CN104862775A - Growth device for sapphire crystal hemisphere cover and growth method for sapphire crystal hemisphere cover - Google Patents
Growth device for sapphire crystal hemisphere cover and growth method for sapphire crystal hemisphere cover Download PDFInfo
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Abstract
The invention relates to a growth device and a growth method for a sapphire crystal hemisphere cover by employing an edge-defined film-fed crystal growth method. The method specifically comprises the following main steps: respectively introducing a protective gas and a cooling gas into a crystal growth furnace and a cooler pan; heating the crystal growth furnace until a high-purity aluminum oxide material is fused; adjusting a hoist pan, so that aluminum oxide melt ascends to the top end of a mold along a center through hole and an annular capillary fissure in the symmetric axis of the mold; descending seed crystal to fuse with the aluminum oxide melt; under the action of affinity and surface tension, enhancing radiation heat exchange between a growth interface and the gas cooler pan by adjusting the flow of the cooling gas in the cooler pan, so as to quicken the expansion of the crystal; and finally limiting the expansion of the crystal by the top edge of the mold. The growth device has the advantages that supply of the melt in the mold is adjusted by controlling the relative positions of the mold and the crucible; continuous providing of the melt in the capillary fissure is ensured, so as to realize continuous growth; and a hexagonal annular cooler pan is prevented from being carbonized to deform by employing the cooling gas.
Description
Technical field
The invention belongs to field of crystal growth, relate to a kind of growing apparatus and growth method of sapphire crystal, particularly a kind of growing apparatus of sapphire crystal half ball cover and growth method thereof.
Background technology
The growth existing a variety of method at present of sapphire crystal material, mainly contain: kyropoulos (Kyropolous method, be called for short Ky method), EFG technique (i.e. Edge Defined Film-fed Growth techniques method, be called for short EFG method), heat-exchanging method (i.e. Heat Exchange Method method, be called for short HEM method), crystal pulling method (Czochralski method is called for short Cz method), Bridgman method (Bridgman method, falling crucible method) etc.
Leading film ratio juris is utilize the capillary on mould to stitch, by capillarity, the raw material in crucible is promoted to die tip.
In current growing sapphire crystal process, rely on the hard felt or metal screen placed near mould, or by gaseous exchange heat exchange, above growth interface, crystalline temp is to drive crystal growth, and the shortcoming of the method is:
(1) only insulation quilt or metal screen is relied on, or gaseous exchange heat exchange, when along with when crystal diameter is comparatively large or thickness is thicker, carbon felt or metal screen its to the thermolysis rapid decay in growth interface centre, metal screen, after high temperature deformation, further causes crystal growth interface radiating condition uneven, makes growth interface shape uneven, result in crystals bubble many, and the undercooling of crystal is exacerbated to stress and the dislocation issues of crystal; Meanwhile, the carbon felt near growth interface can cause carbon to mix crystal, also can affect crystal mass;
(2) processing method that seed crystal and mould phase position constantly move is utilized, but motion seed crystal and mould cannot guarantee growth interface stable be positioned on the symmetry axis of thermal field, therefore growth interface is easily out of shape and unstable, and the growth interface of relative movement, increase the difficulty that crystal mass controls further, and be also difficult to continuous acquisition due to preceding factors major diameter sapphire crystal.
Therefore, be badly in need of a kind of sapphire growth apparatus that can dispel the heat with larger growth interface being compared to uniformity of research and development and method, realize growth continuously simultaneously, meet market application to reduce costs.
