CN217351616U - Large-size sapphire plate growth device adopting mold guide method - Google Patents

Abstract

The utility model discloses a jumbo size sapphire board die guide method growth device, the induction cooker comprises a cooker bod, the furnace body both sides are to opening the door structure mutually, adopt platelike graphite resistance heater, and the hard felt of graphite is as insulation material, and whole thermal field is the dual temperature zone structure, and circular crucible has four platelike graphite heaters all around, for the main zone of heating, is equipped with the afterheater in the both sides of sapphire board big face parallel, and main heating and afterheating warm area are separated both as the heat screen by the hard felt of graphite, and the heat screen level is placed in crucible lid upper portion and is located the mould both sides. The utility model discloses the design of dual-temperature zone avoids crystal stress too big production dislocation, defects such as fracture, avoids the high temperature because the fluctuation of fuse-element temperature leads to the crystal to produce the bubble, ensures the high quality of crystal.

Description

Large-size sapphire plate growth device adopting mold guide method

Technical Field

The utility model relates to a crystal material preparation technical field especially relates to a jumbo size sapphire sheet die guide method growth device.

Background

With the rapid development of the photoelectric/infrared system for military and civil use, people have urgent needs for large-area photoelectric window materials (the length and the width are more than or equal to 250mm), and meanwhile, the requirements for high hardness, high strength, wide waveband and high transmittance are more and more strong on the performance of the window materials. For example, infrared transmittance indices and abrasion resistance are important indices for photovoltaic windows, infrared sash windows, ranging and tracking instrument windows for aircraft, ships and ground vehicles.

The sapphire single crystal is used as an excellent wide-waveband light-transmitting material, has good wave-transmitting rate in ultraviolet, visible light, infrared waveband and microwave, and can meet the requirement of multi-mode composite guidance; meanwhile, the sapphire single crystal has excellent mechanical property, chemical stability and high temperature resistance, high strength and high hardness, and can work in a severe environment of nearly 2000 ℃, so the sapphire single crystal is an optimal photoelectric window material. Although large-sized sapphire crystals have numerous applications in various fields of military use and civil use, the export of related technologies and materials is prohibited in western countries such as the united states, so that large-sized high-quality sapphire crystals cannot be sufficiently supplied internationally.

The most common shape of window material is flat. Currently, the main production methods of large-size sapphire single crystals include a heat exchange method, a kyropoulos method, a horizontally oriented zone melting method, a mold guiding method and the like. Due to the technical difference, the mold-guiding method (also called EFG method) and the horizontal orientation zone melting method are most suitable for the production of large-size sapphire single crystal plates. Both have the advantage that large-size single crystals in the form of plates can be produced directly. The produced crystal blank is a plate with the size close to the target size, and no additional processing is needed except grinding and polishing. The horizontal directional zone-melting method has been able to grow sapphire panels with maximum size of 457mm x 914mm x 38mm, manufactured by Rubicon Technology, inc, of american company, which is still in the laboratory stage due to excessive stress and low mechanical strength of the grown crystals, limiting the range of application, whereas the large size sapphire plates grown by the guided mode method have been industrially produced in saint gobain, france. Another main advantage of growing the sapphire large plate by the guided mode method is that the crystal growth speed of the sapphire large plate grown by the guided mode method is high and reaches up to 25mm/h, the whole crystal growth period only needs 3 days, the crystal growth speeds of other growing methods are all below 5mm/h, and the whole crystal growth period is about 2 weeks.

However, the technology of large-size (more than or equal to 250mm) high-quality sapphire plate growth by a mold-guiding method is still blank at present; and other crystal growth methods cannot process large-size (more than or equal to 250mm) sapphire plates in size or quality. Even if occasionally obtaining high quality crystals allows large sapphire plates to be processed, it is expensive and cannot meet the requirements of mass production. For example, the most common method for producing large-size sapphire crystals in the industry is the kyropoulos method or the heat exchange method, the product is an approximately cylindrical sapphire ingot, and a sapphire single crystal plate is required to be produced by means of cutting processing. And the crystal growth and processing cycle of the mode is long, the waste of crystal raw materials is serious, and meanwhile, when the cutting is carried out, a plate-shaped area which has no bubble layer and meets the requirements of strength and wave transmittance is difficult to find in the cylindrical crystal interval.

