CN109898136A - Multiple Sapphire Crystal Growth device and growing method - Google Patents
Multiple Sapphire Crystal Growth device and growing method Download PDFInfo
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- CN109898136A CN109898136A CN201910264838.4A CN201910264838A CN109898136A CN 109898136 A CN109898136 A CN 109898136A CN 201910264838 A CN201910264838 A CN 201910264838A CN 109898136 A CN109898136 A CN 109898136A
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- 238000002425 crystallisation Methods 0.000 claims abstract description 28
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to multiple Sapphire Crystal Growth device and growing methods, specifically, to realize that multiple crystal are grown simultaneously, the growth furnace internal temperature for arranging more crucibles is kept uniform, and the temperature sensor of multiple seperated heater is used to produce high-quality crystallization, and effectively arrange the related Sapphire Crystal Growth device of thermoregulator and power control unit and multiple growth method of sapphire single crystal using this device.Sapphire Crystal Growth device according to the present invention, more crucibles are located in multiple seperated heater, control the electric power to the application of each heater flexibly to ensure the uniformity of in-furnace temperature, not only in crucible, temperature between each crucible can also keep uniform, its uniform quality is outstanding, can grow multiple crystal with uniform shapes simultaneously, can a large amount of save the costs compared to previous method.
Description
Technical field
The present invention relates to multiple Sapphire Crystal Growth device and growing methods, and in particular to a kind of production is high-quality blue precious
The grower of stone monocrystalline and the growth method of sapphire single crystal for utilizing this device.
Background technique
Recently, constantly bringing forth new ideas with LED industry brings illumination and display industry recombination in the world.With
LED based on GaN semiconductor material can not only be shown because it has the high energy gap that cannot achieve with other materials semiconductor
Cyan and purple colour gamut are shown, can also realize high brightness, therefore effectively applied on high power applications.Therefore modern times LED is produced
It is almost most of in industry all to use GaN semiconductor for the substrate of growing film shape GaN semiconductor, it is needed in principle using GaN
Monocrystalline.But the growth conditions of GaN single crystal is very harsh, it is difficult to realize the growth of large-scale monocrystalline, economy is not also high, therefore
Up to the present it is limited only to carry out in special-purpose in the practical stage.
Nearest industrial technology is after the mode of growing film shape GaN single crystal manufactures blue led on sapphire wafer, by this
It carries out practical, efficient aspect and achieves success.Therefore it is at present manufacture full gamut high-brightness LED, generallys use blue precious
The mode of GaN film is grown in stone (Al2O3) single-wafer.In addition, on the basis of batch production, using more economical material benefit
The mode of LED illumination utensil realize price advantage, thus the applicable LED in almost all of illumination, to this need
It asks also in being continuously increased.
Previous Sapphire Crystal Growth technology has: Verneuil method, Czochralski method, changes at hydro-thermal method
Thermal method, Ji Luobo Loews method, EFG method etc. are more.But such as wants to cater to newest LED industry step, meet ever-increasing market need
It asks, realizes low price and volume production, it is necessary to improve to crystalline growth method.
Can produce in batches has Czochralski method, heat exchange method for the large-scale sapphire method of high quality of LED industry
With Ji Luobo Loews method etc. (Fig. 1 a-1c is referred to respectively, in A to after growth, then obtains effective crystal with the face A, most ambassador
It is respectively 30%, 32-34% and 70%) with rate.In previous sapphire growth method, produced to realize batch production and improving
It can, it is necessary to which enlargement is carried out to crystallization.Long large size of making a living crystallizes, and inevitably elongates growth and the cooling time of crystallization.Cause
This such as wants the enlargement for realizing crystallization, and production capacity is difficult to meet required speed, even more to guarantee crystalline quality, needs to carry out more
Highly difficult technological development etc., there are many difficulties.
In order to overcome the problems referred above, a large amount of to improve after quadrangle crystallization can be grown to improve sapphire crystalline growth production capacity
To this utilization rate.In order to further improve production capacity, considerable scale should not be realized the crystal size of enlargement into
One step of row it is enlarged, but by multiple crystal simultaneously grow method be indispensable.
