CN103556223A - Method for growing large-size square sapphire single crystal - Google Patents
Method for growing large-size square sapphire single crystal Download PDFInfo
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- CN103556223A CN103556223A CN201310579024.2A CN201310579024A CN103556223A CN 103556223 A CN103556223 A CN 103556223A CN 201310579024 A CN201310579024 A CN 201310579024A CN 103556223 A CN103556223 A CN 103556223A
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Abstract
The invention discloses a method for growing a large-size square sapphire single crystal, relating to single crystal materials of aluminum oxides. According to the method, a special crucible is used and a process for upper seeding and directional crystallization is adopted to grow a rectangular or square sapphire crystal with specific crystal orientation, wherein the special crucible has a round outside and a square inside namely the outer surface is cylindrical and the inner space is in the shape of a trapezoidal cone, and the caliber of an upper port of the inner space trapezoidal cone is bigger than that of a bottom port of the inner space trapezoidal cone of the special crucible. The method disclosed by the invention overcomes the defects that the conventional growth method can not ensure the uniformity and stability of a growth interface to result in low crystal quality, and due to anisotropy of the growth rate, the crystal is broken by great thermal stress caused during growing and is low in integrity.
Description
Technical field
Technical scheme of the present invention relates to the monocrystal material of the oxide compound of aluminium, specifically a kind of method of growing large-size and square sapphire single-crystal.
Background technology
Sapphire single-crystal has good optics, mechanics, calorifics, dielectric, radioprotective and corrosion resistant performance, be a kind of crystal of high comprehensive performance, be widely used in semiconductor material with wide forbidden band as the substrate of gan, aerospace, military infrared optical window and femto-second laser substrate material field.Along with the fast development in semiconductor lighting market, sapphire single-crystal material has been proposed to large size, high quality and requirements at the higher level cheaply.In recent years, Apple starts extensively to adopt sapphire material in smart mobile phone field, comprises mobile phone camera minute surface, sapphire HOME key minute surface and sapphire hand-set lid, has further widened sapphire Application Areas, and the market space is further opened.
Traditional sapphire production method, as the complex process of guided mode method (EFG), kyropoulos (KY) and crystal pulling method (CZ), length consuming time, production cost is high.Because the sapphire single-crystal crystal of growing is round, need to require drill through from the side plug according to special crystal orientation, the utilization ratio of crystal is less than 30%, and utilization ratio is lower, causes cost very high.The crucible of traditional sapphire production method application is cylindrical crucible, and being conducive to growth, to have specific symmetry axis be crystal.Because traditional sapphire single-crystal generally adopts A axial growth, and A is to non-sapphire symmetry axis, so conventional growth method can not guarantee homogeneity and the stability of growth interface, causes crystal mass not high.Due to the anisotropy of its growth velocity, easily appearance is compared with large thermal stresses and cracked for crystal growing process simultaneously, and perfection of crystal is poor.
In prior art, CN201310113549 discloses a kind of growth method of large size c orientation sapphire single-crystal, CN201310112926 has disclosed a kind of new method for producing of c orientation sapphire single-crystal, above-mentioned two kinds of methods crystal in process of growth contacts with crucible all the time, the thermal expansivity of crystal and crucible is inconsistent, can make crystal stress concentration even ftracture; CN201310026250 has reported that large size C is to sapphire crystal manufacture method, and aforesaid method complex process can not solve C and easily produce the technical barrier of low angle boundary to crystal growth.The crystal weight that prior art is produced is all at 70～80Kg, and complex manufacturing, during consumption energy consumption, can not produce large size and the high perfect sapphire crystal of utilization ratio over 100Kg.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method that growing large-size and square sapphire single-crystal are provided, use is the special copple that round outside but spuare inside shape and top bore are greater than bottom bore, adopt the technique of top seeding crystallographic orientation, growth has the rectangular parallelepiped of particular crystal plane orientation or the sapphire crystal of square shape, homogeneity and stability that conventional growth method can not guarantee growth interface have been overcome, cause crystal mass not high, while is due to the anisotropy of its growth velocity, crystal growing process easily occurs compared with large thermal stresses and the cracked and poor many defects of perfection of crystal.
