CN102560630A - Thermal field capable of allowing synchronous growth of a plurality of crystals with edge-defined film-fed crystal growth technique and method thereof - Google Patents
Thermal field capable of allowing synchronous growth of a plurality of crystals with edge-defined film-fed crystal growth technique and method thereof Download PDFInfo
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- CN102560630A CN102560630A CN2012100089177A CN201210008917A CN102560630A CN 102560630 A CN102560630 A CN 102560630A CN 2012100089177 A CN2012100089177 A CN 2012100089177A CN 201210008917 A CN201210008917 A CN 201210008917A CN 102560630 A CN102560630 A CN 102560630A
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Abstract
The invention provides a thermal field capable of allowing synchronous growth of a plurality of crystals with an edge-defined film-fed crystal growth technique, which comprises a heating insulation device, a crucible and a seed chuck device, wherein the heating insulation device includes a heating element; the crucible has a first side wall and a second side wall which are parallel to each other; the heating element is a structure which enables the temperature to be equal at a position where the distance between the inside of the crucible and the first side wall is equal to that between the inside of the crucible and the second side wall, a side-by-side mould arranged in the crucible includes a plurality of mould pieces, the distance between each of the mould pieces and the first side wall is equal to that between each mould piece and the second side wall, and the upper surface of each of the mould pieces is of same section size and of same shape with the crystal to grow; seed crystals are arranged above the side-by-side mould, and the bottom of the seed crystals is provided with a face of weld which can simultaneously contact with the upper surface of each of the mould pieces. The thermal field is capable of allowing synchronous growth of a plurality of crystals with a same crystal orientation and a uniform radical temperature gradient.
Description
Technical field
The present invention relates to the thermal field of a kind of crystalline growth method and use thereof, relate in particular to the method and the employed thermal field of this method of many sapphire single-crystal bodies of a kind of guided mode method synchronous growth.
Background technology
Sapphire single-crystal body (α-Al
2O
3Monocrystalline) is a kind of simple corrdination type oxide crystal, belongs to hexagonal system, spacer D
63d
2R
3Mc; Have good mechanical, machinery, calorifics and electric property and stable physical and chemical performance; Be a kind of high temperature resistant, wear-resistant, erosion resistance and the wide high-quality optical function material of transmission region, be widely used in fields such as laser, infrared, semi-conductor, LED substrate, new energy technology, high-grade luxury goods.
Human to sapphire understanding early, growing technology is various.But its speed of growth is slow, and it is repeatable poor to produce, and causes price too expensive, greatly limitations sapphire application.Various sapphire growth methods cut both ways, and wherein, guided mode method (EFG) is to utilize the capillarity of metal through molybdenum mould guiding Al
2O
3Melt; The sapphire profile is limited the shape of molybdenum mould in crystallisation process, and obtains the product in the ideal, and this has simplified the crystalline processing link greatly; Reduced difficulty of processing; Having reduced the waste of blank simultaneously, can significantly improve economic benefit, is one of growth method of the tool potentiality of current artificial sapphire.
Yet, the EFG method growth during many wafers often because poor synchronization, and cause the crystal orientation of each bar wafer to differ, radial symmetry gradient is inhomogeneous, causes the wafer dislocation desity high even form crystal boundary, and has big stress, crystal mass is very undesirable.
Summary of the invention
Problems such as differ in existing many wafer poor synchronization, each wafer crystal orientation when solving many wafers of available technology adopting EFG method growth, radial symmetry gradient is inhomogeneous, the wafer dislocation desity high, internal stress is big the invention provides the thermal field and the method for many wafers of a kind of guided mode method synchronous growth.
