CN103710752A - Die for growing large-diameter tubular sapphire with edge-defined film-fed growth process - Google Patents
Die for growing large-diameter tubular sapphire with edge-defined film-fed growth process Download PDFInfo
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- CN103710752A CN103710752A CN201410006948.8A CN201410006948A CN103710752A CN 103710752 A CN103710752 A CN 103710752A CN 201410006948 A CN201410006948 A CN 201410006948A CN 103710752 A CN103710752 A CN 103710752A
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Abstract
The invention discloses a die for growing a large-diameter tubular sapphire with an edge-defined film-fed growth process, belonging to crystal growth devices. The die is characterized by comprising a platy positioning seat with a through hole, an outer molybdenum tube embedded in the through hole of the positioning seat and an inner molybdenum tube in cup joint in the outer molybdenum tube, wherein a gap-shaped growth seam is formed between the inner and outer molybdenum tubes; at least three molybdenum blocks for controlling the width of the growth seam are clamped in central symmetry in the growth seam; the lower ends of the inner and outer molybdenum tubes pass through the through hole of the positioning seat to form convex feet; feed slots are formed in the convex feet; and the upper openings with wedge-point vertical sections are positioned in the same inclined plane. In the process of growing the large-diameter tubular sapphire with outer diameter over 30mm and thickness over 3mm with an edge-defined film-fed growth process, the phenomenon of crystal embedding is avoided, the problems of difficulty in closing and waste products with cracks occurring in the growth of large-diameter tubular sapphire with outer diameter over 30mm are successfully solved, the qualified rate of finished products is improved to over 95% from about 60% of the prior art, and thus the production cost is remarkably reduced.
Description
Technical field
The present invention relates to crystal growing apparatus, particularly a kind of for the sapphire mould of guided mode method growth large diameter tubular.
Background technology
Sapphire has high rigidity, high temperature resistant, corrosion-resistant, see through the dielectric properties that spectral range is wide, transmitance is high, good.Sapphire is widely used in a series of high-tech sectors such as national defence, military affairs, scientific research with its good performance, also has application very widely simultaneously in civilian industry.Because sapphire growth temperature is up to 2050 ℃, cause that large, the warm field variable of monocrystal growing furnace power is many, non-cutting time is long, causes production cost too high.It is fast that guided mode rule has crystalline growth velocity, and size can accurately be controlled, and save material, time and the energy, thereby increase economic efficiency, be one of the most promising sapphire growth method.
Prior art document 1 is in the < < method for growing high-performance tube type sapphire > > of publication number CN1884634A, " technical scheme of employing is: a kind of blue precious right method of growing high-performance tube, adopt one-time formed wetting edge-defined technology, directly from melt, draw required in, the tubulose sapphire of outside dimension and length, it is characterized in that, first determine the sapphire specification of tubulose, according to above-mentioned specification, make the mould matching, then, select high purity flame melt method sapphire particle as raw material, select the high-quality seed crystal of the <0001> direction of Czochralski grown, use long tube mould, carry out the sapphire growth of tubulose, the warm field condition of crystal growth is wanted rationally, laterally temperature is wanted evenly, transverse temperature difference is in 2 ℃, longitudinal temperature gradient is being 3-4 ℃ in die face 10mm, growth velocity is 30-40mm/h.The tubulose sapphire of above-mentioned specification comprises external diameter 4mm-30mm, wall thickness 1.5mm-3mm, and maximum length is 250mm.Above-mentioned mould is selected high-quality forging and stamping molybdenum materials, and Design and Machining becomes with required crystal face shaping and size and matches, with the high precision long tube mould of the circular tube shaped of capillary seam.”
In the disclosed < < of prior art document 1 method for growing high-performance tube type sapphire > > when relating to the mould of employing, only point out that " Design and Machining becomes with required crystal face shaping and size and matches, with the high precision long tube mould of the circular tube shaped of capillary seam." lack the further restriction to die needed shape and structure; In the disclosed < < of prior art document 1 method for growing high-performance tube type sapphire > >, point out that " the tubulose sapphire of above-mentioned specification comprises external diameter 4mm-30mm; wall thickness 1.5mm-3mm, and maximum length is 250mm relating to when tubulose sapphire comprises external diameter and wall thickness." can only produce 30 millimeters of external diameters and following, 3 millimeters of wall thickness and following tubulose sapphire, cannot produce 30 millimeters of above, 3 millimeters of above large size tubulose sapphires of wall thickness of external diameter.