The present invention solves this technical problem adopted technical scheme: a kind of method of growing large-size and square sapphire single-crystal, and step is:
A. growing large-size and square sapphire single-crystal crystal growing furnace used
The formation of the crystal growing furnace that growing large-size and square sapphire single-crystal are used comprises top water-cooled copper dish, miramint seed rod, top heat protection screen, sidewall of the furnace body water-cooled copper, square seed crystal, steel body of heater, middle part tungsten net well heater, middle part molybdenum sheet heat protection screen, special copple, bottom tungsten net well heater, bottom molybdenum sheet heat protection screen, tungsten support bar, bottom water-cooled copper dish, special copple lid and top tungsten net well heater, top water-cooled copper dish is positioned at the top of top heat protection screen, miramint seed rod is through the circular hole of top heat protection screen and special copple lid, miramint seed rod bottom is positioned at the top of special copple, contact top, miramint seed rod top water-cooled copper dish, top tungsten net well heater and middle part tungsten net well heater are between the sidewall and middle part molybdenum sheet heat protection screen of special copple, bottom tungsten net well heater is between the bottom and bottom molybdenum sheet heat protection screen of special copple, special copple is placed on tungsten support bar, tungsten support bar bottom contacts with bottom water-cooled copper dish, it is inner that sidewall of the furnace body water-cooled copper is positioned at steel body of heater, wherein special copple is round outside but spuare inside shape, be that its outside surface is cylindrical, internal space is trapezoidal cone, the suitable for reading circle that is shaped as of this crucible appearance, it is square that the trapezoidal cone in internal space suitable for reading is shaped as, the bottom of this crucible appearance be shaped as circle, being shaped as of the end mouth of the trapezoidal cone in internal space is square, the bore suitable for reading of the trapezoidal cone in internal space is greater than the bore of the end mouth of the trapezoidal cone in internal space, internal surface four sides of this crucible internal space are isosceles trapezoid, the junction of the stepped inner surface adjacent side of internal space is the chamfering circular arc seamlessly transitting, the junction of the outside of this crucible bottom and crucible outer side is the chamfering circular arc seamlessly transitting, top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater are collectively referred to as well heater, the shape of well heater is corresponding with columned special copple outside surface.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 1.33 * 10
-4pa～1.06 * 10
-4pa, the special copple in the crystal growing furnace of heating described in A, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 200g～230g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2kg～2.5kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, speed with 0.2mm/h～0.5mm/h lifts miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 22000W～21000W, 52000W～51000W and 17000W～16000W, make the power of top and middle part well heater in 30 hours, drop to respectively 20380W～19380W, 48760W～47760W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater dropped to respectively 12580W～11580W in 20 hours, 27760W～26760W and 11000W～10000W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three steps and divide step annealing.
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, the cylindrical height of outer surface of described special copple is 180～520mm, the circular outside diameter that is shaped as that described outer surface is suitable for reading is 140～450mm.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, the length of side of the oblique waist of the trapezoidal cone of the internal space of described special copple is 165～490mm, the suitable for reading square length of side that is shaped as of the trapezoidal cone in internal space is 80～300mm, and the square length of side that is shaped as of the end mouth of the trapezoidal cone in internal space is 70～250mm.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, the shape of the end mouth of the trapezoidal cone of shape suitable for reading and internal space of the trapezoidal cone in internal space of described special copple is rectangle or simultaneously square simultaneously.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, the crucible bottom thickness of described special copple is 10～30mm.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, described special copple is molybdenum crucible or the tungsten crucible that powder metallurgical technique is made.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, the internal surface of described special copple has carried out polished finish.
The method of above-mentioned a kind of growing large-size and square sapphire single-crystal, related starting material all obtain by known approach, and related equipment and operating procedure are that those skilled in the art know and grasp.
The invention has the beneficial effects as follows: compared with prior art, substantive distinguishing features and marked improvement that it is outstanding are in the present invention:
(1) by top seeding technique, guarantee crystal seed hereditary property, improve crystal mass;
(2) after seeding completes, wait sapphire single-crystal to grow to 2kg～2.5kg size and stop the rotation, make it according to each crystal orientation habit free growth of sapphire;
(3) special copple outer shape is circular, and the shape of top tungsten net well heater, middle part tungsten net well heater and three well heaters of bottom tungsten net well heater is also circular, guarantees the relatively stable and homogeneity of the temperature field of Sapphire Crystal Growth chamber;
(4) special copple interior shape is rectangular trapezoidal cone or square trapezoidal cone, by the positive action of crucible, the differentiation of restriction crystal shape, adopt the technique of top seeding crystallographic orientation, guarantee the consistence of sapphire crystal face and crucible inner face, growth has the rectangular parallelepiped of particular crystal plane orientation or the sapphire crystal of square shape, more than significantly improving the utilization ratio to 60% of crystal.Utilize sapphire single-crystal anisotropy is A face, M face and the different characteristic of each face growth velocity of C face simultaneously, the thermal stresses of balance sapphire single-crystal because causing with crucible thermal mismatching, reduce the microdefects such as dislocation, and prevent from the germinating of crackle in sapphire single-crystal from improving crystal mass and yield rate.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the main pseudosection of growing large-size and square sapphire single-crystal crystal growing furnace used.