In Republic of Korea registered patent the 10-1136143rd, using long crucible, and the width and thickness of radiator is transformed, with
When obtaining necessary temperature gradient horizontally and vertically, but such as using strip large size seed crystal, exist according to its seed
Brilliant length is difficult to the problem for keeping temperature uniform.In particular, even more including crucible both ends and middle part when as too long such as crucible length
Divide including temperature, is not only difficult to keep the temperature of horizontal direction uniform, and according to thermal insulation material under 2000 DEG C of temperatures above
Access times or service life change therewith, therefore even if adjustment radiator width and thickness keep its more uniform, but
With the increase of access times and service life, temperature can also change therewith.It is special such as the non-uniform temperature of horizontal direction
It is not when using strip seed crystal, the seed crystal among length direction crucible bottom will be melted, or charging feedstock occur
Phenomena such as can not melting.This phenomenon such as occurs, is not only difficult to grow monocrystalline, but also even if seed crystal is not melted completely,
Appearance fails uniformly to melt, the crystalline quality decline after leading to growth.
To solve the above problems, being provided a kind of for holding life in Republic of Korea registered patent the 10-1229984th
Inner horizontal direction temperature when long is uniform, is spy with respective isolated operation after the multiple seperated heater of crucible disposed outside
The Sapphire Crystal Growth device of point.When using multiple seperated radiator and independent temperature regulating system, respective position is arranged
Temperature can be controlled to a certain extent.But because respective temperature sensor is there are evaluated error, temperature difficult to realize is equal
It is even, in addition being difficult to carry out stable movement by the interference from heater around.That is, respectively thermoregulator be reduce by
The temperature difference between the respective temperature sensor measurement temperature and preset value of automatic control heater temperature sensor, with pid control mode structure
After parameter, signal is sent to electric power control portion.At this point, from electric power control portion control fever temperature in addition to by oneself
It other than the electric power of application influences, to be also affected from adjacent heater, it is existing to be accordingly difficult to the power fluctuation for avoiding moment from occurring
As.In this way, respectively fission section is smaller, power fluctuation phenomenon is bigger, this is just difficult to not have needed for meeting growing high quality monocrystalline
There is the accurate temperature of temperature variation to control.
In addition, according to Korean Patent the 10-1196445th, when such as more crucibles being set in single thermal insulator,
The radiant heat that crucible is directly subject to from heater can be cut off, can ensure the uniform of length direction temperature to a certain extent
Property, the temperature difference occurred in the single crucible of strip can be separated into its smaller crucible, therefore can be effectively prevented in crucible
The growth of more good polycrystal may be implemented in the temperature difference.
Even if being asked in the independent temperature regulating system of multiple fission there are still measuring temperature error using the above method
Topic, this will lead to Electric control deviation, and have some impact on to the thermometric of adjacent heater, it is difficult to stable control is carried out,
Namely because these reasons, it is difficult to avoid the internal temperature difference occurred fundamentally in growth course.That is, according to respective temperature sensing
Device will be affected from adjacent thermometric heater, this practical work explanation passes through temperature sensor and thermoregulator and electric power
The closed loop (closed loop) that control device controls the electric power of heater will be affected from outside, to lead
Actuating is not sufficiently stable, and thus will hinder stable temperature control action.In addition, even if system building it is very perfect, but because of temperature
Sensor is spent there are uncertain factor, and the measured temperature difference equally changes, therefore each crucible internally positioned in growth course
Between the temperature difference can occur, this temperature difference is different according to monocrystalline position base crystal growth rate, is not only difficult to guarantee so excellent
Matter crystalline growth, and mass-dispersion can occur in respective crystallization.
In the present invention, including for reducing temperature change and each earthenware in the sapphire single crystal growth furnace using more crucibles
The temperature difference between crucible and including applicable thermometric and electrical control method, it will thus provide effective temperature control system, this system is not
It can only guarantee high-quality Sapphire Crystal Growth, the monocrystalline with homogeneous quality can also be grown in respective crucible, be criticized to realize
Amount production sapphire single-crystal, to provide single-crystal growing apparatus and growing method.
Summary of the invention
In the present invention, it has studied using multiple seperated heater and the temperature sensor for uniform temperature control, temperature
Adjuster and effective arrangement and control method to power control unit are spent, and essential temperature is steady in crystal growth
It is qualitative and in multiple crystal are grown simultaneously must condition temperature uniformity etc., realized with this with the more of homogeneous quality
The growth of a crystal.