Summary of the invention
The technical problem to be solved in the present invention is to provide and a kind ofly can ensures that growth interface dispels the heat and realizes sapphire crystal half ball cover EFG technique growing apparatus and the growth method thereof of continuously growth with comparing uniformity.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of sapphire crystal half ball cover EFG technique growing apparatus, comprise crystal growing furnace and be arranged on crucible in stove, mould, hanging scaffold and be arranged on the suspension rod of hanging scaffold upper surface, the lower end of described mould is immersed in the aluminum oxide liquation in crucible, and its end, upper end is arranged on hanging scaffold center and drives it to move up and down by suspension rod;
Its innovative point is: described suspension rod is also installed a gas cooling dish, and described gas cooling dish is a hollow cylinder with revolving structure, and this gas cooling dish is horizontally set on the top of hanging scaffold; The center of described gas cooling dish is a seeding passage supplying seed crystal decline seeding or crystal growth, and its inner side-wall has some layers equally distributed cooling fin vertically; In the form of a ring, its hollow arranges and forms a ring cavity passed into for cooling gas described every layer of cooling fin; Described gas cooling dish both sides have one and are symmetrical arranged and the induction trunk extended vertically and outlet passageway, the top of described induction trunk is a total inlet mouth, its lower end has some inlet mouths be communicated with ring cavity, the top of described outlet passageway is a total air outlet, and its lower end has some air outlets be communicated with ring cavity; Described mould is a cylinder with rotary structure, its center, upper surface has the hemispherical groove that supplies crystal growth, the bottom centre of this hemispherical groove has one to axially extend to mold bottom central through hole along mould, described die edge has an annular capillary seam, and this annular capillary seam extends to mold bottom by die top; The bottom of described mould has a foot passage communicated with mold center through hole; Described gas cooling dish and mould are coaxially arranged, and by suspension rod drive its simultaneously near or away from the crucible of below.
Further, described gas cooling dish is sexangle ring-type.
Further, described gas cooling dish is W/Mo salver.
Use a method for above-mentioned sapphire crystal half ball cover EFG technique growing apparatus growing crystal, its innovative point is: described method concrete steps are as follows:
Step S1: put into the high purity aluminium oxide starting material that purity is greater than 99.995% in crucible, mould is fixed on hanging scaffold simultaneously, and the capillary of mould seam is all submerged in crucible;
Step S2: pass into protective gas and cooling gas respectively in crystal growing furnace and coolship, crystal growing furnace is warming up to the fusing of high purity aluminium oxide starting material, hanging scaffold is regulated to make aluminum oxide liquation sew on along the central through hole on mould symmetry axis and annular capillary the top being raised to mould, decline seed crystal and aluminum oxide liquation fuse together, under avidity and capillary effect, utilize the flow regulating cooling gas in coolship, radiation heat transfer between enhancing growth interface and gas cooling dish is to accelerate the expansion of crystal, the expansion of crystal is edge limited by die top eventually,
Step S3: stop the pulling growth that crystal is vertical, and adjustment makes hanging scaffold and crucible relative movement, by mold bottom passage emersion liquation;
Step S4: after shielding gas flows into mould inside by mold bottom, again regulate the relative position of hanging scaffold and crucible, die tip is made to immerse in aluminum oxide liquation, now start vertical pulling growth and utilize the flow of gas in adjustments of gas coolship, the melt films of die edge of going bail for is that crystal continues feed; When aluminum oxide liquation flows back into die tip from mold center's through hole, stop or slowly vertically lift and adjust the radiation heat transfer condition between growth interface and coolship, and regulate the power of well heater, because the semisphere of mould designs, crystal constantly can be grown to central stabilizer by edge in this thermoregulator process, utilizing the continuous change of mould and crucible relative position, the liquid realized in mould hemisphere groove is flowed back in crucible lentamente by mold center hole; After crystal is completed to central growth by die edge, realize first half ball cover growth;
Step S5: regulate the gas flow of coolship and the power of calorifier, guarantee that mould extension has the liquation film of suitable thickness to exist, the relative position of adjustment hanging scaffold and crucible makes the passage emersion liquation of mold bottom, in relative movement by gas flow in controlled cooling model dish to control growth interface solution film thickness, guarantee that furnace pressure and mould inside liquation pressure reduction and capillary force balance, when protective gas flows into mould inside through mold bottom passage, after mould inner melt flows back to crucible, process of growth again in repeating step S4, until melt cannot be sewed on by annular capillary and rises to die tip in crucible,
Step S6: after crystal growth completes, suspension rod of slinging, mold removal, pulls down hanging scaffold.
