阅读说明：本技术 一种激光辅助加热生长大尺寸晶体的方法及专用设备 (A kind of method and special equipment of laser auxiliary heating growing large-size crystal ) 是由 线全刚 张重远 金浩 于 2018-05-23 设计创作，主要内容包括：本发明的目的在于提供一种激光辅助加热生长大尺寸晶体的方法及专用设备,所述设备包括激光心部加热装置、氙灯表面加热装置、底座和真空腔体等,在制备晶体时,采用氙灯与激光协同加热的方式引晶生长。本发明通过对专用设备的结构和功能设计,在悬浮熔区的中央部位引入精度高且可控性强的激光加热热源,形成表面氙灯加热和心部激光加热的复合加热方式,并结合过对工艺过程的控制,解决了大尺寸试棒晶体的生长难题,使其可生长直径达30mm的晶体,以利于实现工程化应用。(The purpose of the present invention is to provide the methods and special equipment of a kind of laser auxiliary heating growing large-size crystal, the equipment includes laser center portion heating device, xenon lamp surface heating device, pedestal and vacuum cavity etc., when preparing crystal, seeding by the way of heating is cooperateed with to grow with laser using xenon lamp.The present invention is designed by the structure and function to special equipment, central part in suspension melting zone introduces the laser heat source that precision is high and controllability is strong, form the composite heating mode of the heating of surface xenon lamp and the heating of center portion laser, and combined control to technical process, solves the growth problem of large scale coupon crystal, make its can growth diameter reach 30mm crystal, in favor of realize engineering application.)

1. a kind of device of laser auxiliary heating growing large-size crystal, it is characterised in that: described device includes that laser center portion adds Thermal (1), xenon lamp surface heating device (2), pedestal (3) and vacuum cavity (4), in which:

Laser center portion heating device (1) is by laser condensing lens head (11), lens bracket (12), upper support bar (13) and optical fiber (15) Composition；Laser condensing lens head (11) is installed on lens bracket (12), and is connected by optical fiber (15) with laser (18)；Upper branch Strut (13) is hollow structure, is fixed on lens bracket (12) lower end by flange and sealing shroud (16), upper support bar (13) with Lens are equipped between laser condensing lens head (11)；

Feeding stick (33) is hollow structure, hangs on upper support bar (13) lower end；Seed crystal stick (34) is located under feeding stick (33) Side, and be fixed on lower support bar (35), lower support bar (35) is fixed on pedestal (3), feeding stick (33) and seed crystal stick (34) Between formed suspension melting zone (36)；

Xenon lamp surface heating device (2) is made of xenon lamp (21), ellipsoidal mirror (22) and xenon lamp fixed device (23), and xenon lamp is solid Determine device (23) to be located between lens bracket (12) and pedestal (3), for fixing xenon lamp (21) and ellipsoidal mirror (22), xenon lamp (21) it is arranged in ellipsoidal mirror (22) concave side, and face feeding stick (33)；

Vacuum cavity (4) is made of upper vacuum cavity (41), quartz ampoule (42) and lower vacuum cavity (43), upper vacuum cavity (41) Quartz ampoule (42) is fixed on centre with lower vacuum cavity (43)；Upper vacuum cavity (41), quartz ampoule (42) and lower vacuum cavity (43) it is connected by flange with vacuum cushion rubber between, forms a vacuum cavity；Upper support bar (13) lower end, feeding stick (33), it is internal to be in quartz ampoule (41) for seed crystal stick (34) and lower support bar (35) upper end.

2. according to the device of laser auxiliary heating growing large-size crystal described in claim 1, it is characterised in that: upper support bar (13) internal diameter is 12~15mm, outer diameter 20mm；Feeding stick (33) internal diameter is 12~15mm, and outer diameter is 32~35mm.

3. according to the device of laser auxiliary heating growing large-size crystal described in claim 1, it is characterised in that: lens bracket (12) lower part be equipped with adjustment device (17), for adjust lens bracket (12) height and with the angle of horizontal direction.

