CN206015132U - Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method - Google Patents
Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method Download PDFInfo
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- CN206015132U CN206015132U CN201620652451.8U CN201620652451U CN206015132U CN 206015132 U CN206015132 U CN 206015132U CN 201620652451 U CN201620652451 U CN 201620652451U CN 206015132 U CN206015132 U CN 206015132U
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Abstract
The utility model is related to carborundum solwution method field, more particularly to real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method, the induction installation of current loop is formed using a kind of high precision galvanometer and with crystal growth system, then again by PID feedback loop, the height for automatically adjusting solid liquid interface is realized；In addition this device is without the need for manually taking observation, it is to avoid the atmosphere convection current in fused solution and the external world, it is to avoid observation is time-consuming long, man-hour length, the delayed drawback such as not in time, solves this difficult problem present in solwution method, more conducively produces high-quality monocrystal SiC material.
Description
Technical field
The utility model belongs in carborundum solwution method engineering device technique field, more particularly to a kind of carborundum solwution method in real time
Monitor and adjust the device of solid liquid interface height.
Background technology
Carborundum（SiC）Compare silicon（Si）There is bigger band gap, SiC single crystal has excellent physical property, at a relatively high
Heat endurance and chemical stability, radioresistance line is strong, and mechanical strength has higher breakdown voltage and thermal conductivity than Si
Deng.Used as the semi-conducting material of a new generation, researcher is constantly being lifted to the desired value of high-quality monocrystal SiC.
With regard to SiC crystal for interior all high-quality semi-conducting material, there are two basic demands：First, crystal
Contain defect as few as possible；Second, impurity concentration present in crystal is low as far as possible.
At present it is known that the representative grower of SiC single crystal be vapor phase method and solwution method.In vapor phase method,
The device for generally adopting at present is still that sublimed method places SiC material powders i.e. in graphite crucible, configures SiC seeds in crucible top
Crystalline substance, carries out the operation of crystal growth under the atmosphere of inert gas to crucible heating.SiC single crystal is prepared using sublimed method, although
Crystal growth rate is fast, but which grows, while growth course
In have the interference of many silicon carbide polytypes structures, the problems referred to above to directly affect the quality of SiC single crystal.Conversely, although solwution method is brilliant
Bulk-growth speed is slow, but the concern for causing researcher as which does not have disadvantages mentioned above.In solwution method, in the future
It is dissolved in melt of si from the C of graphite crucible, forms fused solution.End is placed on above-mentioned melting liquid level is fixed with SiC seed crystals
Graphite rod, by with melting liquid level contact, arrange SiC seed crystals Epitaxial Growing and crystallize and to form SiC single crystal.Should
There is no 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 SiC seed crystals are immersed in above-mentioned fused solution so that seed crystal
Nearby it is subcooled and is in hypersaturated state so that SiC single crystal is in the seed crystal Epitaxial growth.The crystal is in the growth operation phase
Between internal system must not be made to be exposed in air, if now seed crystal depart from melting liquid level interrupt the crystal for growing, interrupt
Crystal growth, is caused seed crystal to be contacted with fused solution and defines unstable crystal on seed crystal, may cause crystal Polytype Transformation
State.
Thermograde of the driving force of crystal growth from the solid liquid interface between crystal and liquid level.Along with crystal
Growth, as solute enters crystal and can to a certain degree volatilize, causes the reduction of liquid level.If being unable to 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 coarse problem of plane of crystal, produces the defects such as inclusion enclave, polycrystalline and crystal boundary.
Therefore, how to judge whether seed crystal touches the height of melting liquid level and real-time monitoring contact and adjust solid-liquid circle
Face is highly particularly important.
Content of the invention
The utility model provides in a kind of carborundum solwution method real-time monitoring and adjusts solid-liquid circle for solving existing issue
The device of face height, is employed a kind of high precision electro flowmeter and is formed the induction installation of current loop with crystal growth system, by
This realization can judge SiC seed crystals in time with melting whether liquid level contacts, while real-time monitoring SiC seed crystal is connect with melting liquid level again
Tactile height, then by PID feedback loop, automatically adjusts the height of solid liquid interface, whole process without the need for manually take observation and
Manual regulation, it is to avoid fused solution and the atmosphere convection current in the external world, while it also avoid the error that manual adjustment is brought, solves molten
This difficult problem present in liquid method.