Further, described protective gas and cooling gas are Ar, CO and CO
2mixed gas.
The invention has the advantages that:
(1) growing apparatus of the present invention, in crystal growing process, utilize the gas cooling dish be arranged on suspension rod, controlled cooling model dish temperature is carried out with growth interface by gas flow in adjustments of gas coolship, avoid conventional carbon felt or metal screen, or gaseous exchange heat exchange only crystals cooled and cannot the situation of Homogeneous cooling growth interface inside, thus obtain uniform and stable growth interface to obtain high-quality sapphire crystal; Gas cooling dish is a hollow cylinder, and has the heat loss through radiation structure of multilayer cooling fin, and crystal grows in the seeding passage of hollow cylinder, this kind of structure good cooling results, and cooling evenly;
Mould makes the crucible of itself and below realize relative movement in the vertical direction by suspension rod, because it is rotary structure, all the time be positioned on the geometirc symmetry axis of thermal field during motion, ensure that symmetrical crystal growth interface, the central through hole at place of mold center, convenient when crucible and the change of mould relative position, liquation flows in mould inside top and crucible, the annular capillary seam of die edge, guarantee that the liquation in crucible can rise to die edge all the time to keep the connection of crystal and liquation, the passage of mold bottom, it is convenient when crucible and mould relative position change, in stove, protective gas imports mould inside top, thus force top inner melt to flow back to crucible, the hemispherical dome structure of mould inside, the shape meeting half ball cover to the full extent optimizes temperature distribution simultaneously, ensure that growth is achieved continuously,
(2) the gas cooling dish in growing apparatus of the present invention is sexangle ring-type, and at growing sapphire crystal half ball cover, select the radiating surface of crystal to be a face or m face, gas cooling dish is sexangle ring-type, can improve the Homogeneouslly-radiating effect of growth interface;
(3) the gas cooling dish in growing apparatus of the present invention is metal W/Mo dish, avoids the pollution of graphite material to growth interface;
(4) growth method of the present invention is for guaranteeing continuous growing sapphire crystal half ball cover, the relative position of mould and crucible must be regulated in process of growth, utilize central through hole and the foot passage of mold center's part, control the liquation in crucible or protective atmosphere inflow die top, in mould and crucible relative movement thereof, need the temperature regulating coolship, to guarantee that melt films thickness is worked as relative position and regulated complete, start in the technological process grown, regulate the airshed of coolship, simultaneously owing to utilizing mould inside semisphere to design, realize that die edge temperature is high and central through hole place temperature is low, when liquation gets back to die tip again, stop or slowly vertical lift be that crystalizing interface Homogeneouslly-radiating coordinates calorifier power regulation simultaneously by coolship, the relative position of continuous adjustment crucible and mould, then crystal ecto-entad growth, ensure that the melt films thickness of the crystalizing interface of growth position meets the demands, then tend towards stability in crystalizing interface limit, smooth and stable crystalizing interface avoids the generation of bubble and dislocation, thus improve crystal mass.
(5) the property shielding gas in sapphire growth method of the present invention and cooling gas are Ar, CO and CO
2mixed gas; this Combination shielding gas can effectively inhibited oxidation aluminium 2100 degree to 2200 degree evaporation while; in the aluminum oxide steam that can also effectively avoid evaporating and thermal field, other graphite material materials react; improve the work-ing life of thermal field; can effectively inhibited oxidation aluminium, graphite, Mo and W be anti-mutually; ensure that metal cools screen because being out of shape the ununiformity causing thermal field, can not extending its work-ing life, reducing cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of sapphire crystal EFG technique of the present invention growing apparatus.
Fig. 2 is the vertical view of coolship in a kind of sapphire crystal EFG technique of the present invention growing apparatus.
Fig. 3 is the crystal orientation schematic diagram of sapphire crystal.
Fig. 4 is the schematic diagram of step S1 in a kind of sapphire crystal EFG technique of the present invention growth method.
Fig. 5 is the schematic diagram of step S2 in a kind of sapphire crystal EFG technique of the present invention growth method.