4. according to the device of laser auxiliary heating growing large-size crystal described in claim 1, it is characterised in that: upper support bar (13), lower support bar (35) is connected with rotating device respectively, for driving feeding stick (33) and seed crystal stick (34) to rotate；Upper support Bar (13) is connected with lifting device, for controlling the lifting of upper support bar (13).

5. according to the device of laser auxiliary heating growing large-size crystal described in claim 1, it is characterised in that: upper vacuum cavity (41) it is provided with the exhaust outlet of exhaust valve (31) on, the air inlet of intake valve (32) is provided on lower vacuum cavity (43).

6. a kind of method using claim 1 described device growing large-size crystal, it is characterised in that: added using laser assisted The device of thermally grown large-size crystals cooperates with seeding by the way of heating to grow using xenon lamp with laser.

7. according to the method for growing large-size crystal described in claim 6, which is characterized in that specific step is as follows:

1) preparation feeding stick (33) and seed crystal stick (34), are required according to ingredient and size, and they are separately fixed at upper support On bar (13), lower support bar (35)；

2) laser (18), optical fiber (15) and laser condensing lens head (11), are adjusted, laser beam is made to reach laser condensing lens head (11) Afterwards, the collimated light beam and upper support bar (13) central through hole, feeding for being focused into the collimated light beam of 3~Φ of Φ 5mm, and ensuring to focus Stick (33) central through hole is coaxial；

3), vacuum cavity (4) is vacuumized, its internal vacuum is made to reach 10^-3Then Pa opens intake valve (32) and exhaust valve (31), argon gas is continually fed into vacuum cavity (4)；

4) lifting device and rotating device, are opened, and sets lifting and velocity of rotation；

5) xenon lamp (21) and laser (18), are opened, feeding stick (33) is heated；Or xenon lamp (21) are first opened to feeding stick (33) external to be heated, after the melting zone that suspends (36) are established, it is then turned on laser (18) heating；

6) crystal, is finally prepared.

8. according to the method for growing large-size crystal described in claim 7, it is characterised in that: in step 4), feeding stick (33) and The rotation speed of seed crystal stick (34) is 0-30r/min, and feeding stick (33) is identical with seed crystal stick (34) direction of rotation or on the contrary, rotates Speed is identical or different.

9. according to the method for growing large-size crystal described in claim 7, it is characterised in that: in step 5), first open xenon lamp (21) after to heating 2-10min is carried out outside feeding stick (33), it is then turned on laser (18) heating；Xenon lamp power 1.0-5.0kw, Laser (18) heating power is uniformly adjusted to 0.1kw-1.0kw from 0W with the speed of 5-10W/min.

10. according to the method for growing large-size crystal described in claim 6, it is characterised in that: the crystalline substance that step 6) is finally prepared Body is having a size of diameter >=30mm.

Technical field

The present invention relates to the preparation methods of crystalline material, especially provide a kind of laser auxiliary heating growing large-size crystal Method and special equipment.

Background technique

Optics floating region furnace is a kind of suspension melting zone directional solidification furnace heated using light, with no crucible, high-cleanness, high temperature The features such as spending gradient and the fast speed of growth；The crystal growth for being widely used in the inter-metallic compound materials such as oxide and TiAl is ground Study carefully, especially those fusant reactions strongly and dystectic crystalline material.Present widely applied optics floating region furnace all uses 2 ~4 ellipsoidal reflectors focus xenon lamp heating, and melt maintains shape mainly by surface tension, grows along the vertical direction, such as Japan CSC The optics floating region furnace of the model FZ-T-12000-X-VP-S of company's production, is evenly equipped with 4 xenon lamps, and fusing point is up to 3000 DEG C, temperature Spend gradient be about 200 DEG C, the speed of growth can accurately be adjusted within the scope of 0~180mm/h, protective atmosphere up to 99.9999% with On, it is one of current optics floating region furnace the most advanced in the world.