SUMMERY OF THE UTILITY MODEL

1. Technical problem to be solved

The utility model aims at solving the problems in the prior art and providing a growth device of a large-size sapphire plate by a die-guide method.

2. Technical scheme

In order to realize the purpose, the utility model adopts the following technical scheme:

the utility model provides a jumbo size sapphire board die-guiding method growth device, includes the furnace body, the furnace body both sides are to the structure of opening the door mutually, adopt plate graphite resistance heater, and the hard felt of graphite is as insulation material, and whole thermal field is two warm area structures, and circular crucible has four slice plate form graphite heaters all around, for the main zone of heating, is equipped with the afterheater in the parallel both sides of sapphire board large face, and main heating separates both with the afterheating warm area as the heat screen by the hard felt of graphite, and the heat screen level is placed in crucible cover upper portion and is located the mould both sides.

Preferably, the main heating zone and the rear heating zone are independently controllable.

Preferably, the die is a splicing structure of two plane plates, the width of the die is 250-450mm, the thickness of the die is 8-30mm, the height of the die is 40-150mm, the width of the middle capillary seam is 0.2-2mm, and the top of the die is at an included angle of 90-180 degrees.

Preferably, the large surface of the sapphire plate is an A surface, the pulling direction is an M direction or a C direction, and the length of the sapphire plate is 400-1000 mm.

Preferably, the crucible material is molybdenum, tungsten, iridium or rhenium.

Preferably, the material of the mould is molybdenum, tungsten, iridium or rhenium.

Preferably, the furnace body is a cuboid.

Preferably, the crucible is fixedly connected with the inner bottom of the furnace body through a crucible supporting rod.

3. Advantageous effects

Compared with the prior art, the utility model has the advantages of:

(1) the utility model discloses in, the design of dual temperature area avoids crystal stress too big dislocation that produces, defects such as fracture, avoids under the high temperature because the fluctuation of fuse-element temperature leads to the crystal gassing, ensures the high quality of crystal.

(2) The utility model discloses in, can grow maximum width 450 mm's high quality sapphire panel, satisfy domestic eager demand to jumbo size photoelectric window and transparent armoured.

Drawings

Fig. 1 is a boiling point diagram of a large-size sapphire plate growth device by a die-casting method according to the present invention;

fig. 2 is the utility model provides a structural schematic diagram of jumbo size sapphire sheet die-guiding growth device.

In the figure: 1-plate-shaped graphite heaters; 2-graphite hard felt; 3-covering the crucible; 4-a crucible; 5 sapphire plate; 6-molding; 7-graphite hard felt; 8-crucible support rods; 9-furnace body.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

Example 1:

referring to fig. 1-2, a large-size sapphire plate die-guide growth device comprises a furnace body 9, wherein the furnace body 9 is a cuboid, two sides of the furnace body 9 are of a door structure which is oppositely opened, a plate-shaped graphite resistance heater 1 and a graphite hard felt 2 are adopted as heat insulation materials, and an integral thermal field is of a dual-temperature-zone structure;

in the utility model, four plate-shaped graphite heaters 1 are arranged around a circular crucible 4, the crucible 4 is fixedly connected with the inner bottom of a furnace body 9 through a crucible supporting rod 8, and the crucible 4 is made of molybdenum, tungsten, iridium or rhenium and is a main heating zone;

in the utility model, the main heating area and the back heating area can be independently controlled respectively, the back heaters are arranged on the two parallel sides of the large surface of the sapphire plate 5, the large surface of the sapphire plate 5 is the surface A, the lifting direction is the direction M or the direction C, and the length of the sapphire plate is 400 plus 1000 mm;

in the utility model, the main heating area and the post-heating area are separated by the graphite hard felt 2 as a heat shield, the heat shield is horizontally arranged on the upper part of the crucible cover 3 and positioned at two sides of the mould 6, and the mould 6 is a splicing structure of two plane plates;

the utility model discloses in, mould 6 width 250-.