And the circular tube shaped die of prior art is when producing tubulose sapphire by guided mode method, tubular die is suitable for reading to be grown in pipe process, from capillary, stitch, be while growing in gap-like growth seam, due to the existence of warm field gradient, inevitable causing on mould circumference successively, there is the brilliant embedding phenomenon of polycrystalline in the tubulose sapphire that causes the growing up to position of in the end closing up, particularly, when growth is more than 30 millimeters during large diameter tubular sapphire, be even difficult to successfully close up, occur being mingled with the waste product in crack.This has just caused the circular tube shaped die of prior art when producing tubulose sapphire by guided mode method, and product qualified rate is low, and growth cost is high.
As can be seen here, study and design a kind of rational in infrastructure, product qualified rate is high, thereby, wall thickness 3 millimeter above large diameter tubular sapphire moulds above for 30 millimeters of guided mode method growth external diameters of significantly having reduced production cost are necessary.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, study and design a kind of rational in infrastructure, product qualified rate is high, thus significantly reduced production cost for 30 millimeters of above, 3 millimeters of above sapphire moulds of large diameter tubular of wall thickness of guided mode method growth external diameter.
The present invention seeks to be achieved through the following technical solutions:
A kind of for the sapphire mould of guided mode method growth large diameter tubular, it is characterized in that comprising the tabular positioning seat with through hole, be embedded in the outer molybdenum pipe in positioning seat through hole, the interior molybdenum pipe being socketed in outer molybdenum pipe combines, in described, between outer molybdenum pipe, there is gap-like growth seam, in described growth seam, be connected with in a center of symmetryly and control at least 3 molybdenum pieces that growth seam width is used, in described, the lower end of outer molybdenum pipe becomes protruding pin through positioning seat through hole, on described protruding pin, offer feed chute, in described, the vertical section suitable for reading of outer molybdenum pipe is wedge tip, described vertical section be wedge tip in, the suitable for reading of outer molybdenum pipe is positioned on same tilting plane.
The described inside and outside molybdenum pipe tilt angle alpha suitable for reading being positioned on same tilting plane is selected at 3-8 ° according to the sapphire pipe diameter size of the large diameter tubular of required growth.The technique effect of above-mentioned design is: grow in pipe process tubular die is suitable for reading, from capillary, stitch, be while growing in gap-like growth seam, existence due to warm field gradient, mouth of pipe eminence temperature is relatively low, mouth of pipe lower temperature is relatively high, and the suitable for reading of inside and outside molybdenum pipe that described vertical section is wedge tip is positioned on same tilting plane; And be positioned at inside and outside molybdenum pipe on same tilting plane tilt angle alpha suitable for reading 3-8 ° selected after, the relatively low mouth of pipe eminence of temperature is just in time carried out low temperature seeding, the mouth of pipe lower that temperature is relatively high just in time carries out high temperature closing in, avoided the tubulose sapphire position of in the end closing up to occur the brilliant embedding phenomenon of polycrystalline, successfully solved when growth is more than 30 millimeters during large diameter tubular sapphire, occurred the waste product problem that is difficult to closing in, is mingled with crack.
The distance that described vertical section is between the top suitable for reading of inside and outside molybdenum pipe of wedge tip equals the sapphire thickness of pipe of large diameter tubular.The technique effect of above-mentioned design is: the design of the wedge tip of the both sides of discharge port, guaranteed that the temperature field between wedge tip is even, and make the tubulose sapphire growing there will not be growth line.
The invention process obtain for the sapphire mould of guided mode method growth large diameter tubular, through on probation, compared with prior art shown following beneficial effect:
1, rational in infrastructure,, wall thickness 3 millimeter above large diameter tubular sapphire processes above for 30 millimeters of guided mode method growth external diameters there will not be brilliant embedding phenomenon, successfully solved when growth is more than 30 millimeters during large diameter tubular sapphire, even occurred the waste product problem that is difficult to closing in, is mingled with crack.Suitable for reading concordant different from the circular tube shaped die of prior art, in technical solution of the present invention, inside and outside molybdenum pipe tilt angle alpha suitable for reading is at 3-8 °, form the relatively low mouth of pipe eminence of temperature and just in time carried out low temperature seeding, the mouth of pipe lower that temperature is relatively high just in time carries out high temperature closing in, avoided the tubulose sapphire position of in the end closing up to occur the brilliant embedding phenomenon of polycrystalline, successfully solved when growth is more than 30 millimeters during large diameter tubular sapphire, even occurred the waste product problem that is difficult to closing in, is mingled with crack.