Technical scheme provided by the present invention is: many crystalline thermal fields of a kind of guided mode method synchronous growth; The seed chuck device that it comprises heating and heat-insulating device at least, is arranged at the inner crucible of heating and heat-insulating device and is used to lift seed crystal, said heating and heat-insulating device comprises the heating element that is used for heating crucible that is arranged at the crucible periphery;
Said crucible has the first side wall and second sidewall that is parallel to each other;
Said heating element is the structure that the inside of said crucible is equated with its first side wall, the equidistant position of second sidewall temperature;
Be provided with the side-by-side mould in the said crucible; Said side-by-side mould comprise be fixed in the said crucible side by side, a plurality of die blade that structure is identical; Each die blade equates to the distance of the first side wall of said crucible, second sidewall, and the upper surface of each die blade all with crystalline sectional dimension, the shape that will grow identical;
The top of said side-by-side mould is provided with said seed crystal; Said seed crystal bottom has the face of weld that can contact simultaneously with the upper surface of each die blade, and the face of weld of said seed crystal contacts with the upper surface of each die blade and the size of the contact surface that forms, measure-alike.
Further; Said crucible is the square body structure; Said heating element is the square body structure with said crucible structure matching; The first side wall of said crucible, second sidewall equate with the inwall distance of said heating element, thereby make the inside of said crucible equate with its first side wall, the equidistant position of second sidewall temperature.
Further, said the crystal that will grow is sheet or arch sheet;
The upper surface of each die blade all have first edge parallel with the first side wall of said crucible and with second edge of second parallel sidewalls of said crucible, and first edge of distance and each die blade of first edge of each die blade to the distance of the first side wall of said crucible, second edge to second sidewall of said crucible all equates to the distance at second edge.
Further; Said seed crystal is the T shape sheet that both sides have jut; The flaky seed crystal of this T shape is parallel to the first side wall, the second sidewall setting of said crucible; And equate that to the distance of the first side wall of said crucible, second sidewall lower surface of said seed crystal forms the said face of weld that can contact simultaneously with the upper surface of each die blade;
Said seed chuck device comprises two molybdenum system covers that are connected with the jut of said seed crystal both sides respectively, and said molybdenum system tackling is useful on the snare structure of the jut that holds said seed crystal; The tuck of said seed crystal extend in the snare structure of said molybdenum system cover, puts thereby said seed crystal is hung over said molybdenum system.
Further, said heating and heat-insulating device also comprises the hard felt stay-warm case of graphite, and it is arranged at the top of said heating element and crucible, and around the periphery that is arranged on said seed crystal and seed chuck device; The surface of the hard felt stay-warm case of said graphite is brushed with oxidation-resistant coating; The hard felt stay-warm case of said graphite is provided with first view port and second view port of being convenient to observe crystal growth, and said first view port and said second view port are symmetricly set on the both sides of said seed crystal.
In the thermal field of the present invention; Crucible and heating element structure improve; Make in the inside of crucible, equate with the first side wall, the equidistant position of second sidewall temperature, and the side-by-side mould in the thermal field of the present invention is arranged in the crucible, each die blade all equates with the distance of the first side wall, second sidewall; Can guarantee that the crystalline radial temperature profile of growing on each die blade is even, front and back are symmetrical, internal stress is little; And adopt same seed crystal to contact simultaneously in the thermal field of the present invention with a plurality of die blade; Many crystal can lift synchronism and the consistence that in seeding, necking down, expansion shoulder and isodiametric growth process, keeps height down at same seed crystal, and therefore, but thermal field synchronous growth of the present invention goes out many crystal orientation unanimities, the uniform crystal of radial symmetry gradient; When guaranteeing that crystal mass is stable; Can significantly increase the crystalline production capacity, reduce production costs, shorten the production cycle.
