CN104962995B - The grower and method of a kind of nitride single-crystal - Google Patents
The grower and method of a kind of nitride single-crystal Download PDFInfo
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- CN104962995B CN104962995B CN201510436581.8A CN201510436581A CN104962995B CN 104962995 B CN104962995 B CN 104962995B CN 201510436581 A CN201510436581 A CN 201510436581A CN 104962995 B CN104962995 B CN 104962995B
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Abstract
The invention discloses a kind of grower of nitride single-crystal and method, including reactor, growth solution is filled with reactor, reactor bottom, which is provided with the top of crystal seed template, reactor, is provided with nitrogen inlet, provided with pressure-regulating valve door in the nitrogen inlet, it is characterized in that, provided with the vortex generating means of growth solution formation vortex are made in the reactor, the vortex generating means are air flow system, nitrogen pipeline system or solution return-flow system, make the growth solution formation vortex in reactor.The present invention effectively overcomes the shortcoming that traditional reaction unit solution convection current is unordered and the supply of N sources is not enough, effectively increases crystal mass and uniformity.
Description
Technical field
The present invention relates to a kind of grower of nitride single-crystal and method.
Background technology
Gallium nitride as third generation semi-conducting material main representative, with the Optimality such as broad-band gap, high withstand voltage, highly thermally conductive
Can, the focus as research concern.Compared to other method, sodium stream method（Na Flux）Growth conditions it is more gentle（700~
1000 DEG C, 4~5MPa）And crystal mass is preferably, the method most potential as gallium nitride material is prepared.Traditional sodium stream method is anti-
Kettle is answered, it is general using overall heating response kettle and single channel nitrogen gas path pipe, not only easily produce unordered convection current, and gas-liquid interface
Polycrystalline is easily produced, hinders N fully to participate in reaction into solution, causes crystal growth slow and crystal mass is relatively low.How to enter
One step improves the solubility and uniformity of N in solution, the key issue as influence gallium nitride single crystal growth.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of nitride single-crystal that vortex can be produced in reactor
Grower and method.
In order to solve the above-mentioned technical problem, the present invention takes following technical scheme：
Growth solution, reactor bottom are filled with a kind of grower of nitride single-crystal, including reactor, reactor
Provided with crystal seed template, it is provided with the top of reactor in nitrogen inlet, the nitrogen inlet provided with pressure-regulating valve door, the reaction
Provided with the vortex generating means for being vortexed growth solution formation in kettle.
The vortex generating means be installed in reactor madial wall air flow system, the air flow system include airway tube and
With the driver that gas flows that makes of the airway tube attaching, the outlet terminal port of airway tube inside reactor with connecting.
The outlet terminal port of the airway tube is located at the ullage of the growth solution in reactor.
The outlet terminal port of the airway tube is located at below the liquid level of the growth solution in reactor and positioned at crystal seed template
Top.
The airway tube tilts down setting from the horizontal by 10~80 degree of angles.
The vortex generating means are nitrogen pipeline system, and the nitrogen pipeline system includes the nitrogen inlet with reactor
Nitrogen inlet duct is connected, the nitrogen inlet duct is located in reactor, and the outlet terminal port of the nitrogen inlet duct is located at growth
Below the liquid level of solution, nitrogen gas outlet is additionally provided with the top of reactor, pressure-regulating valve is provided with the nitrogen gas outlet.
The vortex generating means are solution return-flow system, and the solution return-flow system includes the backflow being arranged in reactor
Solution flow rate controller is provided with passage, return flow line, the bottom port of the return flow line is located at reactor inner bottom part, the backflow
The upper port of passage is located above crystal seed template and below the liquid level of growth solution.
The upper port of the return flow line tilts down setting from the horizontal by 15~60 degree.
A kind of growing method of nitride single-crystal, comprises the following steps：
S1, reactor inner bottom part is placed on by crystal seed template, the crystal seed template with horizontal positioned or from the horizontal by
40~60 degree of slant settings；
S2, toward reactor in placing response thing raw material；
S3, seals reactor, toward reactor in be passed through nitrogen, and reactor is heated, reaches the pressure of reactor
To 1~50MPa, temperature reaches 700~1000 DEG C；
S4, the growth solution flowing generation vortex made in reactor, the central distribution of the vortex is in the top of crystal seed template；
S5, crystal growth are reached after target thickness, are carried out decompression cooling to reactor, are then taken out crystal, growth response
Terminate.
The invention has the advantages that：
1. producing vortex inside solution, mixing effect is more preferable than thermal convection current, stirs more abundant, effectively facilitates reactant molten
Solution.