However, since the heating method of such equipment is light heating, i.e. xenon source focal spot after ellipsoidal reflector focuses It is radiated at coupon surface, is then from outward appearance to inner essence gradually warmed up by heat transfer until melting.For different materials, when coupon is straight When diameter≤15mm, the center of coupon can melt it is thorough and it is inside and outside can stir evenly, suspension melting zone keep stablize, can be smooth Realize crystal growth；As coupon diameter > 15mm, easily leads to coupon center portion and surface is heated non-uniform phenomenon and occurred, coupon Center start to occur melting not thorough, suspension melting zone cannot keep stable and shape, crystal growth and can not carry out.For size For relatively large structural member, engineering application cannot achieve.Therefore, it is impossible to which growing bulky crystal has become optics floating region furnace Major defect.

Summary of the invention

, center portion fusing uneven for the heating in large scale coupon (diameter > 15mm) crystal growing process it is not thorough and The problems such as suspension melting zone is unstable the present invention provides a kind of method of laser auxiliary heating growing large-size crystal and dedicated sets It is standby, it is designed by structure and function to special equipment, the central part in suspension melting zone introduces that precision is high and controllability is strong Laser heat source, forms the composite heating mode of the heating of surface xenon lamp and the heating of center portion laser, and combines to technical process Control, solve the growth problem of large scale coupon crystal, make its can growth diameter >=30mm crystal, in favor of realize work Journey application.

Technical solution of the present invention is as follows:

A kind of device of laser auxiliary heating growing large-size crystal, it is characterised in that: described device includes laser center portion Heating device 1, xenon lamp surface heating device 2, pedestal 3 and vacuum cavity 4, in which:

Laser center portion heating device 1 is made of laser condensing lens head 11, lens bracket 12, upper support bar 13 and optical fiber 15； Laser condensing lens head 11 is installed on lens bracket 12, and is connected by optical fiber 15 with laser 18；Upper support bar 13 is hollow Structure is fixed on 12 lower end of lens bracket by flange and sealing shroud 16, sets between upper support bar 13 and laser condensing lens head 11 There are lens, while passing through laser, and plays sealing function；

Feeding stick 33 is hollow structure, hangs on 13 lower end of upper support bar；Seed crystal stick 34 is located at the lower section of feeding stick 33, and It is fixed on lower support bar 35, lower support bar 35 is fixed on the base 3, and suspension melting zone is formed between feeding stick 33 and seed crystal stick 34 36；

Xenon lamp surface heating device 2 is made of the fixed device 23 of xenon lamp 21, ellipsoidal mirror 22 and xenon lamp, the fixed dress of xenon lamp 23 are set between lens bracket 12 and pedestal 3, for fixing xenon lamp 21 and ellipsoidal mirror 22, the setting of xenon lamp 21 is anti-in ellipsoid 22 concave side of light microscopic, and face feeding stick 33；

Vacuum cavity 4 is made of upper vacuum cavity 41, quartz ampoule 42 and lower vacuum cavity 43, upper vacuum cavity 41 and lower true Cavity body 43 by quartz ampoule 42 be fixed on it is intermediate (upper vacuum cavity 41 is located between lens bracket 12 and xenon lamp fixation device 23, Quartz ampoule 42 is located between the fixed device 23 of xenon lamp and pedestal 3, and lower vacuum cavity 43 is located at 3 lower section of pedestal)；Upper vacuum cavity 41, it is connected by flange with vacuum cushion rubber between quartz ampoule 42 and lower vacuum cavity 43, forms a vacuum cavity；Upper support 13 lower end of bar, feeding stick 33, seed crystal stick 34 and 35 upper end of lower support bar are in inside quartz ampoule 41.

As a preferred technical scheme:

13 internal diameter of upper support bar is 12~15mm, outer diameter 20mm；33 internal diameter of feeding stick be 12~15mm, outer diameter be 32~ 35mm。

12 lower part of lens bracket be equipped with adjustment device 17, for adjust lens bracket 12 height and with horizontal direction Angle.

Upper support bar 13, feeding stick 33, seed crystal stick 34 and lower support bar 35 are coaxial.

It is provided with the exhaust outlet of exhaust valve 31 on upper vacuum cavity 41, is provided with intake valve 32 on lower vacuum cavity 43 Air inlet.

Air-cooled connector and/or water-cooling joint are equipped at laser condensing lens head 11.