The present invention arranges 3 seperated heaters after the Sapphire Crystal Growth device that preparation is formed a line by 6 crucibles
It is a pair of with the auxiliary heater positioned at both ends in furnace, and to obtain uniform temperature by supplying uniform stable electric power, and it is sharp
Sapphire Crystal Growth is implemented with the temperature control system through studying.As a result in Sapphire Crystal Growth almost without generation
Electric power variation is controlled, therefore in the case where in growth furnace almost without temperature change, very stably maintains temperature, is grown
Temperature in furnace is equally kept uniformly, to effectively facilitate the identical Sapphire Crystal Growth of high-quality majority.
Therefore, the present invention is in a certain viewpoint, comprising: warm to keep internal temperature to rise to crystallization raw material melting after heating
Du or more and the growth furnace with surrounding insulation；From seeded growth while being melted inside the growth furnace and for raw material
More crucibles of monocrystalline；To melt the raw material, in the multiple seperated heater of its disposed outside；To be obtained from the heater
Necessary temp and the pyrometer and thermoregulator as temperature sensor of electric power are provided, and exist including power control unit
Interior temperature control system；In the more crucibles for the real time measure raw material be melted after crystal growth height and in furnace body
The multiple heights measurement device of top installation；And to prevent being melted completely for the seed crystal, appropriate temperature ladder up and down is being formed
After degree, for be well on crystalline growth and in the cooling body etc. of the bottom of crucible installation；In the list including above-mentioned items
In crystals growth device, the more crucibles are formed a line by 2-20 crucible, and the cooling body is in every crucible arrangement
With the characteristics of single-crystal growing apparatus bottom.
In the present invention, the crucible is can use at high temperature can not here for growing seed crystal after fused raw material
The not high refractory metal of the reactivity of melting, when tetragonal crucible is formed a line from temperature adjusting and crystalline growth level
It is more easier and economy is also high.Above-mentioned crucible is mainly disposable, therefore is saving expense in selection thin slice gold
Use is welded after belonging to plate, is difficult to maintain own form at high temperature, therefore using reinforcing body to keep within the crystalline growth phase
Shape, and inner molten object can be kept safe.Above-mentioned reinforcing body can select the good graphite of high temperature strength, but reinforcing body and
Crucible may cause reaction and melting, therefore take measures to keep a fixed spacing between reinforcing body and crucible.
In addition, the crucible is to prevent that raw material from not melting or the seed crystal is melted completely, the crucible of the seed crystal is installed
The mode that bottom is preferentially inwardly recessed or outwardly protrudes is formed.
Sapphire Crystal Growth device of the invention will use more crucibles of non-single crucible specifically will be to include
With the characteristics of 2-20 crucible.Every crucible size is W (60-300 ㎜) × H (80-300 ㎜) × L (100-400 ㎜).
According to the present invention, it such as when single-crystal growing apparatus uses more crucibles of non-single crucible, is crystallized in identical holding
While growing and cool down the required time, the quantity of single production monocrystalline can be increased, to improve production capacity.
The effect of the heater is to supply heat to be melted in the sapphire raw material filled inside the crucible, can be with
Select the refractory metal heater or graphite heater using resistance used under normal conditions.The seperated heater is wide
Though degree is not particularly limited, best using 5-50 ㎝ range.The heater width for example less than 5 ㎝ when, heater and fever
Temperature control fitting quantity increases therewith, causes device to become complicated, increases expense.It is difficult to equably when instead more than 50 ㎝
Keep horizontal direction temperature.The heater quantity is depending on the crucible quantity being packed into growth furnace.
In previous invention, the heater is to keep growth furnace internal temperature uniform, more in the crucible disposed outside
After weight is seperated, the control by temperature sensor, thermoregulator, power control unit etc. each independently.But because surveying
Temperature sensor used in temperature has differences, and inevitably occurs occurring difference in measuring temperature, and supplies to each heater
It is also different for answering electric power.In addition, each heater can not avoid the influence from neighbouring heater, therefore according to neighbouring heater
Temperature change changes, just as this indirect interference phenomenon, temperature control will become highly unstable.
In the present invention, non-to obtain in the elongated growth furnace for arranging more crucibles to realize that polycrystal is grown simultaneously
Normal stabilization and uniform temperature, it will thus provide the method for the multiple seperated heater of control.