The present invention also provides the synchronous growth of a kind of guided mode method many crystalline methods, and it is to adopt thermal field of the present invention, directly from melt, draws many crystalline methods of synchronous growth through the guided mode method, may further comprise the steps:
Raw material is packed in the crucible in the monocrystal growing furnace;
After vacuumizing in the monocrystal growing furnace, charging into protective atmosphere to stove internal gas pressure is standard atmospheric pressure;
Heat temperature raising dissolves raw material and becomes melt, and the constant temperature certain hour;
The a distance, top that seed crystal is suspended from the side-by-side mould in the crucible is roasting brilliant; After roasting brilliant several minutes; Seed crystal is slowly dropped on the side-by-side mould, make the abundant welding of melt on the upper surface of face of weld and each die blade of seed crystal, and realize many crystalline seedings;
After necking down and expanding the shoulder process, lift seed crystal, make many crystal carry out isodiametric growth, wherein, in the isodiametric growth process, keep the rate of pulling constant, the rate of pulling is 10～40mm/h;
After treating that many crystal break away from the upper surface of die blade fully under seed crystal lifts, stop to lift, the constant temperature certain hour begins cooling then, when treating that temperature is reduced to room temperature, promptly gets many crystal of synchronous growth.
Further, said " expand shoulder " realizes that through cooling and the method that lifts seed crystal wherein, rate of temperature fall is 1～2 ℃/h, and the rate of pulling is 0～5mm/h, and expanding the fillet degree is 120 °.
Further, the concrete operations step of said " after vacuumizing in the monocrystal growing furnace, charging into protective atmosphere to stove internal gas pressure is standard atmospheric pressure " is:
Being evacuated to vacuum tightness in the monocrystal growing furnace is 10
-3Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure, being evacuated to vacuum tightness again is 4 * 10
-3Pa～8 * 10
-3Behind the Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure once more.
Further, the concrete operations step of said " cooling " is: rate of temperature fall is 2KW/h～6KW/h.
Further, said crystal is sapphire crystal, garnet or silicon single-crystal.
Further, said crystal is sheet or arch sheet.
But adopt the synchronous growth of many crystalline methods of guided mode method of the present invention synchronous growth to go out many crystal, and many crystal mass that grow are stable, the crystal orientation is consistent, radial temperature is even, internal stress is little.
Description of drawings
Fig. 1 representes the structural representation of thermal field of the present invention;
The left view of Fig. 2 presentation graphs 1;
A-A is to structural representation in Fig. 3 presentation graphs 1;
Fig. 4 representes the structural representation of seed crystal.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and characteristic are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
As depicted in figs. 1 and 2; Provide the synchronous growth of a kind of guided mode method many crystalline thermal fields in the embodiment of the invention, the thermal field general structure in the equipment that itself and present guided mode method growing crystal are adopted is similar, comprises heating and heat-insulating device, crucible 1, guided mode mould and seed chuck device 3 at least; Wherein, Heating and heat-insulating device comprises alumina-ceramic base 41, zirconium white sand body 42, load coil 43, alumina ceramic tube 44, heating element 45 and stay-warm case, and crucible 1 is arranged on the inside of heating element 45, and the guided mode mould is arranged on crucible 1 inside; Stay-warm case is arranged at the top of heating element 45 and crucible 1; And the inside of stay-warm case has cavity, and it is around the periphery that is arranged on seed crystal 2 and seed chuck device 3, in order to guarantee many stay-in-grade crystal of synchronous growth; Thermal field of the present invention compared with prior art carries out following technological improvement:
Fig. 3 is that the position of crucible 1, heating element 45, guided mode mould and seed crystal 2 concerns vertical view; As shown in Figure 3; Crucible 1 in the thermal field of the present invention is along having the first side wall 11 and second sidewall 12 that is parallel to each other on its length direction, heating element 45 is for making the inside of crucible 1, the structure that equates with the first side wall 11, second sidewall, 12 equidistant position temperature; Be provided with side-by-side mould 5 in the crucible 1; This side-by-side mould 5 comprises a plurality of die blade 50 that are arranged side by side along crucible 1 length direction; The structure of a plurality of die blade 50 is identical, and the quantity of die blade 50 can be according to requirements set, and die blade 50 quantity are 8 among Fig. 2; Each die blade 50 equates to the first side wall 11 of crucible 1, the distance of second sidewall 12; And the upper surface of each die blade 50 all with size, the shape of the crystal section that will grow identical, on each die blade 50, also have the capillary seam that can the melt in the crucible 1 be guided to its upper surface and be arranged on die blade 50 upper surfaces and with the corresponding mould mouth of capillary seam, have on the die blade 50 that capillary is stitched and the structure of mould mouth is known technology; At this, the capillary of not drawing among figure seam and mould mouth; The bottom of seed crystal 2 has the face of weld 2a that can contact simultaneously with the upper surface of each die blade 50, and the face of weld 2a of seed crystal 2 contacts with the upper surface of each die blade 50 and the size of the contact surface that forms, measure-alike.