Fig. 2 is the side cut away view of special copple.
Fig. 3 is the suitable for reading top that is shaped as rectangular special copple of the trapezoidal cone in internal space.
Fig. 4 is the suitable for reading top that is shaped as foursquare special copple of the trapezoidal cone in internal space.
In figure, 1. top water-cooled copper dish, 2. miramint seed rod, 3. top heat protection screen, 4. sidewall of the furnace body water-cooled copper, 5. square seed crystal, 6. steel body of heater, 7. middle part tungsten net well heater, 8. middle part molybdenum sheet heat protection screen, 9. special copple, 10. bottom tungsten net well heater, 11. bottom molybdenum sheet heat protection screens, 12. tungsten support bars, 13. bottom water-cooled copper dishes, 14. special copple lids, 15. top tungsten net well heaters, 16. outer surfaces are suitable for reading, 17. seamlessly transit chamfering circular arc a, 18. rectangle limits, 19. square limits, the outer surface of 20. crucibles, 21. crucible bottom, 22. seamlessly transit chamfering circular arc b, the end mouth of the 23. trapezoidal cones in internal space, the internal surface of 24. internal spaces, the 25. trapezoidal cones in internal space suitable for reading.
Embodiment
Embodiment illustrated in fig. 1 showing, the formation of the crystal growing furnace that growing large-size of the present invention and square sapphire single-crystal are used comprises top water-cooled copper dish 1, miramint seed rod 2, top heat protection screen 3, sidewall of the furnace body water-cooled copper 4, square seed crystal 5, steel body of heater 6, middle part tungsten net well heater 7, middle part molybdenum sheet heat protection screen 8, special copple 9, bottom tungsten net well heater 10, bottom molybdenum sheet heat protection screen 11, tungsten support bar 12, bottom water-cooled copper dish 13, special copple lid 14, top tungsten net well heater 15, wherein, top water-cooled copper dish 1 is positioned at the top of top heat protection screen 3, miramint seed rod 2 is through the circular hole of top heat protection screen 3 and special copple lid 14, miramint seed rod 2 bottoms are positioned at the top of special copple 9, be used for fixing seed crystal 5, miramint seed rod 2 contact top, top water-cooled copper dishes 1 are to be cooled, top tungsten net well heater 15 and middle part tungsten net well heater 7 are between the sidewall and middle part molybdenum sheet heat protection screen 8 of special copple 9, bottom tungsten net well heater 10 is between the bottom and bottom molybdenum sheet heat protection screen 11 of special copple 9, special copple 9 is placed on tungsten support bar 12, tungsten support bar 12 bottoms contact with bottom water-cooled copper dish 13 for strengthening heat radiation, sidewall of the furnace body water-cooled copper 3 is positioned at steel body of heater 6 inside, is used for strengthening the sidewall heat radiation of steel body of heater 6, wherein special copple 9 is round outside but spuare inside shape, the outer surface 20 of this crucible is cylindrical, crucible bottom 21 outside surfaces be shaped as circle, internal space is trapezoidal cone, outer surface suitable for reading 16 be shaped as circle, the trapezoidal cone in internal space suitable for reading 25 be shaped as square, being shaped as of the end mouth 23 of the trapezoidal cone in internal space is square, suitable for reading 25 bore of the trapezoidal cone in internal space is greater than the bore of the end mouth 23 of the trapezoidal cone in internal space, internal surface 24 4 sides of internal space are isosceles trapezoid, the junction of each isosceles trapezoid internal surface adjacent side of the internal surface 24 of internal space is the chamfering circular arc a17 seamlessly transitting, junction between the outer surface of crucible and crucible bottom outside surface is for seamlessly transitting chamfering circular arc b22, top tungsten net well heater 15, middle part tungsten net well heater 7 and bottom tungsten net well heater 10 are collectively referred to as well heater, the shape of well heater is corresponding with columned special copple 9 outside surfaces.