That is, only using single temperature sensor to eliminate between each temperature sensor because of inhomogeneities caused by error.Also
Have, select the respective power control unit for being controlled to the power supply of each heater, to supply identical electricity to each heater
Power.Such as because a variety of causes is when the temperature difference occurs for furnace interior, in a manner of adjusting to related heater power supply volume, temperature can be overcome
Non-uniform phenomenon.
The above method and the temperature control mode in the monocrystal growing furnace used in general are entirely different.That is, logical
Chang Fangfa is single temperature sensor and single power control unit to be used in furnace, and use each heater serial or parallel connection
The method controlled afterwards.Nearly all heater in the world is according to its impedance of temperature change even sub-fraction can also be sent out
Changing, it is impossible to a certain degree that in fact the electric power of serial or parallel connection bifurcated, which remains,.In addition, as selected in the past
Temperature control mode obtains in furnace especially in the elongated crystallization growth furnace of the more crucibles of arrangement of one of feature of the present invention
Uniform Temperature Distribution is extremely difficult.
In addition, the long-play under the condition of high temperature in sapphire growth furnace, in addition the volatilization of raw alumina, heater
To be damaged quickly, and resistance difference occur according between extent of damage heater, the electric power to each heater bifurcated with when
Between loss also to change, in final producer the phenomenon that non-uniform temperature.
When being such as applicable in electric control system provided in the present invention, the above problem can be avoided, can also taking human as adjust to
The power supply ratio of each heater can solve growth furnace internal temperature non-uniform phenomenon etc., have the advantages that very big.That is,
Though temperature control loop section installation and operation single temperature sensor, by the side for measuring growth furnace each section temperature as needed
Formula can grasp in-furnace temperature distribution situation, in addition the crystallization height that measurement is grown in respective crucible, can control growth in detail
The Temperature Distribution of furnace interior.When the temperature difference such as occurs according to position, each heater power supply ratio can be carried out by electric power controller
It adjusts, therefore easily obtains uniform in-furnace temperature distribution, it is highly beneficial in implementing multicrystalline growth.
In the present invention, the cooling body is to guarantee that the horizontal direction temperature of crucible is uniform, in respective crucible bottom cloth
It is set to feature.
The cooling body has direct or indirect method, and is cooled down using liquid or gas as medium, can also be used
The coldplate etc. that molybdenum, tungsten, tantalum and its alloy or graphite that will not react under hot environment with crucible etc. are processed.
When using single-crystal growing apparatus of the invention, respectively multiple seperated heater and respective Electric control dress will be used
It sets, and is controlled by single thermoregulator, to not only guarantee that temperature is uniform in crucible, can also be kept between each crucible
Temperature is uniform.In addition, being carried out when necessary to the auxiliary heater at both ends using other temperature sensors and other thermoregulators
Individually control.
Growth method of sapphire single crystal according to the present invention, including by the melt stage of sapphire raw material in conventional art and
It is constituted from the crystalline growth stage for the seed crystal for being located at the lower end of the crucible.
That is, the bottom of more crucibles of horizontal direction arrangement arranges in growth furnace in the melt stage of sapphire raw material
Seed crystal, and sapphire raw material is filled to respective crucible.Later, to prevent the seed crystal to be melted completely, by being installed on crucible
Beneath cooling body while cooled down, heated using resistance heater, and then rise to sapphire from room temperature
After the melting temperature temperatures above of raw material is horizontal, sapphire raw material is melted.
After sapphire raw material as above is all melted, in the crystalline growth stage from seed crystal, continue through at the bottom of crucible
While the cooling body of lower installation is cooled down, after fever temperature is carried out cooling at leisure, crystallization is given birth to from seed crystal
It is long.
In above-mentioned melt stage and crystalline growth stage, to make each crucible temperature keep uniformly, utilizing temperature of the invention
The electric power that control method supplies control to heater.
As above, the temperature in growth furnace is kept highly stable, while the temperature of horizontal direction equally keeps uniform.Using more
After crucible, the temperature in crucible keeps certain level, and the temperature between each crucible is kept uniformly, to realize its shape and quality
Uniformly, while a large amount of high-quality sapphire single-crystals being obtained.