In the present embodiment; As shown in Figure 3, crucible 1 is designed to the rectangular body structure, and heating element 45 is designed to the rectangular structure with crucible 1 structure matching; Heating element 45 equates with the Aspect Ratio of crucible 1; And crucible 1 is arranged on the central position of heating element 45, and the first side wall of crucible 1 11, second sidewall 12 equate to the inwall distance of heating element 45, this structure just guaranteed crucible 1 inside, equate with its first side wall 11, second sidewall, 12 equidistant position temperature.In practical application; Crucible 1 can also be designed to have the first side wall 11 that is parallel to each other, the long strip shape structure of second sidewall 12; Heating element 45 is the long strip shape structure with crucible 1 structure matching; Can be implemented in the purpose that its first side wall 11 of crucible 1 inner distance and second sidewall, 12 equidistant position temperature equate equally, certainly, crucible 1 can also be other structure formation with heating element 45.
Crucible 1 and heating element 45 texture improvement in the thermal field of the present invention guarantee that the inside of crucible 1 equates with its first side wall 11, second sidewall, 12 equidistant position temperature; Side-by-side mould 5 is arranged in the crucible 1, and its each die blade 50 all equates with the distance of the first side wall 11, second sidewall 12, thereby the crystal radial temperature profile that has guaranteed growth on each die blade 50 is even, front and back are symmetrical, and internal stress is little; Simultaneously, adopt same seed crystal 2 to contact simultaneously with a plurality of die blade 50 in the thermal field of the present invention, many crystal can lift synchronism and the consistence that in seeding, necking down, expansion shoulder and isodiametric growth process, keeps height down at same seed crystal 2; Therefore, many crystal crystal orientation are consistent, uniform many crystal of radial symmetry gradient but thermal field synchronous growth of the present invention goes out, simultaneously; Guaranteeing under the stable situation of crystal mass; Can significantly increase the crystalline production capacity, reduce production costs, shorten the production cycle.
As shown in Figure 3, in the present embodiment, side-by-side mould 5 is fixed in the crucible 1 through positive stop strip 7.In practical application, side-by-side mould 5 can also be other fixed forms with the fixed form of crucible 1.
Thermal field of the present invention can be used for the tabular crystal of growing, and also can be used to the arch tabular crystal of growing.
In the present embodiment; With the crystal of being grown is that tabular crystal is an example; As shown in Figure 3, the upper surface of each die blade 50 is identical with the tabular crystal cross section, is to have the first edge 50a that is parallel to each other, the rectangle of the second edge 50b; Wherein, The first edge 50a is parallel with the first side wall 11 of crucible 1, and the second edge 50b is parallel with second sidewall 12 of crucible 1, and the first edge 50a of distance and each die blade 50 of the first edge 50a of each die blade 50 to the distance of the first side wall 11 of said crucible 1, the second edge 50b to second sidewall 12 of said crucible 1 all equates to the distance of the second edge 50b; The width that is side-by-side mould 5 is 1/3rd of crucible 1 width, thereby the crystal internal stress that guarantees growth on each die blade 50 is less.
As a kind of concrete embodiment; Shape and putting position according to side-by-side mould 5; The present invention provides a kind of preferred structure of seed crystal 2: like Fig. 1, Fig. 2, shown in Figure 4, seed crystal 2 has the T shape sheet of jut 2b for both sides, and the first side wall 11, second sidewall 12 that the flaky seed crystal 2 of this T shape is parallel to crucible 1 are provided with; And the distance of its first side wall 11 to crucible 1, second sidewall 12 equates; Promptly this seed crystal 2 is vertically installed in the upper surface of side-by-side mould 5 and is arranged on above the middle of side-by-side mould 5, and the lower surface of seed crystal 2 is face of weld 2a, and this face of weld 2a can contact with the upper surface of each die blade 50 simultaneously; The flaky seed crystal 2 of this T shape has been confirmed the direction of growth of wafer, and can guarantee that many crystal are in seeding, expansion shoulder and the medium-altitude synchronism of isodiametric growth process.