Fig. 6 is the schematic diagram of step S3 in a kind of sapphire crystal EFG technique of the present invention growth method.
Fig. 7, Fig. 8 and Fig. 9 are the schematic diagram of step S4 in a kind of sapphire crystal EFG technique of the present invention growth method.
Figure 10 is the schematic diagram of step S5 in a kind of sapphire crystal EFG technique of the present invention growth method.
Embodiment
As shown in Figure 1, the invention discloses a kind of sapphire crystal half ball cover EFG technique growing apparatus, comprise crystal growing furnace and be arranged on crucible 1 in stove, mould 2, hanging scaffold 3 and be arranged on the suspension rod 4 of hanging scaffold 3 upper surface, the lower end of mould 2 is immersed in the aluminum oxide liquation 5 in crucible 1, and its end, upper end is arranged on hanging scaffold 3 center and drives it to move up and down by suspension rod 4; Suspension rod 4 is also installed a gas cooling dish 6, gas cooling dish 6 is a hollow cylinder with revolving structure, and this gas cooling dish 6 is horizontally set on the top of hanging scaffold 3; The center of gas cooling dish 6 is a seeding passage 7 declining seeding or crystal growth for seed crystal 20, and its inner side-wall has some layers equally distributed cooling fin 8 vertically; In the form of a ring, its hollow arranges and forms a ring cavity 9 passed into for cooling gas every layer of cooling fin 8; Gas cooling dish 6 both sides have one and are symmetrical arranged and the induction trunk 10 extended vertically and outlet passageway 11, the top of induction trunk 10 is a total inlet mouth 12, its lower end has some inlet mouths 14 be communicated with ring cavity 9, the top of outlet passageway 11 is a total air outlet 13, and its lower end has some air outlets 15 be communicated with ring cavity 9; Mould 2 is a cylinder with rotary structure, its center, upper surface has the hemispherical groove 16 that supplies crystal growth, the bottom centre of this hemispherical groove 16 has one and axially extends to central through hole 17 bottom mould 2 along mould 2, mould 2 edge has an annular capillary seam 18, and this annular capillary seam 18 extends to bottom mould 2 by mould 2 top; The bottom of mould 2 has a foot passage 19 communicated with mould 2 central through hole 17; Gas cooling dish 6 and mould 2 are coaxially arranged, and by suspension rod 4 drive its simultaneously near or away from the crucible 1 of below; In the present embodiment, as shown in Figure 2, gas cooling dish 6, in sexangle ring-type, like this at growing sapphire crystal half ball cover, as shown in Figure 3, is selected the radiating surface of half ball cover to be a face or m face, can be improved the Homogeneouslly-radiating effect of growth interface; In addition in order to avoid graphite material is to the pollution of growth interface, gas cooling dish 6 is W/Mo salver.
Use a method for above-mentioned sapphire crystal half ball cover EFG technique growing apparatus growing crystal, its innovative point is: method concrete steps are as follows:
Step S1: as shown in Figure 4, puts into the high purity aluminium oxide starting material that purity is greater than 99.995%, is fixed on hanging scaffold 3 by mould 2 simultaneously in crucible 1, and makes the capillary of mould 2 seam all be submerged in crucible 1;
Step S2: as shown in Figure 5, protective gas and cooling gas is passed into respectively in crystal growing furnace and coolship, crystal growing furnace is warming up to the fusing of high purity aluminium oxide starting material, hanging scaffold 3 is regulated to make aluminum oxide liquation 5 rise to the top of mould 2 along the central through hole 17 on mould 2 symmetry axis and annular capillary seam 18, decline seed crystal 20 and aluminum oxide liquation 5 fuse together, under avidity and capillary effect, utilize the flow regulating cooling gas in coolship, radiation heat transfer between enhancing growth interface and gas cooling dish 6 is to accelerate the expansion of crystal, the expansion of crystal is limited by mould 2 top eventually,
