CN109056054A - A kind of crystal oven and its growth technique of growing large-size monocrystalline - Google Patents
A kind of crystal oven and its growth technique of growing large-size monocrystalline Download PDFInfo
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- CN109056054A CN109056054A CN201810896121.7A CN201810896121A CN109056054A CN 109056054 A CN109056054 A CN 109056054A CN 201810896121 A CN201810896121 A CN 201810896121A CN 109056054 A CN109056054 A CN 109056054A
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- crystal
- crucible
- analogue body
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- czochralski method
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/28—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using weight changes of the crystal or the melt, e.g. flotation methods
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to technical field of crystal growth, more particularly to the crystal oven and its growth technique of a kind of growing large-size monocrystalline, czochralski method crystal oven provided by the invention, not only simple structure, it is cheap, and size of burner hearth is big, radial and axial temperature gradient is uniformly adjustable, temperature accuracy is controllable, simultaneously using graphene-silicon carbide rod heating, the disadvantage that hot-spot is vulnerable under conventional heating stick high temperature can be effectively improved, while being suitble to growing large-size and high quality crystal, crystal oven cost, large size single crystal suitable for mass production are greatly reduced;Cooperate czochralski method crystal oven provided by the invention, crystal growth technique provided by the invention, which can obtain diameter, may be up to 10 inches of crystal.
Description
Technical field
The invention belongs to technical field of crystal growth, and in particular to a kind of crystal oven of growing large-size monocrystalline and its growth
Technique.
Background technique
The most common method of crystal growth includes czochralski method, Bridgman-Stockbarger method, flame melt method etc..Wherein czochralski method, also referred to as
Czochralski method, is a kind of method of pulling growth monocrystalline from melt, traditional czochralski method crystal oven mainly by furnace body,
Intermediate frequency power supply, heating coil, balance, control system and cooling system composition, it is characterized in that crystal oven control precision is high, growth
Crystal isometrical spend.But for growing large-size monocrystalline, since the range of weighing of balance is limited, cooling system is complex,
Induced current heat so that melt above temperature gradient it is very big, large-size crystals can not be grown.In addition, traditional czochralski method is brilliant
The intermediate frequency power supply heating that body furnace uses, expensive, large-scale serial production higher cost.Now with downstream application field pair
The demand of large-size crystals is increasing, while more harsh requirement is proposed to the quality of crystal, therefore develops and be suitble to growth
Large-size crystals and quality height, low-cost crystal oven and its growth technique, it is very necessary.
Summary of the invention
To solve the deficiencies in the prior art, it is an object of the present invention to provide a kind of czochralski method crystal oven, not only constructs
Simply, cheap, and size of burner hearth is big, radial and axial temperature gradient is uniformly adjustable, temperature accuracy is controllable, uses simultaneously
Graphene-silicon carbide rod heating, can be effectively improved the disadvantage that hot-spot is vulnerable under conventional heating stick high temperature, be suitble to growth
While large scale and high quality crystal, crystal oven cost, large size single crystal suitable for mass production are greatly reduced.
It is a further object to provide a kind of large-size crystals growth technique, the crystal diameter that the technique obtains
Up to 10 inches.
For achieving the above object, the present invention the following technical schemes are provided:
A kind of czochralski method crystal oven, including furnace body, rotary pulling system, control system and analogue body Weighing system,
The surrounding of the furnace body is insulating brick, and middle bottom is fixed with scalable silicon nitride crucible support base, the crucible branch
Be equipped with crucible on support seat, the crucible top is equipped with insulation cover, and the top of the insulation cover is equipped with upper opening insulating brick, it is described on
Insulating brick top be open equipped with electroheat pair, the furnace interior, insulating brick and crucible supporting seat, crucible and insulation cover are formed whole
It is equipped with graphene-silicon carbide rod between body, can guarantee the uniformity and stability of heating, it is small to can be realized radial symmetry gradient
To 5 DEG C/cm, axial-temperature gradient can achieve 10 DEG C/cm, temperature accuracy ± 0.1 DEG C;
The rotary pulling system includes screw rod, and the top of the screw rod is equipped with lifting motor;
The control system includes temperature control table and control switch, and the control switch is for opening or closing graphene-carbon
The heating of SiClx stick, the temperature control table is for controlling graphene-silicon carbide rod heating temperature;
The analogue body Weighing system includes the support frame being fixed in the middle part of screw rod, support frame as described above can be with screw rod above and below
Movement, the arm beam of steelyard is set on support frame as described above, and the one end of the arm beam of steelyard far from rotary pulling system is by being equipped with the rope of hook
Line is connect with analogue body, and the arm beam of steelyard is connect by pallet with rotating electric machine close to one end of rotary pulling system, the rotation
The bottom end of motor is equipped with seed rod, can adjust arm beam of steelyard both ends balance by pallet, the analogue body is immersed equipped with suspension
In suspension cup, the analogue body Weighing system uses lever principle, and difference × stress point of gravity and buoyancy arrives at analogue body
The gravity of crystal for the distance of support frame=grow passes through adjusting at a distance from difference × rotating electric machine to support frame of buoyancy
Weight or torque are simulated, crystal diameter can be grown in 100~350mm range-controllable.