For with seed crystal 2 respective outer side edges; The present invention also provides a kind of seed chuck device 3; This seed chuck device 3 comprises two molybdenum system covers 31 that are connected with the jut 2b of seed crystal 2 both sides respectively; Each molybdenum system cover 31 has the snare structure of the jut 2b that is used to hold seed crystal 2, and the top of molybdenum system cover 31 is connected with pulling apparatus, and the tuck of the seed crystal 2 both sides molybdenum system that extend into is overlapped in 31 the snare structure; Thereby seed crystal 2 is hung over the bottom of molybdenum system cover 31; Between the upper surface of the snare structure of molybdenum system cover 31 and seed crystal 2, leave the space 31a that seed crystal 2 is moved up and down, when avoiding seed crystal 2 in the seeding process, to combine with side-by-side mould 5, the impact injury of the 2 pairs of side-by-side moulds 5 of seed crystal that cause owing to human error.
In practical application, the structure of seed crystal 2 can also have other structure formations of face of weld 2a for the bottom, seed chuck device 3 can for other forms of seed crystal 2 structure matching.
In the present embodiment, as depicted in figs. 1 and 2, the stay-warm case in the heating and heat-insulating device adopts the hard felt stay-warm case 46 of graphite; Its surface is brushed with oxidation-resistant coating, and the hard felt stay-warm case 6 of graphite is provided with first view port 461 and second view port 462 that is used to observe crystal growth, and first view port 461 and second view port 462 are symmetricly set on the both sides of seed crystal 2; Many crystal radial temperature symmetry to guarantee growth are good, and simultaneously, the hard felt of graphite is light easy to operate; Processing is simple, does not fall slag, does not ftracture, good reproducibility; Purity is high, has than the better heat-insulating property of metal products.
Also provide the synchronous growth of a kind of guided mode method many crystalline methods in the embodiments of the invention, it is to adopt thermal field of the present invention, directly from melt, draws many crystalline methods of synchronous growth through the guided mode method.To produce many sapphire wafers is example, and method of the present invention may further comprise the steps:
(1) raw material is handled: with purity is the high purity aluminium oxide (Al more than 99.999%
2O
3) after pure white powder piece dries in high temperature oxidation atmosphere, in the crucible 1 of packing into.
(2) monocrystal growing furnace shove charge: after the monocrystal growing furnace wiped clean; To pass through that high temperature is empty to be burnt and thermal field frocks such as the heating and heat-insulating device of dust removal process, crucible 1, side-by-side mould 5, seed chuck device 3 are placed in the monocrystal growing furnace; Require thermal field to put level; Can not occur tilting, each thermal field frock guarantees with one heart; Proofread and correct seed chuck device 3; Seed crystal 2 is connected seed chuck device 3 belows; And make the face of weld 2a of seed crystal 2 perpendicular to the middle of side-by-side mould 5; That is, the first side wall 11, second sidewall 12 of flaky seed crystal 2 with crucible 1 laterally arranged, and it is equated with the first side wall 11, second sidewall, 12 distances.
(3) vacuumize, applying argon gas: being evacuated to vacuum tightness in the monocrystal growing furnace is 10
-3Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure, being evacuated to vacuum tightness again is 4 * 10
-3Pa～8 * 10
-3Behind the Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure once more.
(4) dissolve raw material: heat temperature raising, heat temperature raising was undertaken by five steps, and the interval is 15 minutes between each step; The first step intensification power is 0～6Kw, and the second step intensification power is 6～12Kw, and the 3rd step intensification power is 12～8Kw; The 4th step intensification power is 18～24Kw; The 5th step intensification power is 24～30Kw, after dissolving fully to raw material, and constant temperature 1～3 hour.