Step S3: as shown in Figure 6, stops the pulling growth that crystal is vertical, and adjustment makes hanging scaffold 3 and crucible 1 relative movement, by mould 2 foot passage 19 emersion liquation;
Step S4: as shown in Figure 7, when shielding gas is by after flowing into mould 2 inside bottom mould 2, again regulate the relative position of hanging scaffold 3 and crucible 1, mould 2 top is made to immerse in aluminum oxide liquation 5, now start vertical pulling growth and utilize the flow of gas in adjustments of gas coolship 6, the melt films at mould 2 edge of going bail for is that crystal continues feed; As shown in Figure 8, when aluminum oxide liquation 5 flows back into mould 2 top from the central through hole 17 of mould 2, stop or slowly vertically lift and adjust the radiation heat transfer condition between growth interface and coolship, and regulate the power of well heater, because the semisphere of mould 2 designs, crystal constantly can be grown to central stabilizer by edge in this thermoregulator process; As shown in Figure 9, in the continuous change utilizing mould 2 with crucible 1 relative position, the liquid in the hemispherical groove 16 of mould 2 flows back in crucible 1 by mould 2 centre hole lentamente; After crystal is completed to central growth by mould 2 edge, realize first half ball cover growth;
Step S5: as shown in Figure 9, regulate the gas flow of coolship and the power of calorifier, guarantee that mould 2 extension has the liquation film of suitable thickness to exist, adjustment hanging scaffold 3 and the relative position of crucible 1 make the passage emersion liquation bottom mould 2, in relative movement by gas flow in controlled cooling model dish to control growth interface solution film thickness, guarantee that furnace pressure and the inner liquation pressure reduction of mould 2 and capillary force balance, when protective gas flows into mould 2 inside through mould 2 foot passage 19, after mould 2 inner melt flows back to crucible 1, process of growth again in repeating step S4, until melt cannot rise to mould 2 top by annular capillary seam 18 in crucible 1,
Step S6: after crystal growth completes, suspension rod 4 of slinging, mold removal 2, pulls down hanging scaffold 3.
Protective gas in above-mentioned steps S1-S6 and cooling gas are Ar, CO and CO
2mixed gas.
Mentality of designing of the present invention:
(1) growing apparatus of the present invention, in crystal growing process, utilize the gas cooling dish 6 be arranged on suspension rod 4, controlled cooling model dish temperature is carried out with growth interface by gas flow in adjustments of gas coolship 6, avoid conventional carbon felt or metal screen, or gaseous exchange heat exchange only crystals cooled and cannot the situation of Homogeneous cooling growth interface inside, thus obtain uniform and stable growth interface to obtain high-quality sapphire crystal; Gas cooling dish 6 is a hollow cylinder, and has the heat loss through radiation structure of multilayer cooling fin, and crystal grows in the seeding passage 7 of hollow cylinder, this kind of structure good cooling results, and cooling evenly;
Mould 2 makes the crucible 1 of itself and below realize relative movement in the vertical direction by suspension rod 4, because it is rotary structure, all the time be positioned on the geometirc symmetry axis of thermal field during motion, ensure that symmetrical crystal growth interface, the central through hole 17 of mould 2 center, convenient when crucible 1 and the change of mould 2 relative position, liquation flows in mould 2 inner tip and crucible 1, the annular capillary seam 18 at mould 2 edge, guarantee that the liquation in crucible 1 can rise to mould 2 edge all the time to keep the connection of crystal and liquation, passage bottom mould 2, it is convenient when crucible 1 changes with mould 2 relative position, in stove, protective gas imports mould 2 inner tip, thus force top inner melt to flow back to crucible 1, the hemispherical dome structure of mould 2 inside, the shape meeting half ball cover to the full extent optimizes temperature distribution simultaneously, ensure that growth is achieved continuously,