Further, the crucible is selected from platinum crucible, Iridium Crucible and graphite crucible.
Further, the crucible is shape with wide top and narrow bottom.
Further, the analogue body is simulated in nylon analogue body, quartz analogue body, plastics analogue body or organic glass
Body.
Further, the suspension is polyethylene glycol 400.
Czochralski method crystal oven of the invention is expensive by the analogue body Weighing system fictitious hosts built with lever principle
Electronic balance, utilize the difference of gravity at analogue body and buoyancy × at a distance from stress point to fulcrum=weight of the crystal grown
Power reaches a kind of principle of conservation of mass at a distance from difference × rotating electric machine to fulcrum of buoyancy, simulates constitution by adjusting
Amount or position, can obtain diameter range in the crystal of 100~350mm;Simultaneously can by change burner hearth insulating layer material,
Thickness, the size of diameter and insulation cover upper opening and angle realize the adjusting of thermal field;In addition, czochralski method crystal of the invention
Furnace uses graphene-silicon carbide rod resistance heating for the first time, it is ensured that the uniformity and stability of heating are conducive to control temperature
Gradient;Meanwhile of the invention czochralski method crystal oven manufacture craft it is simple, it is easy to operate, low, cost is required just to operator
Preferably, the crystal quality that can be grown the crystal of variety classes and property, and be grown is influenced smaller by personnel's operation, can be pushed away on a large scale
Extensively, mass production.
(3) analogue body crystal oven is with size of burner hearth is big, radial and axial temperature gradient is adjustable, temperature accuracy controllably exists
±0.1℃;
Second aspect, the present invention provide a kind of growth technique of czochralski method crystal oven growing large-size monocrystalline of the present invention, tool
Steps are as follows for body:
Step (1) inoculation: being packed into seed rod for seed crystal, select suitable analog body, keeps analogue body and seed rod holding horizontal
After state, rotating electric machine is opened, rotation speed is 5~8rpm, and graphene-silicon carbide rod is heated to polycrystal material in crucible and melts completely
Change, is cooled to 1350~1480 DEG C;
Step (2) shouldering: after the completion of inoculation, control pull rate is 1.5~3.0mm/h, when shouldering is to 1/3, turns automatic
Growth, while adjusting the crystal quality that analogue body is allowed to and grows and reaching dynamic equilibrium, 20~35h of isodiametric growth;
Step (3) cooling: after the completion of isodiametric growth, the crystal pull grown is gone out into liquid level, with the speed of 30~60 DEG C/h
Rate is cooled to 25~85 DEG C;
Step (4) annealing: the crystal that step (3) obtains is taken out after constant temperature 15h at 1140~1170 DEG C, decaptitating truncates
Afterwards in 40~50mA/cm2Electric current under polarize to obtain the final product.
Growth technique according to the present invention, the seed crystal are positive cube shape, crystal growth direction be [110],
[010], [001] or [104].