It can also additionally include the stage for implementing annealing (anneal ing) in the present invention.Its method is in the sapphire
Crystalline growth terminates and is initially switched off cooling before carrying out cooling with room temperature, to control the temperature difference of crystallization top and the bottom.
In the annealing stage, crucible internal temperature can be kept for 1700-2000 DEG C and 1 hour or more.
Sapphire raw material is just fusible at 2100 DEG C or more under normal conditions, and the growth of crystallization is about in 1920-2100 DEG C
It realizes.Because sapphire melting temperature is 2045 DEG C, melt initiation temperature degree and crystal growth temperature should be 2045 DEG C,
But the raw material of crystalline growth melts in the position and crucible because of measuring temperature has differences between position, so will appear such temperature
Difference, the temperature range when changing temperature measurement location and method as that can change.
In the present invention, the cooling body is that the seed crystal positioned at the bottom of crucible is prevented to be melted completely, is arranged as cooling
The means used under normal conditions can be selected by applying, and be can be selected and carried out forcing cooling tungsten or molybdenum coldplate to gas or liquid
Deng.Therefore, the cooling body for example coldplate when, according to the up and down motion of its coldplate, or according to the up and down motion of crucible,
Cooling will be cut off in a manner of separating coldplate from crucible.
Through the above technical solutions, arranging the Sapphire Crystal Growth device of temperature control system according to the present invention as being applicable in
When, it can not only carry out stablizing and accurate temperature control inside growth furnace, and can guarantee whole temperature inside growth furnace
The uniformity of degree, so that the respective crystalline quality dispersion degree in more crucibles be made to decline, can obtain in a short time has uniformly
A large amount of sapphire single-crystals of quality.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 a-1c is respectively the Czochralski method of the prior art, heat exchange method, the monocrystalline maximum of Ji Luobo Loews method acquisition
Utilization rate schematic diagram；
Fig. 2 is Sapphire Crystal Growth device overlooking structure diagram disclosed in the embodiment of the present invention；
Fig. 3 is Sapphire Crystal Growth device side, sectional view disclosed in the embodiment of the present invention；
Fig. 4 is the method schematic diagram of the multiple seperated heater of control disclosed in the embodiment of the present invention；
Fig. 5 is the Sapphire Crystal Growth device disclosed in the embodiment of the present invention with 8 independent temperature control systems
Schematic diagram；
Fig. 6 is to carry out concatenated Sapphire Crystal Growth device to multiple seperated heater disclosed in the embodiment of the present invention
Schematic diagram.
Digital representation in figure:
10. 20. crucible of growth furnace, 21. reinforcing body
30. 40. heater 41. of thermal insulator assists heater
42. side heater 43. connects 44. electrode of heater
50. cooling body 60. crystallizes 62. seed crystals
70. 80. temperature tube of pyrometer, 90. height measuring device
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.
In particular, the structure of the specific composition of other Sapphire Crystal Growth devices, because with the look-ahead technique announced
It is similar, therefore at this moment will omit and state, the specific embodiments of the present invention constituted below for such as upper type are illustrated.
Embodiment 1: has the Sapphire Crystal Growth device of independent temperature control system
Sapphire Crystal Growth device specification and with material such as the following table 1:
As Figure 2-3,6 crucibles 20 forming a line in the growth furnace 10 with thermal insulator 30, corresponding crucible 20
2 auxiliary heaters 41, corresponding side heater 42 and the connection of reinforcing body 21,6 seperated heaters 40 and left and right ends
Heater 43, the electrode 44 of respective sides heater 42, respective temperature sensor (temperature tube 80 and pyrometer 70), corresponding crucible
In the cooling body 50 of 20 bottoms, the seed crystal 62 being arranged in crucible 20 and corresponding growth crystallization 60, and corresponding crucible 20
The height measuring device 90 of crystallization 60.
As shown in figure 5, realizing blue treasured using the Sapphire Crystal Growth device with 8 independent temperature control systems
Stone crystal growth.Firstly, being filled to each 6 crucibles 20, and risen from room temperature to 2110 DEG C after crushing the total 102kg of sapphire fragment
Temperature after 15 hours, is kept for 2 hours totally.Crystallization 60 is grown in the temperature of heater 40 and rises to 1920 DEG C with 0.2-5 DEG C/hr speed
Afterwards, slow cooling is carried out.Slow cooling is carried out in room temperature in 20 hours later.