(2) the gas cooling dish 6 in growing apparatus of the present invention is in sexangle ring-type, and at growing sapphire crystal half ball cover, select the radiating surface of crystal to be a face or m face, gas cooling dish 6 is sexangle ring-type, can improve the Homogeneouslly-radiating effect of growth interface; Gas cooling dish 6 is metal W/Mo dish, avoids the pollution of graphite material to growth interface;
Adopt metal W/Mo to avoid the pollution of graphite material to growth interface, it sees formula [1] and [2] to the radiating of growth interface:
q
1= Nu
L* (T
s- T
g) * λ / L [1]
q
2= ε* σ * (T
s+ T
cf) * （T
s 2+ T
cf 2） * （T
s- T
cf）[2]
Formula [1] indicates and controls gas flow to the control situation of coolship, considers the high transmission characteristic of sapphire crystal, wherein q simultaneously
1for heat flux, Nu
lfor Nu Saier coefficient, T
sfor coolship temperature, T
gfor passing into gas temperature, λ is thermal conductivity, and L is characteristic length; Formula [2] indicates the cooling situation of coolship to whole crystal growth interface, is wherein ε radiation coefficient, and σ is Boltzmann Changshu, T
scoolship temperature, T
cfbe crystalline temp, should choose plane of crystal respectively and crystals is compared in computation process, simultaneously from [1], utilize coolship inner air path design, the temperature distribution optimizing coolship cools uniformly to guarantee that the growth interface of crystal obtains;
As shown in Figure 3, because sapphire crystal is close-packed hexagonal structure, and half ball cover need select C to being direction, ball top, according to formula Г=1/2 * (E
hkl b+ E
hkl s) interfacial energy in [3] its each face known all has larger difference, Γ in formula
hklfor lattice parameter in crystal unit interval is the relaxation energy of hkl, E
b hklfor lattice parameter in crystal unit interval is the volume energy of hkl, E
s hklfor lattice parameter in crystal unit interval is the interfacial energy of hkl, according to choosing the minimum and a large amount of experiment of energy as a reference, the present invention selects radiating surface to be A face or M face, therefore gas cooling dish is sexangle ring-type, according to the function that radiation coefficient ε in formula [2] is angle and temperature etc., therefore to the Homogeneouslly-radiating effect seeing optimization with suiting measures to local conditions outside coolship also can improve growth interface;
(3) growth method of the present invention is for guaranteeing continuous growing sapphire crystal half ball cover; the relative position of mould and crucible must be regulated in process of growth; utilize central through hole and the foot passage of mold center's part; control the liquation in crucible or protective atmosphere inflow die top, according to formula [4]:
dh/dt = v – ξ
-1* [λ1 * (Tm – Tcf) –λ2 * (Tcf – Ts)]/h [4]
Wherein dh/dt represents melt films thickness and changes in time, and v is lift or the speed of growth, and ξ is latent heat, λ
1for the thermal conductivity of melt, T
mfor Die head temperatures, T
cffor crystallization front temperature, λ
2for crystal thermal conductivity, T
s iscrystalline temp, h is melt liquid membrane, known due to T by formula [4]
mconstant and v equals 0, melt films thickness h only and T
sabout therefore in mould and crucible relative movement thereof, need the temperature regulating coolship Ts, to guarantee melt films thickness h, meet formula [5]:
ΔH*ρ*g*s + Δp * S = 4*π*r*cosΘ(h)*α [5]
Δ H is melt liquid level difference of altitude in melt liquid level height and mould in crucible, ρ is fusant density, g is universal gravity constant, s waits small area, Δ p is that in body of heater, in atmosphere pressures and mould, space pressure is poor, S waits small area, r is die tip radius, cos Θ is the infiltration angle between melt and mould, relevant with melt films thickness h, α is coefficient of surface tension, on the left of equation, Section 1 is the pressure difference because crucible inner melt in relative position moving process and mould inner melt liquid level difference cause, Section 2 is the pressure difference that in mould, gas causes because of compression or expansion, balance with capillary force on the right side of equation, need avoid that h is excessive to be exceeded or close to 2mm, cause the situation that Θ sharply reduces close to 90 ° of capillary forces,