(5) seeding: the 2～4mm place, mould mouth top that seed crystal 2 is suspended from the side-by-side mould 5 in the crucible 1 bakes brilliant; Melt in the crucible 1 is sewed on along the capillary of each die blade 50 and is walked to upper surface; On the upper surface of each die blade 50, form the melt thin layer, after roasting brilliant 20～60 minutes, seed crystal 2 is slowly dropped on each die blade 50 of side-by-side mould 5; Make the abundant welding of melt on the upper surface of face of weld 2a and each die blade 50 of seed crystal 2, thereby realize many crystalline seedings.
(6) necking down: the method through the rising melt temperature realizes necking down, and to reduce the hereditary defect in the seed crystal 2, in the necking down process, any non axial dislocation can progressively be excluded.
(7) expand shoulder: realize expanding shoulder through the method for lowering the temperature and low speed lifts, low speed lifts the expansion shoulder and helps eliminating dislocation and crystal boundary, wherein; Rate of temperature fall is 1～2 ℃/h, and the rate of pulling is 0～5mm/h, makes crystal slowly grow to both sides 50 centres along seed crystal 2 from die blade; Expansion fillet degree when expanding shoulder is good with about 120 ° generally; When expanding shoulder, wafer middle part temperature can not be too low, to avoid causing that polycrystalline or crystal burst; Expand shoulder until expand full till, standard is the crystalline width and the same wide the getting final product of mould mouth of die blade 50.
(8) isodiametric growth: after expanding the shoulder end, lift seed crystal 2, make many crystal carry out isodiametric growth, wherein, in the isodiametric growth process, keep the rate of pulling constant, the rate of pulling is advisable at 10～40mm/h.
(9) cooling: after treating that many crystal break away from the mould mouth 1～3mm of die blade 50 fully under seed crystal 2 lifts, stop to lift constant temperature 1～3 hour; Begin cooling then; Rate of temperature fall is undertaken by elder generation's fast principle in slow back, when treating that temperature is slowly reduced to room temperature between 2～6KW/h; Many crystalline growth endings promptly get many sapphire wafers of synchronous growth.
But adopt 8 of many crystalline methods of guided mode method of the present invention synchronous growth synchronous growths to be of a size of the sapphire single-crystal sheet that 55mm is wide, 3mm is thick, 450mm is long; When having solved many wafers of available technology adopting EFG method growth existing many wafer poor synchronization, each wafer crystal orientation differ, problems such as radial symmetry gradient is inhomogeneous, wafer dislocation desity height; The wafer that grows can be used as substrate, window, semiconducter device, high-accuracy component etc.; Method of the present invention is under the situation that guarantees crystal mass; Can significantly increase the sapphire production capacity, reduce production costs and shorten the production cycle.
Method of the present invention also may be used on other crystal series crystal growth technique, like garnet, silicon single-crystal etc., remedies the domestic technique blank, to sapphire industrialization induced effect.
The above is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from principle according to the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (12)
1. many crystalline thermal fields of guided mode method synchronous growth; The seed chuck device that it comprises heating and heat-insulating device at least, is arranged at the inner crucible of heating and heat-insulating device and is used to lift seed crystal; Said heating and heat-insulating device comprises the heating element that is used for heating crucible that is arranged at the crucible periphery, it is characterized in that:
Said crucible has the first side wall and second sidewall that is parallel to each other;
Said heating element is the inside that makes said crucible, the structure that equates with its first side wall and the equidistant position of second sidewall temperature;
Be provided with the side-by-side mould in the said crucible; Said side-by-side mould comprise be fixed in the said crucible side by side, a plurality of die blade that structure is identical; Each die blade equates to the distance of the first side wall of said crucible, second sidewall, and the upper surface of each die blade all with crystalline sectional dimension, the shape that will grow identical;
The top of said side-by-side mould is provided with said seed crystal; Said seed crystal bottom has the face of weld that can contact simultaneously with the upper surface of each die blade, and the face of weld of said seed crystal contacts with the upper surface of each die blade and the size of the contact surface that forms, measure-alike.