2. vortex brings the N of excess surface inside solution into, it might even be possible to directly reach seed surface, react more abundant,
Gas-liquid interface polycrystal layer is advantageously reduced, rate of crystalline growth is improved.
3. vortex centers are located at crystal seed template surface, raw material reaction is abundant, and growth is provided for multiple-piece crystal growth
Condition, reduces growth cost.
4. by placing multi-disc crystal seed template in reactor, effectively reduce production cost.
Brief description of the drawings
Accompanying drawing 1 is the structural representation of the embodiment of the present invention one；
Accompanying drawing 2 is the overlooking the structure diagram of accompanying drawing 1；
The view that accompanying drawing 3 is vortexed for the formation of the embodiment of the present invention one；
Accompanying drawing 4 is the structural representation of the embodiment of the present invention two；
Accompanying drawing 5 is the structural representation of the embodiment of the present invention three；
Accompanying drawing 6 is the structural representation of the embodiment of the present invention four；
Accompanying drawing 7 be the embodiment of the present invention three in nitrogen inlet duct outlet terminal port dimensional structure diagram；
Accompanying drawing 8 shows for the another form of stereochemical structure of the outlet terminal port of the nitrogen inlet duct in the embodiment of the present invention three
It is intended to；
Accompanying drawing 9 is the structural representation of the embodiment of the present invention five.
Accompanying drawing marks explanation：
In embodiment one:100：Reactor；110：Growth solution；111：Vortex；112：Solution flows back；120：Nitrogen air inlet
Mouthful；123：Pressure-regulating valve door；130：Crystal seed template；140：Air flow system.
In embodiment two： 200：Reactor；210：Growth solution；211：Vortex；212：Solution flows back；220：Nitrogen enters
Gas port；223：Admission line pressure valve；230：Crystal seed template；140：Air flow system.
In embodiment three： 300：Reactor；310：Growth solution；311：Vortex；312：Solution flows back；320：Nitrogen enters
Tracheae；321：Outlet terminal port；323：Pressure-regulating valve door in nitrogen inlet；324：Pressure regulation in nitrogen gas outlet
Valve；330：Crystal seed template.
In example IV： 400：Reactor；410：Growth solution；411：Vortex；412：Solution flows back；420：Nitrogen enters
Tracheae；421：Outlet terminal port；423：Pressure-regulating valve door in nitrogen inlet；424：Pressure regulation in nitrogen gas outlet
Valve；430：Crystal seed template.
In embodiment five： 500：Reactor；510：Growth solution；511：Vortex；512：The backflow of solution return-flow system is led to
Road；513：Current velocity regulator；520：Nitrogen inlet；523：Pressure-regulating valve door in nitrogen inlet；530：Crystal seed template.
Embodiment
For the ease of the understanding of those skilled in the art, the invention will be further described below in conjunction with the accompanying drawings.
Embodiment one, as shown in accompanying drawing 1,2 and 3, a kind of grower of nitride single-crystal, including reactor 100, reaction
Growth solution 110 is filled with kettle 100, the bottom of reactor 100 is provided with crystal seed template 130, and the top of reactor 100 is entered provided with nitrogen
Provided with pressure-regulating valve door 123 in gas port 120, the nitrogen inlet 120, being provided with the reactor 100 makes growth solution shape
Into the vortex generating means of vortex.The vortex generating means are the air flow system 140 installed in reactor madial wall, the air-flow system
System include airway tube 140 and with the airway tube attaching make gas flow driver, the outlet terminal port of airway tube 140 with instead
Answer connection inside kettle.Driver can be built in airway tube, and driver operation makes the nitrogen gas in reactor produce flowing.This
The outer driver for flowing gas is existing known products, if as small-sized driving fan or other can produce gas
Body flows.The outlet terminal port of airway tube is located at the ullage of the growth solution in reactor.The airway tube and level
Direction tilts down setting into 10~80 degree of angles, in the present embodiment one, and airway tube is preferably angular from the horizontal by 45 degree
It is lower to tilt.Outlet terminal mouth-shaped, diameter dimension and the without concrete restriction of airway tube, can flexibly set as needed.Such as will
The diameter of outlet terminal port is set to 5mm.Reactor inner bottom part places five crystal seed templates altogether, and one of them lies in a horizontal plane in instead
Answer bottom portion, four additional is uniformly placed on surrounding centered on the crystal seed template of the horizontal positioned, and be all with level
Placed into 60 degree of overturning angles in direction.In addition, in the present embodiment one, altogether provided with four airway tubes, and all from the horizontal by 45
Degree angle is tilted down.The outlet terminal port of four airway tubes is located on same circumference.