Upper support bar 13, lower support bar 35 are connected with rotating device respectively, for driving feeding stick 33 and 34 turns of seed crystal stick It is dynamic；Upper support bar 13 is connected with lifting device, for controlling the lifting of upper support bar 13.

Xenon lamp 21 is identical with the quantity of ellipsoidal mirror 22, is 2-6, is evenly distributed on the surrounding of feeding stick 33.

The present invention also provides a kind of methods using described device growing large-size crystal, it is characterised in that: utilizes and swashs Light assists the device of heat growth large-size crystals, cooperates with seeding by the way of heating to grow with laser using xenon lamp, specific steps It is as follows:

1) preparation feeding stick 33 and seed crystal stick 34, are required according to ingredient and size, and they are separately fixed at upper support On bar 13, lower support bar 35；

2) laser 18, optical fiber 15 and laser condensing lens head 11, are adjusted, after so that laser beam is reached laser condensing lens head 11, The collimated light beam and 13 central through hole of upper support bar, feeding stick 33 for being focused into the collimated light beam of 3~Φ of Φ 5mm, and ensuring to focus Central through hole is coaxial；

3), vacuum cavity 4 is vacuumized, its internal vacuum is made to reach 10^-3Then Pa opens intake valve 32 and exhaust valve 31, argon gas (preferably 2L/min) is continually fed into vacuum cavity 4；

4) lifting device and rotating device, are opened, and sets lifting and velocity of rotation；

5) xenon lamp 21 and laser 18, are opened, feeding stick 33 is heated；Or first open xenon lamp 21 to feeding stick 33 outside Portion is heated, and after the melting zone 36 that suspends is established, is then turned on the heating of laser 18；

6) crystal, is finally prepared.

As a preferred technical scheme:

In step 4), the rotation speed of feeding stick 33 and seed crystal stick 34 is 0-30r/min, and feeding stick 33 and seed crystal stick 34 revolve Turn that direction is identical or on the contrary, rotation speed is identical or different.

In step 5), after first opening xenon lamp 21 to heating 2-10min is carried out outside feeding stick 33, it is then turned on laser 18 and adds Heat, to grow the crystal of better quality；Xenon lamp power 1.0-5.0kw, 18 heating power of laser is from 0W with 5-10W/min's Speed is uniformly adjusted to 0.1kw-1.0kw.

The crystalline size that step 6) is finally prepared is diameter >=15mm, more preferably having a size of diameter >=30mm.

The present invention uses hollow upper support bar and hollow feeding stick by increasing laser center portion heating device, will gather Burnt good laser light source passes through the center portion of upper support bar and feeding stick, and the central area in suspension melting zone is irradiated to from top, thus Realize the composite heating effect of the heating of xenon lamp surrounding and the heating of laser top center；In combination with excessively to the control of technical process, It is uniformly heated the surface in suspension melting zone with center portion consistent, melting zone, which is realized, stablizes growth, and temperature gradient further increases, Gu Liquid interface is improved, to improve the seeding success rate of large-size crystals and crystal quality, the present invention grow diameter for the first time Up to the crystal of 33mm, solves the growth problem of large scale coupon (diameter >=30mm) crystal.

Detailed description of the invention

The apparatus structure schematic diagram of Fig. 1 laser auxiliary heating growth crystal.

Fig. 2 laser center portion schematic diagram of heating device.

Appended drawing reference: 1, laser center portion heating device, 2, xenon lamp surface heating device, 3, pedestal, 4, vacuum cavity, 11, Laser condensing lens head, 12, lens bracket, 13, upper support bar, 15, optical fiber, 16, sealing shroud, 17, adjustment device, 18, laser, 21, xenon lamp, 22, ellipsoidal mirror, 23, the fixed device of xenon lamp, 31, exhaust valve, 32, intake valve, 33, feeding stick, 34, seed crystal Stick, 35, lower support bar, 36, suspension melting zone, 41, upper vacuum cavity, 42, quartz ampoule, 43, lower vacuum cavity.