For realizing the purpose of above-mentioned utility model, the utility model concrete technical scheme scheme is as follows：
Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method, using a kind of high precision electricity
Flowmeter the induction installation with crystal growth system formation current loop, then automatically adjust solid-liquid by PID feedback loop again
The height at interface；
The induction installation structure is as follows：
Including grower, crucible axis and high precision galvanometer, described grower is included for accommodating fused solution
Graphite crucible and seed shaft inside graphite crucible can be stretched into；The lower end of described seed shaft is SiC seed crystal substrates；Described
Heat-insulating material is enclosed with the outside of graphite crucible；Described graphite crucible bottom is provided with for supporting its crucible axis；Described
Crucible axis and grower between electrically connected by high precision galvanometer；Wherein wire positive pole connects seed shaft, and wire is born
Pole connects crucible axis；Described seed shaft is graphite material；
Described graphite crucible, for the solution after storing raw material polysilicon and fusing；Graphite crucible is both to hold solution
Container, provide carbon source for crystal growth again.The Si of melting is formed after unmelted polycrystalline silicon, corrodes graphite crucible, form SiC molten
Liquid.
In described carborundum solwution method, the device of real-time monitoring liquid level contact height, concretely comprises the following steps：Can be with during use
Seed shaft is stretched into inside graphite crucible, and polysilicon is put in graphite crucible, inert gas is passed through, so after closing graphite crucible
Set device temperature afterwards, and keep heating graphite crucible, the temperature of crucible is risen to more than raw material fusing point, melting is formed
Silicon；By corrosion of the solution to graphite crucible, SiC fused solutions are formed, subsequently SiC seed crystals are immersed in the SiC,
Solution near seed crystal is at least made in supercooled state, the hypersaturated state of the SiC being consequently formed, SiC single crystal is made on seed crystal
Growth.The SiC seed crystals are fixed on rotatable seed shaft, drive the rotation of SiC seed crystals, fixing axle by this seed shaft
The seed crystal of end is contacted with the fused solution surface by being dissolved in C containing Si, opens current loop switch, in operation seed rod contact
Concern high precision galvanometric pointer change during liquid level, according to.Before not contacting, pointer transfixion；Contact in seed crystal
Melting liquid level moment, galvanometer deflect；As seed crystal contacts deeper with fused solution contact surface, galvanometric reading is higher, therewith
It is directly proportional, the calibration curve according to the height and electric current registration that are contacted with fused solution according to seed crystal is extrapolated seed crystal and connect with fused solution
Tactile height.Then according to the growth demand of crystal, by the backfeed loop of PID, by the Motor drive seed above seed shaft
Crystallographic axis is moved up and down, the position of dynamic adjustment 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.
Described calibration curve specifically calculates that process is as follows：
A. seed crystal contact liquid level of solution, writes down high precision galvanometer registration.
B., after growing 1 hour, solution evaporation speed causes liquid level to reduce more than long crystalline substance speed, and solid liquid interface highly increases
Greatly, now high precision galvanometer registration is write down.
C., after growing 2 hours, solid liquid interface highly continues increase, 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, the solution height of measurement remnant, obtaining liquid level of solution reduces speed, the solid-liquid being obtained in crystal growth certain time period
Interfacial level, draws calibration curve by the corresponding relation of galvanometer registration and solid liquid interface height is so obtained.
The height that described current loop is contacted with fused solution with seed crystal can corresponding relation exist principle：
In described current loop, resistance is several by solution and graphite crucible etc. in seed shaft, the solution of solid liquid interface, crucible
Sections in series is constituted, and wherein seed shaft and graphite crucible are fixed resistance, and in solid liquid interface solution and crucible, solution is for can power transformation
Resistance.
The computing 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 computing formula of resistance, resistance is inversely proportional to sectional area, is directly proportional with length.When liquid level changes
When, 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
When, resistance can change, so as to react in the registration change of rheometer.When solid liquid interface is uprised, resistance increases, electric current
Meter registration diminishes, and when solid liquid interface reduces, resistance reduces, and galvanometer registration becomes big.
The device provided using the utility model, can directly according to the device adjusting parameter of existing solution growth SiC crystal
Produced, such as mode of heating, heat time, growth atmosphere, heating rate and cooldown rate etc., inventor's here is no longer gone to live in the household of one's in-laws on getting married
State.
PID feedback loop described in the utility model is prior art.
In sum, using the utility model, need not take time to observe constantly graphite rod and the contact condition of silicon melt,
Without unlimited growing system, or observation window is set in melting ullage, directly can be carried out using closed growing system
Crystal growth, the galvanometer using a set of high precision outside growing system connect crystal growth system device, design an electricity
Road is flowed back to, judges at once whether seed crystal touches melting liquid level by the deflection of galvanometer pointer, then feeding back to by PID
Road can primary Calculation go out that seed crystal contact with melting liquid level concrete be adjusted solid-liquid circle highly and according to the demand of crystal growth
The height in face, so without the need for opening wide growing system it may determine that seed crystal contact with silicon melt face feelings in crystal growing apparatus
Condition, it is possible to reduce and the crystal growth defect that atmosphere convection current causes is eliminated, greatly improve the stability of crystal growth, there is provided
A kind of device of the monocrystal SiC material for producing high-quality.