Detailed description of the invention
Fig. 1 is the overall structure diagram of czochralski method crystal oven of the present invention;
Fig. 2 is the furnace structure schematic diagram of czochralski method crystal oven of the present invention;
Fig. 3 is the rotary pulling system and analogue body Weighing system structural schematic diagram of czochralski method crystal oven of the present invention;
Fig. 4 is the analogue body Weighing system schematic illustration of czochralski method crystal oven of the present invention;
Fig. 5 be embodiment 1 grow large size single crystal, 8 inches of diameter;
In figure,
1- furnace body, 11- insulating brick, 12- crucible supporting seat, 13- crucible, 14- insulation cover, 15- upper opening insulating brick, 16-
Thermocouple, 17- graphene-silicon carbide rod;
2- rotary pulling system, 21- screw rod, 22- lift motor;
3- control system;
4- analogue body Weighing system, 41- support frame, the 42- arm beam of steelyard, 43- analogue body, 44- pallet, 45- rotating electric machine, 46-
Seed rod, 47- suspension cup.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, with reference to the accompanying drawings and detailed description
Invention is described further, but the present invention is not limited thereto.
As Figure 1-Figure 4, czochralski method crystal oven of the invention, including furnace body 1, rotary pulling system 2, control system 3
With analogue body Weighing system 4, the surrounding of the furnace body 1 is insulating brick 11, and middle bottom is fixed with scalable silicon nitride crucible support
Seat 12, is equipped with crucible 13 on the crucible supporting seat 12, and 13 top of crucible is equipped with insulation cover 14, the insulation cover 14 it is upper
Portion is equipped with upper opening insulating brick 15, is equipped with electroheat pair 16 beside the insulation cover 14, inside the furnace body 1, insulating brick 11 and earthenware
Graphene-silicon carbide rod 17 is used between the entirety that crucible support base 12, crucible 13 and insulation cover 14 are formed;
The rotary pulling system 2 includes screw rod 21, and the top of the screw rod 21 is equipped with lifting motor 22;
The control system 3 includes temperature control table and control switch, and the control switch is for opening or closing graphene-carbon
SiClx stick 17 heats, and the temperature control table is for controlling 17 heating temperature of graphene-silicon carbide rod;
The analogue body Weighing system 4 includes the support frame 41 for being fixed on 21 middle part of screw rod, and the arm beam of steelyard 42 is set to the branch
On support 41, the described one end of the arm beam of steelyard 42 far from rotary pulling system 2 is connect by being equipped with the rope yarn of hook with analogue body 43,
The arm beam of steelyard 42 is connect by pallet 44 in rotating electric machine 45 close to one end of rotary pulling system 2, the rotating electric machine 45
Bottom end seed rod 46 is housed, arm beam of steelyard both ends balance can be adjusted by pallet 44, the analogue body 43, which immerses, is equipped with suspension
Suspension cup 47 in;
Specifically, the crucible 13 is selected from platinum crucible, Iridium Crucible and graphite crucible;
Specifically, the crucible 13 is shape with wide top and narrow bottom;
Specifically, the analogue body 43 mould in nylon analogue body, quartz analogue body, plastics analogue body or organic glass
Quasi- body;
Specifically, the suspension is polyethylene glycol 400.
Embodiment 1: the growth of large-size crystals
Seed crystal is loaded on seed rod, selects suitable analogue body, adjusts analogue body and seed rod keeps horizontality, lead to
Electricity opens rotating electric machine, controls graphene-silicon carbide rod by temperature control table and heats up, so that the polycrystal material in platinum crucible melts,
Constant temperature starts to be inoculated with after one hour, and crystal growth direction is [104], and inoculation temperature is 1480 DEG C, rotation speed 5rpm, lifting
Speed is 1.5mm/h.The crystal matter for when shouldering is to 1/3, turning automatic growth, while adjusting the analogue body of arm beam of steelyard two sides and growing
Amount reaches dynamic equilibrium, and isodiametric growth is kept 20h, the crystal pull grown is gone out liquid level, is cooled to the rate of 30 DEG C/h
25℃.It anneals after crystal is taken out, constant temperature 15h under the conditions of 1160 DEG C.In 40mA/ after obtained crystal decaptitating is truncated
cm2Electric current under polarize, obtained crystal equal-diameter part diameter is about 150mm, as shown in Figure 5.