2. thermal field according to claim 1 is characterized in that: said crucible is the square body structure, and said heating element is and the square body structure of said crucible structure matching that the first side wall of said crucible, second sidewall equate to the inwall distance of said heating element.
3. thermal field according to claim 1 is characterized in that: said the crystal that will grow is sheet or arch sheet;
The upper surface of each die blade all have first edge parallel with the first side wall of said crucible and with second edge of second parallel sidewalls of said crucible, and first edge of distance and each die blade of first edge of each die blade to the distance of the first side wall of said crucible, second edge to second sidewall of said crucible all equates to the distance at second edge.
4. according to each described thermal field of claim 1 to 3; It is characterized in that: said seed crystal is the T shape sheet that both sides have jut; The flaky seed crystal of this T shape is parallel to the first side wall, the second sidewall setting of said crucible; And equate that to the distance of the first side wall of said crucible, second sidewall lower surface of said seed crystal forms the said face of weld that can contact simultaneously with the upper surface of each die blade;
Said seed chuck device comprises two molybdenum system covers that are connected with the jut of said seed crystal both sides respectively, and said molybdenum system tackling is useful on the snare structure of the jut that holds said seed crystal; The tuck of said seed crystal extend in the snare structure of said molybdenum system cover, puts thereby said seed crystal is hung over said molybdenum system.
5. thermal field according to claim 4 is characterized in that: said heating and heat-insulating device also comprises the hard felt stay-warm case of graphite, and it is arranged at the top of said heating element and crucible, and around the periphery that is arranged on said seed crystal and seed chuck device; The surface of the hard felt stay-warm case of said graphite is brushed with oxidation-resistant coating; The hard felt stay-warm case of said graphite is provided with first view port and second view port of being convenient to observe crystal growth, and said first view port and said second view port are symmetricly set on the both sides of said seed crystal.
6. many crystalline methods of guided mode method synchronous growth is characterized in that, it is to adopt like each described thermal field of claim 1 to 5, directly from melt, draw many crystalline methods through the guided mode method, may further comprise the steps:
Raw material is packed in the crucible in the monocrystal growing furnace;
After vacuumizing in the monocrystal growing furnace, charging into protective atmosphere to stove internal gas pressure is standard atmospheric pressure;
Heat temperature raising dissolves for behind the melt constant temperature certain hour to raw material;
Seed crystal is dropped on the side-by-side mould, make the abundant welding of melt on the upper surface of face of weld and each die blade of seed crystal bottom, realize many crystalline seedings;
After necking down, expanding shoulder, lift seed crystal, make many crystal carry out isodiametric growth;
After many isodiametric growth of crystal finished, cooling promptly got many crystal of synchronous growth.
7. method according to claim 6 is characterized in that: said " expanding shoulder " realizes that through the method that cooling and low speed lift seed crystal wherein, rate of temperature fall is 1～2 ℃/h, and the rate of pulling is 0～5mm/h, and expanding the fillet degree is 120 °.
8. method according to claim 6 is characterized in that: in said isodiametric growth process, keep the rate of pulling constant, the rate of pulling is 10～40mm/h.
9. method according to claim 6 is characterized in that, the concrete operations step of said " after vacuumizing in the monocrystal growing furnace, charging into protective atmosphere to stove internal gas pressure is standard atmospheric pressure " is:
Being evacuated to vacuum tightness in the monocrystal growing furnace is 10
-3Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure, being evacuated to vacuum tightness again is 4 * 10
-3Pa～8 * 10
-3Behind the Pa, argon filling to stove internal gas pressure is a standard atmospheric pressure once more.
10. method according to claim 6 is characterized in that, the rate of temperature fall of said " cooling " is 2KW/h～6KW/h.
11. method according to claim 6 is characterized in that: said crystal is sapphire crystal, garnet or silicon single-crystal.