When relative position regulates complete, start, in the technological process grown, the airshed of coolship be regulated, according to formula [6]:
h = R*sinα[ arch(h/（2*r*sinα）)-arch(1/sinα)] [6]
Simultaneously owing to utilizing mould inside semisphere to design, realize that die edge temperature is high and central through hole place temperature is low, when liquation gets back to die tip again, stop or slowly vertical lift be that crystalizing interface Homogeneouslly-radiating coordinates calorifier power regulation simultaneously by coolship, the relative position of continuous adjustment crucible and mould, then crystal ecto-entad growth, ensure that the melt films thickness h of the crystalizing interface of growth position meets equation [6], then tend towards stability in crystalizing interface limit, smooth and stable crystalizing interface avoids the generation of bubble and dislocation, thus improve crystal mass,
(4) the property shielding gas in sapphire growth method of the present invention and cooling gas are Ar, CO and CO
2mixed gas; this Combination shielding gas can effectively inhibited oxidation aluminium 2100 degree to 2200 degree evaporation while; in the aluminum oxide steam that can also effectively avoid evaporating and thermal field, other graphite material materials react; improve the work-ing life of thermal field; can effectively inhibited oxidation aluminium, graphite, Mo and W be anti-mutually; ensure that metal cools screen because being out of shape the ununiformity causing thermal field, can not extending its work-ing life, reducing cost.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (5)
1. a sapphire crystal half ball cover EFG technique growing apparatus, comprise crystal growing furnace and be arranged on crucible in stove, mould, hanging scaffold and be arranged on the suspension rod of hanging scaffold upper surface, the lower end of described mould is immersed in the aluminum oxide liquation in crucible, and its end, upper end is arranged on hanging scaffold center and drives it to move up and down by suspension rod;
It is characterized in that: described suspension rod is also installed a gas cooling dish, described gas cooling dish is a hollow cylinder with revolving structure, and this gas cooling dish is horizontally set on the top of hanging scaffold; The center of described gas cooling dish is a seeding passage supplying seed crystal decline seeding or crystal growth, and its inner side-wall has some layers equally distributed cooling fin vertically; In the form of a ring, its hollow arranges and forms a ring cavity passed into for cooling gas described every layer of cooling fin; Described gas cooling dish both sides have one and are symmetrical arranged and the induction trunk extended vertically and outlet passageway, the top of described induction trunk is a total inlet mouth, its lower end has some inlet mouths be communicated with ring cavity, the top of described outlet passageway is a total air outlet, and its lower end has some air outlets be communicated with ring cavity;
Described mould is a cylinder with rotary structure, its center, upper surface has the hemispherical groove that supplies crystal growth, the bottom centre of this hemispherical groove has one to axially extend to mold bottom central through hole along mould, described die edge has an annular capillary seam, and this annular capillary seam extends to mold bottom by die top; The bottom of described mould has a foot passage communicated with mold center through hole;
Described gas cooling dish and mould are coaxially arranged, and by suspension rod drive its simultaneously near or away from the crucible of below.
2. sapphire crystal half ball cover EFG technique growing apparatus according to claim 1, is characterized in that: described gas cooling dish is sexangle ring-type.
3. sapphire crystal half ball cover EFG technique growing apparatus according to claim 1, is characterized in that: described gas cooling dish is W/Mo salver.
