contact height of the SiC seed crystals and molten liquid, thereby ensuring the accuracy of the crystal growth experiment and the real-time controllability of the contact liquid surface, and visually and effectively achieving the goal of obtaining the liquid surface height contacted by the seed crystals. Besides, the method better promotes controllable growth of the SiC crystals to some extent. In addition, the process does not need manual observation, avoids the atmosphere convection between the molten liquid and the outside, avoids defects of long time consumption for observation, long working hours, no timeliness and the like, solves the problems in the solution process, and is more beneficial to producing the high-quality monocrystal SiC material.
Description
Technical field
The invention belongs to carborundum solwution method technical field, particularly relate to a kind of carborundum solwution method is monitored in real time and adjusted
The method of solidating liquid interfacial level.
Background technology
Carborundum (SiC) has bigger band gap than silicon (Si), and SiC single crystal has the physical property of excellence, at a relatively high
Heat stability and chemical stability, radioprotective line is strong, and mechanical strength has higher breakdown voltage and thermal conductivity than Si
Deng.As the semi-conducting material of a new generation, the expected value of high-quality monocrystal SiC is constantly being promoted by research worker.
About SiC crystal for interior all high-quality semi-conducting material, there are two basic demands: one, crystal
Containing the fewest defect；Its two, impurity concentration is the lowest present in crystal.
At present it is known that the representative growing method of SiC single crystal be vapor phase method and solwution method.In vapor phase method,
The most commonly used method is still sublimed method and i.e. places SiC material powder in graphite crucible, configures SiC seed at crucible top
Crystalline substance, carries out the operation of crystal growth under the atmosphere of noble gas to crucible heating.Sublimed method is used to prepare SiC single crystal, although
Crystal growth rate is fast, but contains more micro-pipe and have substantial amounts of crystal defect, simultaneously growth course in its growth gained crystal
In have the interference of many silicon carbide polytypes structures, the problems referred to above directly affect the quality of SiC single crystal.On the contrary, although solwution method is brilliant
Bulk-growth speed is slow, but owing to it does not has disadvantages mentioned above causing the concern of research worker.In solwution method, in the future
It is dissolved in melt of si from the C of graphite crucible, forms fused solution.Above-mentioned melted liquid level is placed end and is fixed with SiC seed crystal
Graphite rod, by contacting with melted liquid level, arrange SiC seed crystal Epitaxial Growing and crystallize formation SiC single crystal.Should
There is not inevitable micro-pipe problem present in sublimed method in method, 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 operation of solution growth SiC crystal, need to be immersed in above-mentioned fused solution SiC seed crystal so that seed crystal
Near supercool and be in hypersaturated state so that SiC single crystal is at described seed crystal Epitaxial growth.Described crystal is in the growth operation phase
Between internal system must not be made to be exposed in air, if now seed crystal departs from melted liquid level and interrupts the crystal grown, interrupt
Crystal growth, causes seed crystal to contact the crystal defining instability on seed crystal with fused solution, may cause crystal Polytype Transformation
State.
The driving force of crystal growth derives from the thermograde of the solid liquid interface between crystal and liquid level.Along with crystal
Growth, owing to solute enters crystal and to a certain degree can volatilize, causes the reduction of liquid level.If can not real-time monitoring
The height of solid liquid interface, can cause the change of the thermograde of solid liquid interface, and then cause the change of crystal growth rate.If
Thermograde is excessive, it may appear that the problem that plane of crystal is coarse, produces the defects such as inclusion enclave, polycrystalline and crystal boundary.
Therefore, how to judge whether seed crystal touches melted liquid level and the height of monitoring contact in real time and adjust solid-liquid circle
Face height is particularly important.
Summary of the invention
The present invention solves existing issue to provide in a kind of carborundum solwution method and monitor and adjust solid liquid interface height in real time
The method of degree, have employed a kind of high precision electro flowmeter and forms the induction installation of current loop with crystal growth system, thus real
Now can judge whether SiC seed crystal contacts with melted liquid level in time, monitoring SiC seed crystal contacts with melted liquid level the most in real time
Highly, then passing through PID feedback loop, be automatically adjusted the height of solid liquid interface, whole process is time-consumingly observed and manual without artificial
Regulation, it is to avoid fused solution and extraneous atmosphere convection current, it also avoid the error that manual adjustment is brought simultaneously, solve solwution method
Present in this difficult problem.