2, product qualified rate is high during, 3 millimeters of above large diameter tubular sapphires of wall thickness above for 30 millimeters of guided mode method growth external diameters, thereby has significantly reduced production cost.As previously mentioned, in technical solution of the present invention, inside and outside molybdenum pipe tilt angle alpha suitable for reading is at 3-8 °, received mouth of pipe eminence low temperature seeding, the good result that the capable high temperature of mouth of pipe lower closes up, avoided the tubulose sapphire position of in the end closing up to occur the brilliant embedding phenomenon of polycrystalline, particularly solved when growth external diameter more than 30 millimeters, wall thickness are more than 3 millimeters during large diameter tubular sapphire, be difficult to close up, appearance is mingled with the problem of the waste product in crack, product qualified rate is brought up to more than 95% from approximately 60% of prior art, thereby has significantly reduced production cost.
Accompanying drawing explanation
Fig. 1 is the structural representation that meets theme of the present invention; Fig. 2 is the structural representation that in Fig. 1, the present invention shows along A-A section.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect and understand and understand, below in conjunction with concrete diagram, further illustrate the present invention:
As Fig. 1, shown in 2, a kind of for the sapphire mould of guided mode method growth large diameter tubular, it is characterized in that comprising tabular positioning seat 1, be embedded in the outer molybdenum pipe 2 in positioning seat through hole, the interior molybdenum pipe 3 being socketed in outer molybdenum pipe combines, in described, between outer molybdenum pipe, there is gap-like growth seam 4, in described growth seam, be connected with in a center of symmetryly and control at least 3 molybdenum pieces 5 that growth seam width is used, in described, the lower end of outer molybdenum pipe becomes protruding pin 6 through positioning seat through hole, on described protruding pin, offer feed chute 61, in described, suitable for reading 21 of outer molybdenum pipe, 31 vertical sections are wedge tip, described vertical section be wedge tip in, the suitable for reading of outer molybdenum pipe is positioned on same tilting plane 7.
As shown in Figure 2, inside and outside molybdenum pipe 21,31 the tilt angle alpha suitable for reading being positioned at described on same tilting plane 7 is selected at 3-8 ° according to the sapphire pipe diameter size of the large diameter tubular of required growth.
As shown in Figure 2, the distance that described vertical section is between 21,31 the top suitable for reading of inside and outside molybdenum pipe of wedge tip equals the sapphire thickness of pipe of large diameter tubular.
Embodiment 1 produces the tubulose sapphire mould of 31 millimeters of external diameters, 4.4 millimeters of thickness
As shown in Figure 1, 2, rubbing board shape positioning seat 1 is for offering 34 millimeters of through holes, the rectangle molybdenum plate of thick 15 millimeters, be embedded in the outer molybdenum pipe 2 of 34 millimeters of external diameters in positioning seat through hole, 4 millimeters of wall thickness, be socketed on the interior molybdenum pipe 3 of 25.2 millimeters of external diameters in outer molybdenum pipe, 4 millimeters of wall thickness, the growth of wide 0.4 millimeter seam 4 between inside and outside molybdenum pipe, in growth seam, become each other 120 ° of inscribed angle to be connected with the molybdenum piece 5 of 0.4 millimeter of 3 thickness, it is on the same tilting plane 7 of 3 ° that inside and outside molybdenum pipe suitable for reading is all positioned at tilt angle alpha.
As shown in Figure 1, 2, rubbing board shape positioning seat 1 is for offering 37 millimeters of through holes, the rectangle molybdenum plate of thick 15 millimeters, be embedded in the outer molybdenum pipe 2 of 37 millimeters of external diameters in positioning seat through hole, 4 millimeters of wall thickness, be socketed on the interior molybdenum pipe 3 of 32 millimeters of external diameters in outer molybdenum pipe, 4 millimeters of wall thickness, the growth of wide 0.5 millimeter seam 4 between inside and outside molybdenum pipe, in growth seam, become each other 120 ° of inscribed angle to be connected with the molybdenum piece 5 of 0.5 millimeter of 3 thickness, it is on the same tilting plane 7 of 6 ° that inside and outside molybdenum pipe suitable for reading is positioned at tilt angle alpha.