4. use a method for the sapphire crystal half ball cover EFG technique growing apparatus growing crystal described in claim 1, it is characterized in that: described method concrete steps are as follows:
Step S1: put into the high purity aluminium oxide starting material that purity is greater than 99.995% in crucible, mould is fixed on hanging scaffold simultaneously, and the capillary of mould seam is all submerged in crucible;
Step S2: pass into protective gas and cooling gas respectively in crystal growing furnace and coolship, crystal growing furnace is warming up to the fusing of high purity aluminium oxide starting material, hanging scaffold is regulated to make aluminum oxide liquation sew on along the central through hole on mould symmetry axis and annular capillary the top being raised to mould, decline seed crystal and aluminum oxide liquation fuse together, under avidity and capillary effect, utilize the flow regulating cooling gas in coolship, radiation heat transfer between enhancing growth interface and gas cooling dish is to accelerate the expansion of crystal, the expansion of crystal is edge limited by die top eventually,
Step S3: stop the pulling growth that crystal is vertical, and adjustment makes hanging scaffold and crucible relative movement, by mold bottom passage emersion liquation;
Step S4: after shielding gas flows into mould inside by mold bottom, again regulate the relative position of hanging scaffold and crucible, die tip is made to immerse in aluminum oxide liquation, now start vertical pulling growth and utilize the flow of gas in adjustments of gas coolship, the melt films of die edge of going bail for is that crystal continues feed; When aluminum oxide liquation flows back into die tip from mold center's through hole, stop or slowly vertically lift and adjust the radiation heat transfer condition between growth interface and coolship, and regulate the power of well heater, because the semisphere of mould designs, crystal constantly can be grown to central stabilizer by edge in this thermoregulator process, utilizing the continuous change of mould and crucible relative position, the liquid realized in mould hemisphere groove is flowed back in crucible lentamente by mold center hole; After crystal is completed to central growth by die edge, realize first half ball cover growth;
Step S5: regulate the gas flow of coolship and the power of calorifier, guarantee that mould extension has the liquation film of suitable thickness to exist, the relative position of adjustment hanging scaffold and crucible makes the passage emersion liquation of mold bottom, in relative movement by gas flow in controlled cooling model dish to control growth interface solution film thickness, guarantee that furnace pressure and mould inside liquation pressure reduction and capillary force balance, when protective gas flows into mould inside through mold bottom passage, after mould inner melt flows back to crucible, process of growth again in repeating step S4, until melt cannot be sewed on by annular capillary and rises to die tip in crucible,
Step S6: after crystal growth completes, suspension rod of slinging, mold removal, pulls down hanging scaffold.
5. sapphire crystal half ball cover EFG technique growth method according to claim 4, is characterized in that: described protective gas and cooling gas are Ar, CO and CO
2mixed gas.
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| CN106676625A (en) * | 2017-02-21 | 2017-05-17 | 洛阳金诺机械工程有限公司 | Blowing device for drawing silicon cores |
| RU2743354C1 (en) * | 2020-08-31 | 2021-02-17 | Федеральное государственное бюджетное учреждение науки Институт физики твердого тела Российской академии наук (ИФТТ РАН) | Method for producing end surfaces with curvature on sapphire single crystals |
| CN112501690A (en) * | 2020-12-02 | 2021-03-16 | 通辽精工蓝宝石有限公司 | Growth method of sapphire single crystal |
| CN112663140A (en) * | 2020-12-07 | 2021-04-16 | 山东大学 | Mold device for preparing quaternary halide crystal and preparation method |
| CN112795986A (en) * | 2020-12-31 | 2021-05-14 | 山东大学 | Single crystal growth device capable of regulating and controlling crystallization solid-liquid interface in real time and use method |
| CN113424082A (en) * | 2019-02-13 | 2021-09-21 | 京瓷株式会社 | Optical member, and image display device and head-up display using same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106676625A (en) * | 2017-02-21 | 2017-05-17 | 洛阳金诺机械工程有限公司 | Blowing device for drawing silicon cores |
| CN106676625B (en) * | 2017-02-21 | 2023-05-26 | 洛阳金诺机械工程有限公司 | Air blowing device for drawing silicon core |
| CN113424082A (en) * | 2019-02-13 | 2021-09-21 | 京瓷株式会社 | Optical member, and image display device and head-up display using same |
| CN113424082B (en) * | 2019-02-13 | 2024-02-23 | 京瓷株式会社 | Optical member, image display device using the same, and head-up display |
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| CN112501690A (en) * | 2020-12-02 | 2021-03-16 | 通辽精工蓝宝石有限公司 | Growth method of sapphire single crystal |
| CN112663140A (en) * | 2020-12-07 | 2021-04-16 | 山东大学 | Mold device for preparing quaternary halide crystal and preparation method |
| CN112795986A (en) * | 2020-12-31 | 2021-05-14 | 山东大学 | Single crystal growth device capable of regulating and controlling crystallization solid-liquid interface in real time and use method |
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