For realizing the purpose of foregoing invention, the present invention concrete technical scheme scheme is as follows:
A kind of method monitored in real time and adjust solid liquid interface height in carborundum solwution method, uses a kind of high precision galvanometer
And form the induction installation of current loop with crystal growth system, the most again by PID feedback loop, it is automatically adjusted solid liquid interface
Height；
This induction installation structure is as follows:
Including grower, crucible axis and high precision galvanometer, described grower includes the stone for accommodating fused solution
Ink crucible and the seed shaft within graphite crucible can be stretched into；The lower end of described seed shaft is SiC seed crystal substrate；Described graphite
The outside of crucible is enclosed with adiabator；The crucible axis for supporting it it is provided with bottom described graphite crucible；Described earthenware
Electrically connected by high precision galvanometer between crucible axle and seed shaft；Wherein wire positive pole connects seed shaft, and wire negative pole connects
Crucible axis；Described seed shaft is graphite material；
Described graphite crucible, the solution after storing raw material polysilicon and fusing；Graphite crucible is the appearance holding solution
Device, provides carbon source for crystal growth again.Form melted Si after unmelted polycrystalline silicon, corrode graphite crucible, form SiC.
The method monitoring liquid level contact height in described carborundum solwution method in real time, concretely comprises the following steps: permissible during use
Seed shaft is stretched into inside graphite crucible, in graphite crucible, put into polysilicon, after closing graphite crucible, be passed through noble gas, so
Rear set device temperature, and keep graphite crucible is heated, the temperature of crucible is risen to more than raw material fusing point, is formed melted
Silicon；By the solution corrosion to graphite crucible, form SiC fused solution, subsequently SiC seed crystal be immersed in this SiC,
The solution near seed crystal is at least made to be in supercooled state, the hypersaturated state of the SiC being consequently formed, make SiC single crystal on seed crystal
Growth.Described SiC seed crystal is fixed on rotatable seed shaft, drives SiC seed crystal to rotate by this seed shaft, fixing axle
The seed crystal of end contacts with by C is dissolved in the fused solution surface containing Si, opens current loop switch, in operation seed rod contact
The change of high precision galvanometric pointer is paid close attention to during liquid level, according to.Before no contact, pointer transfixion；Contact at seed crystal
Melted liquid level moment, galvanometer deflects；Along with seed crystal contacts the deepest with fused solution contact surface, galvanometric reading is the highest, therewith
It is directly proportional, extrapolates seed crystal according to the standard curve of the height contacted with fused solution according to seed crystal and electric current registration and connect with fused solution
The height touched.Then according to the growth demand of crystal, by the feedback circuit of PID, seed is driven by the motor above seed shaft
Moving up and down of crystallographic axis, dynamically adjusts the position of seed shaft, it is ensured that solid liquid interface keeps a stable numerical value, so that it is guaranteed that crystal
The stationarity of growth.
It is as follows that described 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, more than long brilliant speed, causes liquid level to reduce, and solid liquid interface height increases
Greatly, now high precision galvanometer registration is write down.
C., after growing 2 hours, solid liquid interface height continues to increase, and writes down now high precision galvanometer registration.
D. the like, until crystal growth terminates, record the change of high precision galvanometer registration always.Grown junction
Shu Hou, measures remaining solution height, obtains liquid level of solution and reduces speed, the solid-liquid in available crystal growth certain time period
Interfacial level, the corresponding relation that the most i.e. can get galvanometer registration and solid liquid interface height can draw standard curve.
The height that described current loop contacts with fused solution with seed crystal can corresponding relation exist principle:
In described current loop, resistance is by a few part such as solution and graphite crucible in seed shaft, the solution of solid liquid interface, crucible
Being composed in series, wherein seed shaft and graphite crucible are fixed resistance, and in solid liquid interface solution and crucible, solution is variable resistance.
Wherein the computing formula of resistance is: R=ρ L/S wherein R be resistance, S be sectional area, L be length, ρ be resistivity.
According to the computing formula of resistance, resistance is inversely proportional to sectional area, with length is directly proportional.When liquid level changes
Time, sectional area is not changed in, and resistivity is not changed in, the only length of change.So when the height of solid liquid interface changes
Time, resistance can change, thus reaction is on the registration of rheometer changes.When solid liquid interface uprises, resistance increases, electric current
Meter registration diminishes, and when solid liquid interface reduces, resistance reduces, and galvanometer registration becomes big.
It is as follows that the present invention also protects a kind of induction installation structure:
Including grower, crucible axis and high precision galvanometer, described grower includes the stone for accommodating fused solution
Ink crucible and the seed shaft within graphite crucible can be stretched into；The lower end of described seed shaft is SiC seed crystal substrate；Described graphite
The outside of crucible is enclosed with adiabator；The crucible axis for supporting it it is provided with bottom described graphite crucible；Described earthenware
Electrically connected by high precision galvanometer between crucible axle and grower；Wherein wire positive pole connects seed shaft, and wire negative pole is even
Connect crucible axis；Described seed shaft is graphite material.