The utility model discloses in, a jumbo size sapphire panel die-guide method growth method, including following step:

step 1: firstly, charging raw materials, and then vacuumizing the furnace body 9;

step 2: then, the furnace body 9 is inflated, and then the temperature of the furnace body 9 is raised to melt the sapphire;

and 3, step 3: seeding and shouldering to an equal diameter stage and continuing until the crystal growth is finished;

and 4, step 4: then, the furnace body 9 is annealed in situ, the crucible 4 is lowered, the temperature is reduced to the room temperature, and then the crystal is taken out.

The utility model discloses in, the design of dual-temperature area is avoided crystal stress too big production dislocation, defects such as fracture, avoids the high temperature because the fluctuation of fuse-element temperature leads to the crystal to produce the bubble, ensures the high quality of crystal.

The utility model discloses in, any liquid and its upper portion direct contact's gas finally all can reach gaseous phase equilibrium state, and the aluminium oxide fuse-element can reach dynamic balance rather than the gaseous phase on upper portion after the definite time, if there is the disturbance between double-phase, like temperature fluctuation or mechanical shock, the bubble that the fuse-element produced probably rises to the growth interface through mould capillary seam and gets into inside the crystal

The utility model discloses in, figure 1 is a general boiling point diagram, and component 1 boils under higher temperature, can be the sapphire fuse-element, and component 2 boils under lower temperature, can be any gaseous phase composition (argon gas, CO or CO2) of dissolving in the sapphire fuse-element. As shown in fig. 1, the solubility of component 2 in component 1 decreases with increasing temperature.

The utility model discloses in, be in the balanced fuse-element of gaseous phase under specific temperature, the gas that has dissolved can the supersaturation under higher temperature. Therefore, the increase in temperature promotes the formation of bubbles in the melt. In order to inhibit the formation of bubbles in a melt, the temperature of a rear heater is only regulated in the crystal growth process, the temperature of the melt in a crucible is kept constant, and the generation of bubbles in the crystal due to the fact that the bubbles in the melt enter the crystal is avoided from the source.

The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims (8)

1. The utility model provides a jumbo size sapphire board die-guiding method growth device, includes furnace body (9), its characterized in that, furnace body (9) both sides are the structure of opening a door mutually, adopt platelike graphite heater (1), and hard felt of graphite (2) are as insulation material, and whole thermal field is two warm area structures, and circular crucible (4) have four platelike graphite heater (1) all around, for the main zone of heating, are equipped with the after-heating in sapphire board (5) big parallel both sides of face, and main heating and after-heating warm area are separated both as the heat screen by hard felt of graphite (2), and the heat screen level is placed in crucible cover (3) upper portion and is located mould (6) both sides.

2. The large-size sapphire plate die-guided growth device of claim 1, wherein the main heating zone and the post heating zone are independently controllable.

3. The large-size sapphire plate die-guided growth device according to claim 1, wherein the die (6) is a two-plate split structure, the width of the die (6) is 250-450mm, the thickness is 8-30mm, the height is 40-150mm, the width of the middle capillary seam is 0.2-2mm, and the top of the die (6) has an included angle of 90-180 degrees.

4. The large-size sapphire plate die-guided growth device according to claim 1, wherein the large surface of the sapphire plate (5) is an A surface, the pulling direction is M direction or C direction, and the length of the sapphire plate is 400-1000 mm.

5. The large-size sapphire plate die-casting growth device according to claim 1, wherein the crucible (4) is made of molybdenum, tungsten, iridium or rhenium.

6. The large-size sapphire plate die-guided growth device according to claim 1, wherein the die (6) is made of molybdenum, tungsten, iridium or rhenium.

7. The large-size sapphire plate die-guide growth device according to claim 1, wherein the furnace body (9) is a cuboid.

8. The large-size sapphire plate die-guide growth device according to claim 1, wherein the crucible (4) is fixedly connected with the inner bottom of the furnace body (9) through a crucible supporting rod (8).

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