In the sapphire growth device for having respective independent temperature control system, even if in optimal control algolithm and control
Under constant processed, the electric power applied to each heater 40 inevitably changes.That is, having independent temperature in each heater 40
When spending control system, the radiant heat from neighbouring heater 40 can impact temperature, this is because outside control ring
Influence caused by, therefore confirmed to lead to highly unstable movement.In addition, averagely being sent out to the electric power that each heater 40 applies
The difference of raw 2-10%, this phenomenon are judged as temperature sensor respectively caused by error.In addition, the temperature according to position does not have
There is face-off, can not avoiding moment, there is a phenomenon where 1 DEG C or more changes.When such as growing the sapphire monocrystalline of heavy caliber, press
Cool down according to the cooling velocity within long section needs per hour 0.5 DEG C, but as described above, rises 1 DEG C with temperature moment
The above changed device, growing high quality heavy caliber sapphire single-crystal is unsuitable.
Sapphire single-crystal after growth does not have the defects of bubble and crack (crack), but with after chip (wafer) processing
EPD (Etch Pit Density) is measured after being etched in 300 DEG C of KOH solution as a result, each position and chip are in the presence of poor
It is different, but its degree is average 500-1000/cm2 degree.
This compares (average 500-1000/cm2) with the chip used using previous technology, shows almost phase
The quality of same level.But the mass deviation respectively between crystallization 60 is larger, in addition it is existing mass-dispersion occur according to 60 positions of crystallization
As.In addition, 60 or so height of crystallization has differences, it is difficult to realize 60 growth of uniform crystallization of not mass-dispersion.Therefore, exist
Have in seperated heater 40 and the grower of independent temperature control system, after there is quality difference between crystallization 60, is changing
When attempting to improve quality after change growth conditions, it is difficult to reduce mass deviation.
Embodiment 2: single temperature sensor is used, and uses respective power control unit in multiple seperated heater 40
Sapphire growth device
As shown in figure 4, utilizing the Sapphire Crystal Growth device of embodiment 1, single temperature sensor and single temperature tune
Device is saved, the system for applying electric power to heater 40 corresponding with multiple independent power control device is constructed.As described in Example 1
Method has carried out 60 growth of crystallization and cooling procedure.
It is different from shown in embodiment 1, do not observe the electric power difference applied between respective seperated heater 40,
It acts highly stable.In embodiment 1, even if highly precisely being calibrated, no each heater 40 of normal direction is carried out equably
Power supply can not avoid the phenomenon that changing to the electric power moment that respective seperated heater 40 is supplied, in contrast, can be confirmed
The highly stable in a long time and good control performance of reproducibility.It is accordingly possible to ensure batch production sapphire single-crystal institute
The safety of the precision, equipment operation that need and reproducibility etc., the 60 current potential density of crystallization after growth equally show average 200-
300/cm2 degree, it may be said that be it is very outstanding, do not observe yet it is each crystallization 60 between mass deviation.
Embodiment 3: concatenated sapphire growth device is carried out to multiple seperated heater 40
Using the Sapphire Crystal Growth device in embodiment 1,2, constructs and use single temperature sensor as shown in Figure 6
With single thermoregulator, single power control unit is reused, and applies the system of electric power after 3 heaters 40 are connected.
It is adjusted in addition, implementing independent temperature to the auxiliary heater 40 at both ends.
As the temperature rises within 1900 DEG C that impedance also rises simultaneously for graphite heater 40 used in the present embodiment, but
Under its temperatures above, the tendency that has that as the temperature rises impedance declines instead.Therefore, in the crystallization 60 of about 2100 DEG C of degree
It grows under start temperature, when respective temperature difference such as occurs between concatenated each heater 40, low-temperature heating body 40 compares surrounding
Heater 40 has opposite impedance, therefore applying bigger voltage makes its calorific value increase (because electric current is identical, apply bigger electricity
Power).Therefore, the calorific value of low-temperature heating body 40 temperature while increasing also rises, and finally will be provided with temperature and tends to be identical
Property.On the contrary, calorific value is also reduced while the application voltage of high temperature exothermic body 40 reduces, finally have temperature downward trend,
Respectively fission 40 temperature of heater tends to keep uniform.