Embodiment 2: the growth of large-size crystals
Seed crystal is loaded on seed rod, adjusts analogue body and seed rod keeps horizontality, be powered, open rotating electric machine,
Graphene-Si-Mo rod heating is controlled by temperature control table, so that the polycrystal material in platinum crucible melts, constant temperature one hour starts to connect
Kind, crystal growth direction is [001], and inoculation temperature is 1350 DEG C, rotation speed 8rpm, pull rate 3.0mm/h.Shouldering
When to 1/3, turn automatic growth, while the crystal quality for adjusting the analogue body of arm beam of steelyard two sides and growing reaches dynamic equilibrium, etc.
Diameter growth keeps 35h, and the crystal pull grown is gone out liquid level, is cooled down 85 DEG C with the rate of 60 DEG C/h.Crystal is taken out laggard
Row annealing, constant temperature 15h under conditions of 1170 DEG C.In 50mA/cm after obtained crystal decaptitating is truncated2Electric current under carry out pole
Change, obtained crystal diameter is about 100mm.
Embodiment 3: the growth of large-size crystals
Seed crystal is loaded on seed rod, adjusts analogue body and seed rod keeps horizontality, be powered, open rotating electric machine,
Graphene-Elema heating is controlled by temperature control table, so that the polycrystal material in platinum crucible melts, constant temperature one hour starts to connect
Kind, crystal growth direction is [110], and inoculation temperature is 1420 DEG C, rotation speed 6rpm, pull rate 2.0mm/h.Shouldering
When to 1/3, turn automatic growth, while the crystal quality for adjusting the analogue body of arm beam of steelyard two sides and growing reaches dynamic equilibrium, etc.
Diameter growth keeps 30h, and the crystal pull grown is gone out liquid level, is cooled down 75 DEG C with the rate of 40 DEG C/h.Crystal is taken out laggard
Row annealing, constant temperature 15h under conditions of 1160 DEG C.In 45mA/cm after obtained crystal decaptitating is truncated2Electric current under carry out pole
Change, obtained crystal diameter is about 200mm.
Embodiment 4: the growth of large-size crystals
Seed crystal is loaded on seed rod, adjusts analogue body and seed rod keeps horizontality, be powered, open rotating electric machine,
Graphene-Elema heating is controlled by temperature control table, so that the polycrystal material in platinum crucible melts, constant temperature one hour starts to connect
Kind, crystal growth direction is [010], and inoculation temperature is 1460 DEG C, rotation speed 7rpm, pull rate 2.6mm/h.Shouldering
When to 1/3, turn automatic growth, while the crystal quality for adjusting the analogue body of arm beam of steelyard two sides and growing reaches dynamic equilibrium, etc.
Diameter growth keeps 28h, and the crystal pull grown is gone out liquid level, is cooled down 50 DEG C with the rate of 50 DEG C/h.Crystal is taken out laggard
Row annealing, constant temperature 15h under conditions of 1160 DEG C.In 48mA/cm after obtained crystal decaptitating is truncated2Electric current under carry out pole
Change, obtained crystal diameter is about 350mm.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.And these
Belong to the obvious changes or variations that spirit of the invention is extended out to be still in the protection scope of this invention.
Claims (7)
1. a kind of czochralski method crystal oven, including furnace body (1), rotary pulling system (2), control system (3) and analogue body weigh system
It unites (4),
The surrounding of the furnace body (1) is insulating brick (11), and middle bottom is fixed with scalable silicon nitride crucible support base (12), described
It is equipped on crucible supporting seat (12) crucible (13), crucible (13) top is equipped with insulation cover (14), the insulation cover (14)
Top is equipped with upper opening insulating brick (15), is equipped with electroheat pair (16) beside the insulation cover (14), and the furnace body (1) is internal, protects
Graphene-silicon carbide is used between the entirety that warm brick (11) and crucible supporting seat (12), crucible (13) and insulation cover (14) are formed
Stick (17);
The rotary pulling system (2) includes screw rod (21), and the top of the screw rod (21) is equipped with lifting motor (22);
The control system (3) includes temperature control table and control switch, and the control switch is for opening or closing graphene-carbonization
Silicon rod (17) heating, the temperature control table is for controlling graphene-silicon carbide rod (17) heating temperature;
The analogue body Weighing system (4) includes the support frame (41) being fixed in the middle part of screw rod (21), and the arm beam of steelyard (42) is set to institute
It states on support frame (41), the one end of the arm beam of steelyard (42) far from rotary pulling system (2) is by being equipped with the rope yarn and mould of hook
Quasi- body (43) connection, the arm beam of steelyard (42) pass through pallet (44) and rotating electric machine (45) close to the one end of rotary pulling system (2)
The bottom end of connection, the rotating electric machine (45) is equipped with seed rod (46), can adjust arm beam of steelyard both ends balance, institute by pallet (44)
Analogue body (43) are stated to immerse in the suspension cup (47) equipped with suspension.