Specific embodiment

As shown in Figure 1, a kind of device of laser auxiliary heating growth crystal, including laser center portion heating device 1, xenon lamp table Face heating device 2, pedestal 3 and vacuum cavity 4, in which:

Laser center portion heating device 1 is made of laser condensing lens head 11, lens bracket 12, upper support bar 13 and optical fiber 15； Laser condensing lens head 11 is installed on lens bracket 12, and is connected by optical fiber 15 with laser 18, and laser condensing lens head 11 exists Position and adjustable angle on horizontal and vertical direction；Upper support bar 13 is hollow structure (internal diameter 12mm, outer diameter 20mm), It is fixed on 12 lower end of lens bracket by flange and sealing shroud 16, is equipped between upper support bar 13 and laser condensing lens head 11 saturating Mirror, the lens are sealed with sealing shroud 16, the effect of lens are as follows: keep leading to laser smoothly while 4 vacuum degree of vacuum cavity Cross the center that upper support bar 13 reaches suspension melting zone 36；

Feeding stick 33 is hollow structure (internal diameter 15mm, outer diameter 32mm), hangs on 13 lower end of upper support bar, is assembled When, upper support bar 13 and 33 central through hole height of feeding stick need to be kept coaxial, to ensure that optical path is unimpeded；Seed crystal stick 34 is located at feeding The lower section of stick 33, and being fixed on lower support bar 35, lower support bar 35 is fixed on the base 3, feeding stick 33 and seed crystal stick 34 it Between formed suspension melting zone 36；

Xenon lamp surface heating device 2 is made of the fixed device 23 of xenon lamp 21, ellipsoidal mirror 22 and xenon lamp, the fixed dress of xenon lamp 23 are set between lens bracket 12 and pedestal 3, for fixing xenon lamp 21 and ellipsoidal mirror 22, the setting of xenon lamp 21 is anti-in ellipsoid 22 concave side of light microscopic, feeding stick 33 are located at a focal point of ellipsoidal mirror 22；Xenon lamp 21 and ellipsoidal mirror 22 are respectively provided with 4 It is a, it is evenly distributed on the surrounding of feeding stick 33；

Vacuum cavity 4 is made of upper vacuum cavity 41, quartz ampoule 42 and lower vacuum cavity 43, and upper vacuum cavity 41 is located at mirror Between head bracket 12 and the fixed device 23 of xenon lamp, quartz ampoule 42 is located between the fixed device 23 of xenon lamp and pedestal 3, lower vacuum cavity 43 are located at 3 lower section of pedestal；It is connected by flange with vacuum cushion rubber between upper vacuum cavity 41, quartz ampoule 42 and lower vacuum cavity 43 It is logical, form a vacuum cavity；13 lower end of upper support bar, feeding stick 33, seed crystal stick 34 and 35 upper end of lower support bar are coaxial, and Inside quartz ampoule 41, it is provided with the exhaust outlet of exhaust valve 31 on upper vacuum cavity 41, band is set on lower vacuum cavity 43 The air inlet of some intake valves 32.

Upper support bar 13, lower support bar 35 are connected with rotating device respectively, for driving feeding stick 33 and 34 turns of seed crystal stick It is dynamic；Upper support bar 13 is connected with lifting device, for controlling the lifting of upper support bar 13.

Crystal preparation process is as follows:

1) preparation feeding stick 33 and seed crystal stick 34, are required according to ingredient and size, and they are separately fixed at upper support On bar 13, lower support bar 35；

2) laser 18, optical fiber 15 and laser condensing lens head 11, are adjusted, after so that laser beam is reached laser condensing lens head 11, The collimated light beam and 13 central through hole of upper support bar, feeding stick 33 for being focused into the collimated light beam of 3~Φ of Φ 5mm, and ensuring to focus Central through hole is coaxial；

3), vacuum cavity 4 is vacuumized, its internal vacuum is made to reach 10^-3Then Pa opens intake valve 32 and exhaust valve 31, argon gas (2L/min) is continually fed into vacuum cavity 4；

4) lifting device and rotating device, are opened, and sets lifting and velocity of rotation；

5) xenon lamp 21 and laser 18, are opened, feeding stick 33 is heated；Or first open xenon lamp 21 to feeding stick 33 outside Portion is heated, and after the melting zone 36 that suspends is established, is then turned on the heating of laser 18；

6) crystal, is finally prepared.