When 60 growth of crystallization, the difference of the electric power actually applied to heater 40 is difficult to the degree observed, and observes stop
In in error range.In addition, even in this case, the electric power applied to each heater 40 is more stable, and reproducibility is also excellent
It is elegant.The current potential density of the crystallization 60 grown by the above method also truthfully applies example 2,300-400/cm2 degree of average out to, compared with
It is outstanding, do not observe the mass deviation between each crystallization 60 yet.
But sapphire single crystal growth furnace 10 will keep the condition of high temperature for a long time, in addition the volatilization of fusant, unavoidably
It is impaired that heater 40 occurs for ground.It is impaired according to access times heater 40, in addition its impaired journey according to the position in growth furnace 10
Degree is also different, therefore with the increase of number of use, the electric current between heater 40 and voltage generation inevitably has occurred
Variation.That is, the impedance of heater 40 also becomes different according to the difference of the extent of damage of heater 40, hair is automatically determined therewith
The electric power of bifurcated between hot body 40, is difficult to find out from outside and is difficult to the method controlled, therefore, when such as thinking to reuse for a long time, by
Restriction is arrived.When actually in view of crystallizing 60 mass after growth, service limits is preferably limited within about 3 times.
In addition, in construct including sundries in the heater 40 and furnace constituted with graphite, therefore with using the time
Promote, start high-purity process, positive influence can be caused to monocrystalline quality using time longer growth, as the service life it is short frequently more
It changes, quality is adversely affected.Therefore, the method according to shown in embodiment 3, judgement are difficult to the indigo plant for carrying out having economic advantages
The industrialization production of jewel；Effect of the invention shown in embodiment 2 be it is very outstanding, judge in practical industry scene,
It can efficiently use.
The arrangement or effect and condition not being described in detail above, it is similar with disclosed look-ahead technique in advance, so this
In be omitted and illustrate and illustrate.
As above the specific part for describing the content of present invention in detail, has the industry people of usual knowledge, this skill
A kind of situation that art is only preferentially implemented is not to carry out limitation to the scope of the present invention to know better.Therefore, this hair
Bright essential scope should be defined with appended claims and its equivalent.
Claims (20)
1. a kind of multiple Sapphire Crystal Growth device characterized by comprising to guarantee that the internal temperature after heating rises to
It is more than the melting temperature of the high-purity alpha-alumina of sapphire raw material, the growth furnace heat-insulated from warmed body around；Positioned at the life
Long furnace interior, and from more crucibles of seeded growth monocrystalline while the sapphire raw material is melted；For melting the indigo plant
Raw material for gem and the multiple seperated heater installed outside the crucible；And to prevent the seed crystal from melting and shape completely
At upper and lower temperature gradient, in the cooling body that the bottom of the crucible is installed；
In above-mentioned Sapphire Crystal Growth device, to guarantee accurate temperature control inside the growth furnace and keeping single direction
The elongated growth furnace internal temperature is uniform, after arranging the multiple fission heater, uses single temperature sensor and temperature
Adjuster is spent, and is controlled after the power control unit connection corresponded with the multiple seperated heater.
2. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that the temperature sensor is height
Temperature meter, end carry out temperature measuring using the pipe for blocking shape.
3. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that the length of the heater is
5-50㎝。
4. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that the heater is close to described
Thermal insulator inner sidewall arrangement also has the multiple side heater respectively connected to unitary electrode and from the side heater
The connection heater that portion is attached.
5. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that the both ends of the growth furnace are also
A pair of of auxiliary heater is installed, and to control the power control unit powered and used to the auxiliary heater.
6. multiple Sapphire Crystal Growth device according to claim 5, which is characterized in that also have for being individually performed
The temperature control system that temperature is adjusted.
7. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that being will be from the single temperature
The information of adjuster output is inputted to the multiple power control unit for providing electric power after corresponding with the heater,
It is additionally provided with the signal distributor designed and produced with multiple output conversion regime.
8. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that further include protruding into the crucible
The interior height measuring device for being used to measure the height that raw material is melted or the monocrystalline height grown.
9. multiple Sapphire Crystal Growth device according to claim 1, which is characterized in that the shape of the crucible is four
It is angular, it is supported the crucible by the reinforcing body outside the crucible is arranged in and is inhibited the change of the crucible at high temperature
Shape.