Embodiment illustrated in fig. 2 showing, junction between the outer surface 20 of the cylindrical crucible of special copple 9 of the present invention and crucible bottom 21 outside surfaces is for seamlessly transitting chamfering circular arc b22, the internal space being formed by the internal surface 24 of internal space is trapezoidal cone, and suitable for reading 25 bore of the trapezoidal cone in internal space indicating with dotted line in figure is greater than the bore of the end mouth 23 of the trapezoidal cone in internal space.
Embodiment illustrated in fig. 3 showing, suitable for reading 25 of the trapezoidal cone in internal space of special copple 9 of the present invention is rectangle, outer surface suitable for reading 16 be shaped as circle, the junction of each isosceles trapezoid internal surface adjacent side of internal space is for seamlessly transitting chamfering circular arc a17, the suitable for reading rectangle limit 18 that is shaped as of the trapezoidal cone in internal space.
Embodiment illustrated in fig. 4 showing, suitable for reading 25 of the trapezoidal cone in internal space of special copple 9 of the present invention is square, outer surface suitable for reading 16 be shaped as circle, the junction of each isosceles trapezoid internal surface adjacent side of internal space is for seamlessly transitting chamfering circular arc a17, and the trapezoidal cone in internal space suitable for reading is shaped as square limit 19.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 180mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 140mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 165mm, suitable for reading 25 the rectangular long length of side that is shaped as of the trapezoidal cone in internal space is that 90mm and the broadside length of side are 80mm, the rectangular long length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is that 80mm and the broadside length of side are 70mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is rectangle simultaneously, crucible bottom 21 thickness are 10mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 200g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.2mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 22000W, 52000W and 17000W, make the power of top and middle part well heater in 30 hours, drop to respectively 20380W, 48760W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater dropped to respectively 12580W in 20 hours, 27760W and 11000W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 350mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 290mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 300mm, suitable for reading 25 the rectangular long length of side that is shaped as of the trapezoidal cone in internal space is that 210mm and the broadside length of side are 190mm, the rectangular long length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is that 180mm and the broadside length of side are 160mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is rectangle simultaneously, crucible bottom 21 thickness are 15mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 215g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2.2kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.35mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 21800W, 51800W and 16800W, make the power of top and middle part well heater in 30 hours, drop to respectively 20180W, 48560W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater was dropping to respectively 12380W in 20 hours, 27560W and 10800W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 520mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 450mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 490mm, suitable for reading 25 the rectangular long length of side that is shaped as of the trapezoidal cone in internal space is that 300mm and the broadside length of side are 280mm, the rectangular long length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is that 250mm and the broadside length of side are 220mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is rectangle simultaneously, crucible bottom 21 thickness are 30mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 230g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2.5kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.5mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 21600W, 51600W and 16600W, make the power of top and middle part well heater in 30 hours, drop to respectively 19980W, 48360W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater was dropping to respectively 12180W in 20 hours, 27360W and 10600W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 180mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 140mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 165mm, suitable for reading 25 the foursquare length of side that is shaped as of the trapezoidal cone in internal space is 80mm, the foursquare length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is 70mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is square simultaneously, crucible bottom 21 thickness are 10mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 200g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.5mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 21400W, 51400W and 16400W, make the power of top and middle part well heater in 30 hours, drop to respectively 19780W, 48160W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater dropped to respectively 11980W in 20 hours, 27160W and 10400W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 350mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 300mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 330mm, suitable for reading 25 the foursquare length of side that is shaped as of the trapezoidal cone in internal space is 190mm, the foursquare length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is 160mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is square simultaneously, crucible bottom 21 thickness are 15mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 1.2 * 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 215g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2.2kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.3mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 21200W, 51200W and 16200W, make the power of top and middle part well heater in 30 hours, drop to respectively 19580W, 47960W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater was dropping to respectively 11780W in 20 hours, 26960W and 10200W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
A. growing large-size and square sapphire single-crystal crystal growing furnace used
Embodiment forms the present embodiment growing large-size used and square sapphire single-crystal crystal growing furnace used as shown in Figure 1, wherein the cylindrical height of outer surface 20 of the crucible of special copple 9 is 520mm, the circular outside diameter that is shaped as of described outer surface suitable for reading 16 is 450mm, the length of side of the oblique waist of the trapezoidal cone of internal space is 490mm, suitable for reading 25 the foursquare length of side that is shaped as of the trapezoidal cone in internal space is 300mm, the foursquare length of side that is shaped as of the end mouth 23 of the trapezoidal cone in internal space is 250mm, the shape of the end mouth 23 of suitable for reading 25 the trapezoidal cone of shape and internal space of the trapezoidal cone in internal space is square simultaneously, crucible bottom 21 thickness are 30mm, the tungsten crucible that special copple 9 is made for powder metallurgical technique, the internal surface of special copple 9 has carried out polished finish.