As shown in Figure 1, 2, rubbing board shape positioning seat 1 is for offering 39 millimeters of through holes, the rectangle molybdenum plate of thick 15 millimeters, be embedded in the outer molybdenum pipe 2 of 39 millimeters of external diameters in positioning seat through hole, 4 millimeters of wall thickness, be socketed on the interior molybdenum pipe 3 of 34 millimeters of external diameters in outer molybdenum pipe, 4 millimeters of wall thickness, the growth of wide 0.5 millimeter seam 4 between inside and outside molybdenum pipe, in growth seam, become each other 120 ° of inscribed angle to be connected with the molybdenum piece 5 of 0.5 millimeter of 3 thickness, it is on the same tilting plane 7 of 8 ° that inside and outside molybdenum pipe suitable for reading is positioned at tilt angle alpha.
Claims (4)
1. one kind for the sapphire mould of guided mode method growth large diameter tubular, it is characterized in that comprising tabular positioning seat (1), be embedded in the outer molybdenum pipe (2) in positioning seat through hole, be socketed on the interior molybdenum pipe (3) in outer molybdenum pipe, in described, between outer molybdenum pipe, there is gap-like growth seam (4), in described growth seam, be connected with in a center of symmetryly and control at least 3 molybdenum pieces (5) that growth seam width is used, in described, the lower end of outer molybdenum pipe becomes protruding pin (6) through positioning seat through hole, on described protruding pin, offer feed chute (61), in described, (21) suitable for reading of outer molybdenum pipe, (31) vertical section is wedge tip, described vertical section be wedge tip in, the suitable for reading of outer molybdenum pipe is positioned on same tilting plane (7).
2. according to claim 1 for the guided mode method many sapphire moulds of tubulose of growing simultaneously, it is characterized in that described growth seam (4) lower end opening for feed is communicated in feed chute (61).
3. according to claim 1 for the sapphire mould of guided mode method growth large diameter tubular, the tilt angle alpha that is positioned at inside and outside molybdenum pipe (21) suitable for reading on same tilting plane (7), (31) described in it is characterized in that is selected at 3-8 ° according to the sapphire pipe diameter size of the large diameter tubular of required growth.
4. according to claim 1 for the sapphire mould of guided mode method growth large diameter tubular, it is characterized in that described vertical section is (21) suitable for reading of the inside and outside molybdenum pipe of wedge tip, the distance between the top of (31) equals the sapphire thickness of pipe of large diameter tubular.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110468451A (en) * | 2019-09-11 | 2019-11-19 | 同济大学 | A kind of mold and method for EFG technique growth end seal sapphire pipe |
EP3805436A4 (en) * | 2018-05-31 | 2022-03-02 | Kyocera Corporation | Device and method for producing tubular single crystals |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN85103282A (en) * | 1985-04-29 | 1986-10-29 | 天津市硅酸盐研究所 | The method of growing bar shaped ruby and device thereof |
CN1884634A (en) * | 2006-05-22 | 2006-12-27 | 天津市硅酸盐研究所 | Method for growing high-performance tube type sapphire |
US20110056430A1 (en) * | 2009-09-08 | 2011-03-10 | Keigo Hoshikawa | Equipment for growing sapphire single crystal |
-
2014
- 2014-01-07 CN CN201410006948.8A patent/CN103710752A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN85103282A (en) * | 1985-04-29 | 1986-10-29 | 天津市硅酸盐研究所 | The method of growing bar shaped ruby and device thereof |
CN1884634A (en) * | 2006-05-22 | 2006-12-27 | 天津市硅酸盐研究所 | Method for growing high-performance tube type sapphire |
US20110056430A1 (en) * | 2009-09-08 | 2011-03-10 | Keigo Hoshikawa | Equipment for growing sapphire single crystal |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3805436A4 (en) * | 2018-05-31 | 2022-03-02 | Kyocera Corporation | Device and method for producing tubular single crystals |
CN110468451A (en) * | 2019-09-11 | 2019-11-19 | 同济大学 | A kind of mold and method for EFG technique growth end seal sapphire pipe |
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Application publication date: 20140409 |