12. according to each described method of claim 6 to 11, it is characterized in that: said crystal is sheet or arch sheet.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN103422162A (en) * | 2013-09-03 | 2013-12-04 | 无锡鼎晶光电科技有限公司 | Single crystal furnace thermal field structure for square sapphire generation |
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| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
| CN105189837A (en) * | 2013-03-15 | 2015-12-23 | 圣戈本陶瓷及塑料股份有限公司 | Sapphire ribbons and apparatus and method for producing a plurality of sapphire ribbons having improved dimensional stability |
| CN106498488A (en) * | 2016-10-28 | 2017-03-15 | 同济大学 | Multiple doping CaF are grown simultaneously2The device of crystal and the preparation method based on the device |
| CN106702481A (en) * | 2017-03-20 | 2017-05-24 | 宁夏佳晶科技有限公司 | Improved multi-flake guide-die artificial sapphire preparation technology |
| CN107059114A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | The mould and method of a kind of EFG technique growth crystal optical fibre |
| CN108570707A (en) * | 2017-03-09 | 2018-09-25 | 中科钢研节能科技有限公司 | EFG technique sapphire crystallization system |
| CN110983431A (en) * | 2019-11-28 | 2020-04-10 | 中国科学院包头稀土研发中心 | Heating and heat-insulating device for producing rare earth eutectic fluorophor by guide die method |
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| CN103060901B (en) * | 2013-02-05 | 2015-04-22 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN105189837A (en) * | 2013-03-15 | 2015-12-23 | 圣戈本陶瓷及塑料股份有限公司 | Sapphire ribbons and apparatus and method for producing a plurality of sapphire ribbons having improved dimensional stability |
| CN103422162A (en) * | 2013-09-03 | 2013-12-04 | 无锡鼎晶光电科技有限公司 | Single crystal furnace thermal field structure for square sapphire generation |
| CN103696005A (en) * | 2014-01-07 | 2014-04-02 | 镇江和和蓝晶科技有限公司 | Mold for simultaneous growth of multiple sapphire tubes through edge-defined film-fed growth technique |
| CN103696004A (en) * | 2014-01-07 | 2014-04-02 | 镇江和和蓝晶科技有限公司 | Mold for simultaneously growing multiple thin platy sapphires by edge-defined film-fed growth technique |
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| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN103806102B (en) * | 2014-02-14 | 2017-01-11 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
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| CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
| CN106498488A (en) * | 2016-10-28 | 2017-03-15 | 同济大学 | Multiple doping CaF are grown simultaneously2The device of crystal and the preparation method based on the device |
| CN106498488B (en) * | 2016-10-28 | 2019-04-02 | 同济大学 | A variety of doping CaF are grown simultaneously2The device of crystal and preparation method based on the device |
| CN107059114A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | The mould and method of a kind of EFG technique growth crystal optical fibre |
| CN108570707A (en) * | 2017-03-09 | 2018-09-25 | 中科钢研节能科技有限公司 | EFG technique sapphire crystallization system |
| CN108570707B (en) * | 2017-03-09 | 2020-06-16 | 中科钢研节能科技有限公司 | Sapphire crystal growth system by guided mode method |
| CN106702481A (en) * | 2017-03-20 | 2017-05-24 | 宁夏佳晶科技有限公司 | Improved multi-flake guide-die artificial sapphire preparation technology |
| CN106702481B (en) * | 2017-03-20 | 2019-01-29 | 宁夏佳晶科技有限公司 | A kind of improved multiple-piece EFG technique synthetic sapphire preparation process |
| CN110983431A (en) * | 2019-11-28 | 2020-04-10 | 中国科学院包头稀土研发中心 | Heating and heat-insulating device for producing rare earth eutectic fluorophor by guide die method |
| CN110983431B (en) * | 2019-11-28 | 2021-04-23 | 中国科学院包头稀土研发中心 | Heating and heat-preserving device for producing rare earth eutectic fluorophor by mold guiding method and crystal growing furnace |
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