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 1.2 * 10
-4pa, arranges the special copple in the above-mentioned crystal growing furnace of heater power programmed heating, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 230g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2.5kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, with 0.5mm/h speed, lift miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 21000W, 51000W and 16000W, make the power of top and middle part well heater in 30 hours, drop to respectively 19380W, 47760W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater dropped to respectively 11580W in 20 hours, 26760W and 10000W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three-step annealing,
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
The related starting material of above-described embodiment all obtain by known approach, and related equipment and operating procedure are that those skilled in the art know and grasp.
Claims (7)
1. a method for growing large-size and square sapphire single-crystal, is characterized in that step is:
A. growing large-size and square sapphire single-crystal crystal growing furnace used
The formation of the crystal growing furnace that growing large-size and square sapphire single-crystal are used comprises top water-cooled copper dish, miramint seed rod, top heat protection screen, sidewall of the furnace body water-cooled copper, square seed crystal, steel body of heater, middle part tungsten net well heater, middle part molybdenum sheet heat protection screen, special copple, bottom tungsten net well heater, bottom molybdenum sheet heat protection screen, tungsten support bar, bottom water-cooled copper dish, special copple lid and top tungsten net well heater, top water-cooled copper dish is positioned at the top of top heat protection screen, miramint seed rod is through the circular hole of top heat protection screen and special copple lid, miramint seed rod bottom is positioned at the top of special copple, contact top, miramint seed rod top water-cooled copper dish, top tungsten net well heater and middle part tungsten net well heater are between the sidewall and middle part molybdenum sheet heat protection screen of special copple, bottom tungsten net well heater is between the bottom and bottom molybdenum sheet heat protection screen of special copple, special copple is placed on tungsten support bar, tungsten support bar bottom contacts with bottom water-cooled copper dish, it is inner that sidewall of the furnace body water-cooled copper is positioned at steel body of heater, wherein special copple is round outside but spuare inside shape, be that its outside surface is cylindrical, internal space is trapezoidal cone, the suitable for reading circle that is shaped as of this crucible appearance, it is square that the trapezoidal cone in internal space suitable for reading is shaped as, the bottom of this crucible appearance be shaped as circle, being shaped as of the end mouth of the trapezoidal cone in internal space is square, the bore suitable for reading of the trapezoidal cone in internal space is greater than the bore of the end mouth of the trapezoidal cone in internal space, internal surface four sides of this crucible internal space are isosceles trapezoid, the junction of the stepped inner surface adjacent side of internal space is the chamfering circular arc seamlessly transitting, the junction of the outside of this crucible bottom and crucible outer side is the chamfering circular arc seamlessly transitting, top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater are collectively referred to as well heater, the shape of well heater is corresponding with columned special copple outside surface,
B. operation steps
The first step, the arrangement of sapphire single-crystal seed crystal
By upper surface, be that to be wide of C face and side tie up on miramint seed rod with tungsten filament for the rectangular-shaped sapphire single-crystal seed crystal of M face for A face, side leptoprosopy;
Second step, the adding of raw material
The high purity aluminium oxide crystal block raw material that reaches 99.999% is joined in the special copple of growing large-size described in A and square sapphire single-crystal crystal growing furnace used, this special copple is put into the desired location of growing large-size described in A and square sapphire single-crystal crystal growing furnace used;
The 3rd step, the melting of raw material
Above-mentioned crystal growing furnace is evacuated to 1.33 * 10
-4pa～1.06 * 10
-4pa, the special copple in the crystal growing furnace of heating described in A, to add the high purity aluminium oxide crystal block raw material in special copple in melting second step;
The 4th step, seeding and the growth of brilliant neck
Said miramint seed rod in the decline the first step, makes the surface of liquation of bottom surface contact the 3rd step gained of sapphire single-crystal seed crystal, starts seeding, waits crystal to grow into 200g～230g and proceeds to next step;
The 5th step, shouldering and isodiametric growth
Reduce the power of top tungsten net well heater, middle part tungsten net well heater and bottom tungsten net well heater, solid-liquid interface is passed with steady speed, make isodiametric growth of crystal, while growing into 2kg～2.5kg in crystal, the rotation of miramint seed rod stops, by view port, observe crystal, guarantee the consistence of sapphire crystal face and crucible inner face;
The 6th step, ending and annealing
After treating that the crystal growth of the 5th step is complete, speed with 0.2mm/h～0.5mm/h lifts miramint seed rod, make crystal separated with crucible, then divide three-step annealing, its processing sequence is: top tungsten net well heater is first set, the power of middle part tungsten net well heater and bottom tungsten net well heater is respectively 22000W～21000W, 52000W～51000W and 17000W～16000W, make the power of top and middle part well heater in 30 hours, drop to respectively 20380W～19380W, 48760W～47760W, keep this heater power 5 hours, then make this top tungsten net well heater, the power of middle part tungsten net well heater and three well heaters of bottom tungsten net well heater dropped to respectively 12580W～11580W in 20 hours, 27760W～26760W and 11000W～10000W, keep this heater power 3 hours, be filled with argon gas simultaneously, then make these three heater powers in 30 hours, all be reduced to respectively 0W, complete three steps and divide step annealing.