10. multiple Sapphire Crystal Growth device according to claim 9, which is characterized in that the reinforcing body is set as
With the consistent quadrangle of the crucible.
11. multiple Sapphire Crystal Growth device according to claim 9, which is characterized in that the reinforcing body includes can
The bottom of assembly and disassembly and 4 side plates.
12. multiple Sapphire Crystal Growth device according to claim 9, which is characterized in that the material of the reinforcing body
For high-melting-point ceramics, tungsten or graphite.
13. multiple Sapphire Crystal Growth device according to claim 9, which is characterized in that the crucible and reinforcing body
Between for keep gap, contact surface is minimized using independent plate or needle, to inhibit to react.
14. multiple Sapphire Crystal Growth device according to claim 13, which is characterized in that in the crucible and reinforcing
The plate or needle material being inserted between body are by tungsten or molybdenum or its alloy.
15. multiple Sapphire Crystal Growth device according to claim 13, which is characterized in that in the crucible and reinforcing
The plate or needle being inserted between body are inserted into after reinforcing body processes groove, easy to install.
16. multiple Sapphire Crystal Growth device according to claim 13, which is characterized in that in the crucible and reinforcing
The plate or needle material being inserted between body are by tungsten or molybdenum or its alloy, plate one or more.
17. multiple Sapphire Crystal Growth device according to claim 16, which is characterized in that the material of multiple overlapping plates
Matter is respectively tungsten or molybdenum or one or more overlappings of its alloy.
18. a kind of multiple growth method of sapphire single crystal based on claim 8, which is characterized in that be included in more crucibles and protect
While holding uniform temperature, the stage for melting sapphire raw material, and the stage that crystallization is grown from seed crystal.
19. multiple growth method of sapphire single crystal according to claim 18, which is characterized in that in the crystalline growth stage,
Growth furnace interior temperature distribution is predicted after being measured from the monocrystalline height that respective crucible is grown, so that growth furnace internal temperature
It is evenly distributed, and after the speed of growth of the monocrystalline grown in respective crucible is consistent, it is final to realize high-quality multiple indigo plant
It is grown while jewel monocrystalline, also there is the step of being adjusted the Electric control mutually coped with each heater.
20. multiple growth method of sapphire single crystal according to claim 18, which is characterized in that the crystalline growth terminates
Afterwards, after cutting off cooling using cooling body before room temperature is cooling, while temperature is kept constant, also have and implement annealing
Stage.
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|---|---|---|---|---|
| CN102597334A (en) * | 2009-09-05 | 2012-07-18 | 科里斯科技有限公司 | Method and apparatus for growing a sapphire single crystal |
| KR101196445B1 (en) * | 2012-05-03 | 2012-11-01 | 주식회사 크리스텍 | Apparatus for Growing Sapphire Crystal and Method for Growing Sapphire Crystal Using the Same |
| KR101639627B1 (en) * | 2015-09-07 | 2016-07-14 | 에스엠엔티 주식회사 | Sapphire single crystal growing apparatus and method using of cruciable supporter |
| KR20170109335A (en) * | 2016-03-21 | 2017-09-29 | 에스엠엔티 주식회사 | Apparatus for growing grystal having auxiliary heat source member |
| CN210314564U (en) * | 2019-04-03 | 2020-04-14 | 贝民贤 | Multiple sapphire single crystal growth device |
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2019
- 2019-04-03 CN CN201910264838.4A patent/CN109898136A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102597334A (en) * | 2009-09-05 | 2012-07-18 | 科里斯科技有限公司 | Method and apparatus for growing a sapphire single crystal |
| KR101196445B1 (en) * | 2012-05-03 | 2012-11-01 | 주식회사 크리스텍 | Apparatus for Growing Sapphire Crystal and Method for Growing Sapphire Crystal Using the Same |
| KR101639627B1 (en) * | 2015-09-07 | 2016-07-14 | 에스엠엔티 주식회사 | Sapphire single crystal growing apparatus and method using of cruciable supporter |
| KR20170109335A (en) * | 2016-03-21 | 2017-09-29 | 에스엠엔티 주식회사 | Apparatus for growing grystal having auxiliary heat source member |
| CN210314564U (en) * | 2019-04-03 | 2020-04-14 | 贝民贤 | Multiple sapphire single crystal growth device |
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