Extraneous nitrogen is entered in reactor by nitrogen inlet, starts air flow system, four airway tubes are to reaction
Nitrogen in kettle is regulated and controled, and is controlled flow velocity and the direction of nitrogen, the nitrogen is formed orderly flowing, the flow direction of nitrogen is tangential
Circumference, driving solution flowing downward from the horizontal by 45 °, so as to produce vortex 111,111 one side of vortex are sufficiently stirred for life
Long solution 110, accelerates reactant dissolving；On the other hand solution backflow 112 is produced, is made higher at the gas-liquid interface in reactor
Concentration N participates in reacting well into the internal-response area of solution 110；And vortex 111 is centrally located at the surface of crystal seed template 130, effectively
Improve crystal mass and uniformity.
Embodiment two, as shown in Figure 4, the present embodiment two and the structure of embodiment one are essentially identical, in reactor 200
Vortex generating means are also air flow system, and difference is the growth that the air flow system in the present embodiment two is located in reactor 200
Below the liquid level of solution 220 and above crystal seed template.The air flow system include airway tube 240 and with the airway tube attaching
The driver for flowing gas, the outlet terminal port of airway tube 240 is connected with the inside of reactor 200.Driver can be built in and lead
Tracheal strips, nitrogen enters from the nitrogen inlet 220 on reactor 200, the pressure that can be set by adjusting in nitrogen inlet
Regulating valve 223 adjusts nitrogen inlet, and driver operation makes the nitrogen gas in reactor 200 produce flowing.In addition make gas
Body flowing driver be existing known products, as long as small-sized driving fan or other can produce gas flowing i.e.
Can.Specially airway tube 240 is entirely located in the lower section of the liquid level of growth solution.In the present embodiment two, four are equally provided with
Airway tube, and all airway tube is all to tilt down setting into 45 degree of angles with horizontal direction.The outlet terminal of four airway tubes
Mouth is located on same circumference.
The tangential circumference of flow direction of nitrogen, driving solution flowing downward from the horizontal by 45 °, form vortex 211.Vortex
Tilted-putted crystal seed is distributed with above horizontal positioned crystal seed template 230, and on 211 flowing through channel of vortex in 211 central distributions
Template 230, the N sources needed for reaction can be substantially focused in crystal seed template 230, increase effectively reaction speed and crystal mass.
Embodiment three, as shown in accompanying drawing 5,6 and 7, the agent structure of the present embodiment three and the agent structure base of embodiment one
This is identical, and difference is vortex generating means concrete structure.A kind of grower of nitride single-crystal, including reactor 300, instead
Answer and growth solution 310 is filled with kettle 300, the bottom of reactor 300 is provided with crystal seed template 330, the top of reactor 300 is provided with nitrogen
Provided with pressure-regulating valve door 324 in air inlet, the nitrogen inlet, being provided with the reactor 300 makes growth solution formation whirlpool
The vortex generating means of stream.The vortex generating means are nitrogen pipeline system, and the nitrogen pipeline system includes and reactor 300
Nitrogen inlet connection nitrogen inlet duct 320, the nitrogen inlet duct 320 is located in reactor 300, and the nitrogen inlet duct
320 outlet terminal port 321 is located at below the liquid level of growth solution 310, and the top of reactor 300 is additionally provided with nitrogen gas outlet, should
Pressure-regulating valve 324 is provided with nitrogen gas outlet.Wherein the quantity of nitrogen inlet duct can flexibly be set as needed, herein simultaneously
Without concrete restriction.In the present embodiment three, be provided with four nitrogen inlet ducts altogether, each nitrogen inlet duct individually with extraneous gas
Source is connected, and an outlet terminal port is only set on each nitrogen inlet duct.The shape of outlet terminal port can for it is square, three
Angular, circular or other shapes, are not specifically limited herein, the size of same outlet terminal port also without concrete restriction,
It such as may be configured as diameter 5mm.In addition, outlet terminal port can be configured as angularly having a down dip from the horizontal by certain 10~80 degree
Tiltedly, in the present embodiment three, the outlet terminal port of nitrogen inlet duct is set to tilt down from the horizontal by 15 degree of angles.Pass through
The pressure-regulating valve of nitrogen inlet and the pressure-regulating valve of nitrogen gas outlet are controlled, can be had to the pressure in reactor
Effect regulation.