2. czochralski method crystal oven as described in claim 1, it is characterised in that: the crucible (13) is selected from platinum crucible, iraurite
Crucible and graphite crucible.
3. czochralski method crystal oven as described in claim 1, it is characterised in that: the crucible (13) is shape with wide top and narrow bottom.
4. czochralski method crystal oven as described in claim 1, it is characterised in that: the analogue body (43) be selected from nylon analogue body,
Analogue body in quartz analogue body, plastics analogue body or organic glass.
5. czochralski method crystal oven as described in claim 1, it is characterised in that: the suspension is polyethylene glycol 400.
6. the growth technique of czochralski method crystal oven growing large-size monocrystalline as described in claim 1, the specific steps are as follows:
Step (1) inoculation: being packed into seed rod for seed crystal, select suitable analog body, and analogue body and seed rod is made to keep horizontality
Afterwards, rotating electric machine is opened, rotation speed is 5~8rpm, and graphene-silicon carbide rod is heated to polycrystal material in crucible and melts completely,
It is cooled to 1350~1480 DEG C;
Step (2) shouldering: after the completion of inoculation, control pull rate is that 1.5~3.0mm/h turns automatic growth when shouldering is to 1/3,
Adjusting the crystal quality that analogue body is allowed to and grows reaches dynamic equilibrium, 20~35h of isodiametric growth simultaneously;
Step (3) cooling: after the completion of isodiametric growth, going out liquid level for the crystal pull grown, is dropped with the rate of 30~60 DEG C/h
Temperature is to 25~85 DEG C;
Step (4) annealing: the crystal that step (3) obtains is taken out after constant temperature 15h at 1140~1170 DEG C, decaptitating truncate after
40~50mA/cm2Electric current under polarize to obtain the final product.
7. growth technique as claimed in claim 6, step (1) described seed crystal is positive cube shape, and crystal growth direction is
[110], [010], [001] or [104].
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Citations (5)
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CH648122A5 (en) * | 1980-07-09 | 1985-02-28 | Vyzk Ustav Keramiky | Sedimentation balance |
JPH0255290A (en) * | 1988-08-19 | 1990-02-23 | Mitsubishi Metal Corp | Method for growing high-dissociation pressure compound semiconductor single crystal and apparatus therefor |
CN203411656U (en) * | 2013-07-30 | 2014-01-29 | 元亮科技有限公司 | Lower weighing device for crystal oven |
CN104202848A (en) * | 2014-08-08 | 2014-12-10 | 苏州宏久航空防热材料科技有限公司 | High conductive and high thermal radiation carbon crystal powder and preparation method thereof |
CN104562183A (en) * | 2014-12-31 | 2015-04-29 | 西南技术物理研究所 | Method for growing large-sized rare-earth-doped barium yttrium fluoride single crystals |
-
2018
- 2018-08-08 CN CN201810896121.7A patent/CN109056054A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CH648122A5 (en) * | 1980-07-09 | 1985-02-28 | Vyzk Ustav Keramiky | Sedimentation balance |
JPH0255290A (en) * | 1988-08-19 | 1990-02-23 | Mitsubishi Metal Corp | Method for growing high-dissociation pressure compound semiconductor single crystal and apparatus therefor |
CN203411656U (en) * | 2013-07-30 | 2014-01-29 | 元亮科技有限公司 | Lower weighing device for crystal oven |
CN104202848A (en) * | 2014-08-08 | 2014-12-10 | 苏州宏久航空防热材料科技有限公司 | High conductive and high thermal radiation carbon crystal powder and preparation method thereof |
CN104562183A (en) * | 2014-12-31 | 2015-04-29 | 西南技术物理研究所 | Method for growing large-sized rare-earth-doped barium yttrium fluoride single crystals |
Non-Patent Citations (1)
Title |
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