The 7th step, gets crystalline substance
After the 6th step has operated, be filled with argon gas, while waiting air pressure in crystal growing furnace the same with normal atmosphere, crystalline substance is got in blow-on, makes large size and square sapphire single-crystal.
2. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: the cylindrical height of outer surface of described special copple is 180～520mm, the circular outside diameter that is shaped as that described outer surface is suitable for reading is 140～450mm.
3. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: the length of side of the oblique waist of the trapezoidal cone of the internal space of described special copple is 165～490mm, the suitable for reading square length of side that is shaped as of the trapezoidal cone in internal space is 80～300mm, and the square length of side that is shaped as of the end mouth of the trapezoidal cone in internal space is 70～250mm.
4. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: the shape of the end mouth of the trapezoidal cone of shape suitable for reading and internal space of the trapezoidal cone in internal space of described special copple is rectangle or simultaneously square simultaneously.
5. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: the crucible bottom thickness of described special copple is 10～30mm.
6. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: described special copple is molybdenum crucible or the tungsten crucible that powder metallurgical technique is made.
7. according to the method for the said a kind of growing large-size of claim 1 and square sapphire single-crystal, it is characterized in that: the internal surface of described special copple has carried out polished finish.
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| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN104611764A (en) * | 2015-01-21 | 2015-05-13 | 华中科技大学 | Micro-pulling-down crystal growing furnace |
| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN105401211A (en) * | 2014-08-08 | 2016-03-16 | 上海超硅半导体有限公司 | Crystal growing furnace and method for drawing C-axis sapphire single crystal |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN108277534A (en) * | 2018-04-27 | 2018-07-13 | 济南金曼顿自动化技术有限公司 | A kind of graphite resistance heating SiC crystal growth furnace |
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| JP2013006758A (en) * | 2011-05-20 | 2013-01-10 | Showa Denko Kk | Apparatus and method for producing single crystal and single crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105401211A (en) * | 2014-08-08 | 2016-03-16 | 上海超硅半导体有限公司 | Crystal growing furnace and method for drawing C-axis sapphire single crystal |
| CN105401211B (en) * | 2014-08-08 | 2017-12-26 | 上海超硅半导体有限公司 | Draw C axles sapphire single crystal growth furnace and method |
| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN104611764A (en) * | 2015-01-21 | 2015-05-13 | 华中科技大学 | Micro-pulling-down crystal growing furnace |
| CN104611764B (en) * | 2015-01-21 | 2017-10-31 | 华中科技大学 | A kind of micro- downward lifting crystal growing furnace |
| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN104711676B (en) * | 2015-03-16 | 2017-05-24 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN108277534A (en) * | 2018-04-27 | 2018-07-13 | 济南金曼顿自动化技术有限公司 | A kind of graphite resistance heating SiC crystal growth furnace |
| CN111379016A (en) * | 2018-12-28 | 2020-07-07 | 环球晶圆股份有限公司 | Silicon single crystal growth method and silicon single crystal growth equipment |
| US11377752B2 (en) | 2018-12-28 | 2022-07-05 | Globalwafers Co., Ltd. | Mono-crystalline silicon growth method |
| US11708642B2 (en) | 2018-12-28 | 2023-07-25 | Globalwafers Co., Ltd. | Mono-crystalline silicon growth apparatus |
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