Nitrogen is in nitrogen inlet duct 320 is entered 310 in growth solution through outlet terminal port 321 again, terminal port diameter
5mm, from the horizontal by angle, 15 ° tilt down.Nitrogen drives solution to produce vortex 311, and 311 central distributions of vortex are in level
The top of crystal seed template 330 is placed, 311 one side of vortex are sufficiently stirred for growth solution 310, accelerate reactant dissolving；On the other hand
Solution backflow 312 is produced, the higher concentration N at the gas-liquid interface in reactor is joined well into the internal-response area of solution 310
With reaction；And vortex 311 is centrally located at the surface of crystal seed template 330, the N sources needed for reaction can be substantially focused on crystal seed template 330
On, it increase effectively reaction speed and crystal mass.
Example IV, the present embodiment four and embodiment three are essentially identical, and difference is that the outlet on nitrogen inlet duct is whole
The quantity of port is different.In embodiment three, an outlet terminal port is all only set on each nitrogen inlet duct.And this implementation
In example four, as shown in Figure 8, also it is provided with altogether on four nitrogen inlet ducts 420, each nitrogen inlet duct 420 and is both provided with three
Nitrogen outlet is provided with individual outlet terminal port 421, same reactor 400 and pressure regulation is provided with the nitrogen outlet
Pressure-regulating valve 423 is provided with valve 424, the nitrogen inlet being connected with nitrogen inlet duct 420.
Nitrogen is entered in growth solution 410 by terminal port, outlet terminal port diameter 5mm, from the horizontal by 15 ° of angle to
It is lower to tilt.Nitrogen drives solution to produce vortex 411, and 411 central distributions of vortex are in the top of horizontal positioned crystal seed template 430, vortex
411 one side are sufficiently stirred for growth solution 410, accelerate reactant dissolving；On the other hand solution backflow 412 is produced, makes reactor
Higher concentration N at gas-liquid interface in 400 participates in reacting well into the internal-response area of solution 410；And 411 centre bits of vortex
In the surface of crystal seed template 330, the N sources needed for reaction can be substantially focused in crystal seed template 430, increase effectively reaction speed and
Crystal mass.
Embodiment five, the present embodiment and the agent structure of embodiment one are essentially identical, and difference is the tool of vortex generating means
Body structure is different.As shown in Figure 9, filled in a kind of grower of nitride single-crystal, including reactor 500, reactor 500
There is growth solution 510, the bottom of reactor 500 is provided with crystal seed template 530, and the top of reactor 500 is provided with nitrogen inlet 520, should
Provided with pressure-regulating valve door 523 in nitrogen inlet 520, being provided with the reactor 500 makes the whirlpool of growth solution formation vortex
Stream generation apparatus.The vortex generating means are solution return-flow system, and the solution return-flow system includes being arranged in reactor 500
Solution flow rate controller 513 is provided with return flow line 512, return flow line 512, the bottom port of the return flow line 512 is located at instead
Answer the lower section of kettle 500.Solution flow rate controller can be water pump or the controller of other guiding Solution flow rates, be existing known
The application of product, in this not go into detail.The upper port of return flow line is tilted down from the horizontal by 15~60 degree and set
Put.In the present embodiment using five crystal seed templates 530, one of crystal seed template is placed horizontally in the bottom of reactor 500
Heart district domain, remaining four crystal seed templates are uniformly distributed in the crystal seed of horizontal positioned to be placed from the horizontal by 60 degree of overturning angles
Template surrounding.
Shape, the size all without concrete restrictions of the terminal port of return flow line 512, spirit can be carried out according to actual needs
It is living to set.Solution is entered by bottom terminal mouthful, bottom terminal mouthful diameter 6mm, is flowed through flow speed controller, is flowed from top terminals mouthful
Go out, top terminals mouthful diameter 5mm, from the horizontal by angle, 30 ° tilt down.
Solution return-flow system is by guiding the olderly flowage of growth solution, so as to regulate and control the flow velocity that nitrogen enters growth solution
And direction, so as to produce vortex 511.It is vortexed 511 one side and is sufficiently stirred for reactant solution 510, accelerates reactant dissolving；It is another
Aspect produces solution backflow 512, makes the higher concentration N at gas-liquid interface participate in reacting well into the internal-response area of solution 510；
And vortex 511 is centrally located at the surface of crystal seed template 530, effectively increases crystal mass and uniformity.
On the other hand, present invention further teaches a kind of growing method of nitride single-crystal, comprise the following steps：
S1, reactor inner bottom part is placed on by crystal seed template, the crystal seed template with horizontal positioned or from the horizontal by
40~60 degree of slant settings.Can also be while holding multiple pieces crystal seed template, such as one piece horizontal positioned, other then slant setting be simultaneously
And be evenly distributed on around horizontal positioned.
S2, toward reactor in placing response thing raw material Ga, Na, C and corresponding additive, this is growing nitride single crystal
Common knowledge, no longer carefully state one by one herein.