Use the apparatus and method that the present invention provides, directly can adjust ginseng according to the method for existing solution growth SiC crystal
Number produces, and such as mode of heating, heat time heating time, growth atmosphere, heating rate and cooldown rate etc., inventor is the most superfluous at this
State.
Heretofore described PID feedback loop is prior art.
In sum, use the present invention, it is not necessary to the moment of taking time observes the contact condition of graphite rod and silicon melt, also without
Growing system need to be opened wide, or be provided above observation window at melted liquid level, can directly use airtight growing system to carry out crystal
Growth, uses the galvanometer of a set of high precision to connect crystal growth system device outside growing system, designs an electric current and return
By the deflection of galvanometer pointer, road, judges whether seed crystal touches melted liquid level at once, then can by the feedback circuit of PID
Primary Calculation goes out concrete height that seed crystal contacts with melted liquid level and is adjusted solid liquid interface according to the demand of crystal growth
Highly, so without unlimited growing system it may determine that in crystal growing apparatus seed crystal and silicon melt face contact situation,
Can reduce and eliminate the crystal growth defect that atmosphere convection current causes, be greatly improved the stability of crystal growth, it is provided that one
The method planting the monocrystal SiC material producing high-quality.
Accompanying drawing explanation
Fig. 1 is induction installation structural representation of the present invention；
In figure, 1 is seed shaft, and 2 is grower, and 3 is SiC seed crystal substrate, and 4 is adiabator, and 5 is graphite crucible, and 6 is melted
Liquid, 7 is crucible axis, and 8 is high precision galvanometer.
Detailed description of the invention
Embodiment 1
A kind of method monitored in real time and adjust solid liquid interface height in carborundum solwution method, uses a kind of high precision galvanometer
And form the induction installation realization of current loop with crystal growth system, this induction installation structure is as follows:
1) including grower 2, crucible axis 7 and high precision galvanometer 8, described grower 2 includes for accommodating melted
The graphite crucible 5 of the liquid 6 and seed shaft 1 within graphite crucible 5 can be stretched into；The lower end of described seed shaft 1 is SiC seed crystal substrate
3；The outside of described graphite crucible 5 is enclosed with adiabator 4；It is provided with for supporting it bottom described graphite crucible 5
Crucible axis 7；Being electrically connected by high precision galvanometer 8 between described crucible axis 7 and seed shaft 1, wherein wire positive pole connects
Seed shaft 1, wire negative pole connects crucible axis 7；Described seed shaft 1 is graphite material.
The method monitored in real time and adjust solid liquid interface height in described carborundum solwution method, concretely comprises the following steps:
Can seed shaft be stretched into inside graphite crucible during use, in graphite crucible, put into polysilicon, after closing graphite crucible
It is passed through noble gas, then set device temperature, and keeps graphite crucible is heated, the temperature of crucible is risen to raw material and melts
More than Dian, form melted silicon；By the solution corrosion to graphite crucible, form SiC fused solution, subsequently SiC seed crystal is impregnated
In this SiC, the solution near seed crystal is at least made to be in supercooled state, the hypersaturated state of the SiC being consequently formed, make
SiC single crystal grows on seed crystal.Described SiC seed crystal is fixed on rotatable seed shaft, drives SiC by this seed shaft
Seed crystal rotates, and the seed crystal of fixing shaft end contacts with by C is dissolved in the fused solution surface containing Si, opens current loop and switchs,
The change of high precision galvanometric pointer is paid close attention to when operating seed rod contact liquid level.Before no contact, pointer transfixion；
In seed crystal contact melted liquid level moment, galvanometer deflects；Along with seed crystal contacts the deepest with fused solution contact surface, galvanometric reading
The highest, proportional therewith, the height contacted with fused solution according to seed crystal and electric current registration draw standard curve extrapolate seed crystal with
The height of fused solution contact.Then according to the growth demand of crystal, by the feedback circuit of PID, by the electricity above seed shaft
Machine drives moving up and down of seed shaft, dynamically adjusts the position of seed shaft, it is ensured that solid liquid interface keeps a stable numerical value, thus
Guarantee the stationarity of crystal growth.