Description of the drawings
Fig. 1 is induction installation structural representation described in the utility model；
In figure, 1 is seed shaft, and 2 is grower, and 3 is SiC seed crystal substrates, and 4 is heat-insulating material, and 5 is graphite crucible, and 6 are
Fused solution, 7 is crucible axis, and 8 is high precision galvanometer.
Specific embodiment
Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method, using a kind of high precision electricity
Flowmeter the induction installation with crystal growth system formation current loop, then automatically adjust solid-liquid by PID feedback loop again
The height at interface is realized；
The induction installation structure is as follows：
Including grower 2, crucible axis 7 and high precision galvanometer 8, described grower 2 includes molten for accommodating
Melt the graphite crucible 5 and the seed shaft 1 that can be stretched into inside graphite crucible 5 of liquid 6；The lower end of described seed shaft 1 is SiC seed crystal bases
Plate 3；The outside of described graphite crucible 5 is enclosed with heat-insulating material 4；Described 5 bottom of graphite crucible is provided with for supporting which
Crucible axis 7；Electrically connected by high precision galvanometer 8 between described crucible axis 7 and grower 2, wherein wire positive pole
Connection seed shaft 1, wire negative pole connect crucible axis 7；Described seed shaft 1 is graphite material.
Claims (2)
1. real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method, it is characterised in that：Using one kind
High precision galvanometer the induction installation with crystal growth system formation current loop, then pass through PID feedback loop again, from
The dynamic height for adjusting solid liquid interface is realized；
The induction installation structure is as follows：
Including grower (2), crucible axis (7) and high precision galvanometer (8), described grower (2) is included for holding
Receive fused solution (6) graphite crucible (5) and the internal seed shaft (1) of graphite crucible (5) can be stretched into；Described seed shaft (1)
Lower end is SiC seed crystal substrates (3)；Heat-insulating material (4) is enclosed with the outside of described graphite crucible (5)；Described graphite crucible
(5) bottom is provided with for supporting its crucible axis (7)；By high-accuracy between described crucible axis (7) and grower (2)
Degree galvanometer (8) electrical connection, wherein wire positive pole connection seed shaft (1), wire negative pole connection crucible axis (7).
2. real-time monitoring the device of solid liquid interface height is adjusted in carborundum solwution method according to claim 1, which is special
Levy and be：Described seed shaft (1) is graphite material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620652451.8U CN206015132U (en) | 2016-06-28 | 2016-06-28 | Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method |
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| CN201620652451.8U CN206015132U (en) | 2016-06-28 | 2016-06-28 | Real-time monitoring the device of solid liquid interface height is adjusted in a kind of carborundum solwution method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106048713A (en) * | 2016-06-28 | 2016-10-26 | 山东天岳晶体材料有限公司 | Method for monitoring and regulating solid-liquid interface height in silicon carbide solution process in real time |
-
2016
- 2016-06-28 CN CN201620652451.8U patent/CN206015132U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106048713A (en) * | 2016-06-28 | 2016-10-26 | 山东天岳晶体材料有限公司 | Method for monitoring and regulating solid-liquid interface height in silicon carbide solution process in real time |
| CN106048713B (en) * | 2016-06-28 | 2018-06-26 | 山东天岳晶体材料有限公司 | A kind of method for monitoring in real time in silicon carbide solwution method and adjusting solid liquid interface height |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190320 Address after: 250100 AB Block 1106-6-01, Century Fortune Center, West Side of Xinyu Road, Jinan High-tech Zone, Shandong Province Patentee after: Shandong Tianyue Advanced Material Technology Co., Ltd. Address before: 250018 Meilihu Meili Road, Huaiyin District, Jinan City, Shandong Province Patentee before: Shandong Tianyue Crystal Material Co., Ltd. |
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| TR01 | Transfer of patent right | ||
| CP03 | Change of name, title or address |
Address after: No.99, Tianyue South Road, Huaiyin District, Jinan City, Shandong Province Patentee after: Shandong Tianyue advanced technology Co., Ltd Address before: 250100 AB Block 1106-6-01, Century Fortune Center, West Side of Xinyu Road, Jinan High-tech Zone, Shandong Province Patentee before: Shandong Tianyue Advanced Materials Technology Co.,Ltd. |
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| CP03 | Change of name, title or address |