S3, seals reactor, toward reactor in be passed through nitrogen, and reactor is heated, reaches the pressure of reactor
To 1~50MPa, temperature reaches 700~1000 DEG C, reaches the environment in reactor and meets crystal growth condition.
Nitrogen pressure and temperature in S4, reactor reach crystal growth condition（700~1000 DEG C of temperature, pressure 1~
50MPa）When, the life in reactor is made by above-described air flow system or nitrogen pipeline system or solution return-flow system
The flowing of long solution produces vortex, and the central distribution of the vortex is inclined in being distributed with the top of crystal seed template, and vortex flowing through channel
The crystal seed template tiltedly placed, reaction needed for N sources can be substantially focused in crystal seed template, increase effectively rate of crystalline growth and
Crystal mass.
S5, crystal growth are reached after target thickness, are carried out decompression cooling to reactor, are then taken out crystal, growth response
Terminate.
It should be noted that described above is not the restriction to technical solution of the present invention, the wound of the present invention is not being departed from
On the premise of making design, any obvious replacement is within protection scope of the present invention.
Claims (3)
1. being filled with growth solution in a kind of grower of nitride single-crystal, including reactor, reactor, reactor bottom is set
Have and be provided with the top of crystal seed template, reactor in nitrogen inlet, the nitrogen inlet provided with pressure-regulating valve door, the reactor
Interior be provided with makes the vortex generating means of growth solution formation vortex, it is characterised in that
The vortex generating means be installed in reactor madial wall air flow system, the air flow system include airway tube and with this
Airway tube attaching makes the driver that gas flows, and the outlet terminal port of airway tube is connected with reactor inside, airway tube and water
Square tilt down setting into 10~80 degree of angles, and the outlet terminal port of airway tube is located on same circumference；
Or, the vortex generating means are nitrogen pipeline system, and the nitrogen pipeline system includes the nitrogen air inlet with reactor
The nitrogen inlet duct of mouth connection, the nitrogen inlet duct is located in reactor, and the outlet terminal port of the nitrogen inlet duct is located at
Below the liquid level of growth solution, nitrogen gas outlet is additionally provided with the top of reactor, pressure-regulating valve, nitrogen are provided with the nitrogen gas outlet
The quantity of gas air inlet pipe is flexibly set as needed, and the outlet terminal port of nitrogen inlet duct is arranged to from the horizontal by 10~80
Degree angle is tilted down；
Or, the vortex generating means are solution return-flow system, and the solution return-flow system includes being arranged on returning in reactor
Solution flow rate controller is provided with circulation road, return flow line, the bottom port of the return flow line is located at reactor inner bottom part, this time
The upper port of circulation road be located at crystal seed template above and positioned at growth solution liquid level below, the upper port of return flow line with
Horizontal direction tilts down setting into 15~60 degree.
2. the grower of nitride single-crystal according to claim 1, it is characterised in that the outlet terminal of the airway tube
Mouth is located at the ullage of the growth solution in reactor.
3. the grower of nitride single-crystal according to claim 1, it is characterised in that the outlet terminal of the airway tube
Mouth is located at below the liquid level of the growth solution in reactor and above crystal seed template.
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Families Citing this family (4)
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| CN105420814B (en) * | 2015-11-26 | 2017-10-27 | 北京大学东莞光电研究院 | A kind of crystal growth reactor |
| CN105256372B (en) * | 2015-11-27 | 2018-09-07 | 北京大学东莞光电研究院 | A kind of GaN single crystal device |
| CN105442046B (en) * | 2016-01-11 | 2018-01-23 | 东莞市中镓半导体科技有限公司 | A kind of growing nitride single crystal device and method |
| CN105780124B (en) * | 2016-03-12 | 2018-05-22 | 东莞市中镓半导体科技有限公司 | A kind of laser assisted iii-v crystal growing apparatus and method |
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| CN1922345A (en) * | 2004-02-19 | 2007-02-28 | 松下电器产业株式会社 | Method of manufacturing compound single crystal and apparatus for manufacturing it |
| JP3929657B2 (en) * | 1999-09-29 | 2007-06-13 | 株式会社リコー | Crystal growth method and group III nitride crystal production method |
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| JP3929657B2 (en) * | 1999-09-29 | 2007-06-13 | 株式会社リコー | Crystal growth method and group III nitride crystal production method |
| CN1922345A (en) * | 2004-02-19 | 2007-02-28 | 松下电器产业株式会社 | Method of manufacturing compound single crystal and apparatus for manufacturing it |
| CN104047058A (en) * | 2013-03-13 | 2014-09-17 | 株式会社理光 | Method for producing group 13 nitride crystal and apparatus for producing the same |
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