Embodiment 2
A kind of induction installation structure is as follows:
Including grower, crucible axis and high precision galvanometer, described grower includes the stone for accommodating fused solution
Ink crucible and the seed shaft within graphite crucible can be stretched into；The lower end of described seed shaft is SiC seed crystal substrate；Described graphite
The outside of crucible is enclosed with adiabator；The crucible axis for supporting it it is provided with bottom described graphite crucible；Described earthenware
Electrically connected by high precision galvanometer between crucible axle and seed shaft；Wherein wire positive pole connects seed shaft, and wire negative pole connects
Crucible axis；Described seed shaft is graphite material.
Claims (4)
1. the method monitored in real time and adjust solid liquid interface height in a carborundum solwution method, it is characterised in that: use one
High precision galvanometer also forms the induction installation of current loop with crystal growth system, the most again by PID feedback loop, from
The height of dynamic regulation solid liquid interface realizes；
This induction installation structure is as follows:
Including grower (2), crucible axis (7) and high precision galvanometer (8), described grower (2) includes for holding
Receive the graphite crucible (5) of fused solution (6) and the seed shaft (1) that graphite crucible (5) is internal can be stretched into；Described seed shaft (1)
Lower end is SiC seed crystal substrate (3)；The outside of described graphite crucible (5) is enclosed with adiabator (4)；Described graphite crucible
(5) bottom is provided with the crucible axis (7) for supporting it；High precision is passed through between described crucible axis (7) and seed shaft (1)
Galvanometer (8) electrically connects, and wherein wire positive pole connects seed shaft (1), and wire negative pole connects crucible axis (7)；Described seed shaft
(1) it is graphite material；
The method monitored in real time and adjust solid liquid interface height in described carborundum solwution method, concretely comprises the following steps:
(1), before using, the height contacted with fused solution according to seed crystal and electric current registration draw standard curve；
(2) described SiC seed crystal substrate is fixed on rotatable seed shaft, drives SiC seed crystal to rotate by this seed shaft,
The SiC seed crystal substrate of fixing shaft end contacts with by C is dissolved in the fused solution surface containing Si, opens current loop and switchs,
Pay close attention to the change of high precision galvanometric pointer during operation seed rod contact liquid level, extrapolate the height that seed crystal contacts with fused solution
Degree；Then by the feedback circuit of PID, drive moving up and down of seed shaft by the motor above seed shaft, dynamically adjust seed
The position of crystallographic axis.
The method monitoring liquid level contact height in carborundum solwution method the most according to claim 1 in real time, it is characterised in that:
It is as follows that described 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, more than long brilliant speed, causes liquid level to reduce, and solid liquid interface height increases, and remembers
Under now high precision galvanometer registration；
C., after growing 2 hours, solid liquid interface height continues to increase, and writes down now high precision galvanometer registration；
D. the like, until crystal growth terminates, record the change of high precision galvanometer registration always；
After growth terminates, measuring remaining solution height, obtain liquid level of solution and reduce speed, available crystal growth is sometime
Solid liquid interface height in Duan, the most i.e. can get the standard curve of the corresponding relation of galvanometer registration and solid liquid interface height.
3. realize a kind of carborundum solwution method described in claim 1 being monitored in real time and adjusting the sensing dress of solid liquid interface height
Put, it is characterised in that: concrete structure is as follows: include grower (2), crucible axis (7) and high precision galvanometer (8), described
Grower (2) include the graphite crucible (5) for accommodating fused solution (6) and the seed crystal that graphite crucible (5) is internal can be stretched into
Axle (1)；The lower end of described seed shaft (1) is SiC seed crystal substrate (3)；The outside of described graphite crucible (5) is enclosed with thermal insulation
Material (4)；Described graphite crucible (5) bottom is provided with the crucible axis (7) for supporting it；Described crucible axis (7) and seed
Being electrically connected by high precision galvanometer (8) between crystallographic axis (1), wherein wire positive pole connects seed shaft (1), and wire negative pole connects
Crucible axis (7).
Induction installation the most according to claim 3, it is characterised in that: described seed shaft (1) is graphite material.
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| CN110751889A (en) * | 2019-10-30 | 2020-02-04 | 阳皓 | Method for constructing current model |
| CN114411236A (en) * | 2022-02-10 | 2022-04-29 | 北京青禾晶元半导体科技有限责任公司 | Growth method of simulated crystal, growth method of crystal and 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 |
| CN115597682A (en) * | 2022-12-13 | 2023-01-13 | 常州臻晶半导体有限公司（Cn） | Method for accurately measuring liquid level height value in growth process of silicon carbide single crystal by liquid phase method |
| CN115815544A (en) * | 2022-12-27 | 2023-03-21 | 河南科技大学 | Crystallizer, continuous casting device and method for measuring position of solid-liquid interface |
| CN116607216A (en) * | 2023-07-20 | 2023-08-18 | 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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