CN103160934B - Thermograde control device and method thereof when a kind of grown crystal material - Google Patents
Thermograde control device and method thereof when a kind of grown crystal material Download PDFInfo
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- CN103160934B CN103160934B CN201210020279.0A CN201210020279A CN103160934B CN 103160934 B CN103160934 B CN 103160934B CN 201210020279 A CN201210020279 A CN 201210020279A CN 103160934 B CN103160934 B CN 103160934B
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Abstract
Thermograde control device and method thereof when a kind of grown crystal material, relate to a kind of growth apparatus of crystalline material, in furnace chamber (1), be provided with crucible (5), the bottom of crucible, in sleeve (4), is provided with heater (3) in sleeve outside; Cooling medium cooling mechanism is arranged on the bottom in sleeve; Form the thermograde control at the bottom of the high temperature of lower of crucible upper temp by cooling medium cooling mechanism; The present invention is by the outside at crucible by jacket casing, first heater heats jacket casing, jacket casing is again to crucible heating, because the present invention is higher at the vertical shaft height of crucible bottom and sleeve bottom, and vertical shaft is also higher in the bottom level of sleeve, passing into after inert gas, the area of dissipation of described vertical shaft also obviously strengthens, make to form low-temperature space between the bottom in crucible bottom and sleeve, obtained preferably thermograde; Due to the effect of jacket casing, also can guarantee the non-homogeneous nucleus of the few appearance of crucible.
Description
[technical field]
The present invention relates to a kind of growth apparatus of crystalline material, specifically the present invention relates to a kind of growth blueHeating-up temperature gradient control device and method thereof when the crystalline materials such as jewel, polysilicon or monocrystalline silicon.
[background technology]
In the crystal material growth processes such as polysilicon, monocrystalline silicon or sapphire, wherein polysilicon particle existsWhen being grown to serve as polycrystal silicon ingot and polysilicon in crucible and being converted to monocrystalline silicon, by the hot temperature that adds to crucibleDegree is controlled, and utilizes and be arranged on the seed crystal of crucible bottom, make to melt and around the crystal of the new growth of seed crystal byCrystal grain arrangement mode according to seed crystal is arranged: when wherein seed crystal is monocrystalline, and the silicon atom of new grown crystalBe arranged in many nucleus with diamond lattice, these nucleus grow up to the crystal grain identical with seed crystal high preferred orientation,The crystal of new growth is exactly monocrystalline silicon; If when seed crystal is polycrystalline, these nucleus grow up to seed crystal crystal face to be gotTo different crystal grain, the crystal of new growth is exactly polysilicon; But this process must be close at oneIn the body of heater closing, complete.
In the process of new crystal growth, the crucible in furnace chamber need to form and bend down high thermograde,For formation temperature gradient, legacy equipment, by changing the bottom heat insulation effect of crucible, increases the loose of heatLose so as to form crucible required bend down high thermograde.
Also having technology is by pass into the cryogens such as liquid helium in lower shaft, is realized and is taken away earthenware by cryogenThe object of crucible bottom heat, thus the effect of the upper and lower temperature difference " thermograde " of crucible formed; With heatExchange process is example, and its growing method is:
A, first by the crystalline material particle in calandria heat fused crucible, particle melt temperature is protectedHold a little more than 5～10 DEG C of fusing points;
B, in the time that the seed crystal upper part of crucible bottom setting is melted, " at this moment crystalline material particle alsoThrough melting ", the temperature starting in slow decreasing furnace chamber " also makes the temperature of crucible reduce simultaneously, to meltThe crystalline material particle crystallization of changing ";
C, the lower shaft of crucible bottom in furnace chamber is injected to helium, the temperature transmission by lower shaft to crucible at the bottom ofPortion forces cooling, being crucible bottom and being arranged in crucible of perception low temperature first in this processThe seed crystal of bottom, low temperature can be along with seed crystal be to the crystalline material particle radiation of melting;
The crystalline material of D, thawing will, taking seed crystal as core, grow the crystalline substance that is full of whole crucible graduallyBody; This is the crystallization process of crystalline material.
Aforesaid way required important document in the time of growth comprises: the bottom of crucible must closely be connected with lower shaft, shapeBecome temperature conductor; Early stage, heat consumption was very big when heating crucible; Crucible in heating process due to anglesReason, make calandria inhomogeneous for the heating of crucible, make the easy shape of outer edge surface of crucible surroundingBecome partial distance hotter, other temperature with respect to hotter part is colder, under this environment, just canThere is non-homogeneous nucleus.
In like manner, sapphire processing method comprise czochralski method, Bridgman-Stockbarger method, guided mode method, heat-exchanging method,Kyropoulos etc., for the method for at present being prepared by sapphire, above preparation method adopts supporter rotationThe scheme that drives crucible synchronous rotary, the sapphire crystallization process in crucible is subject to microseism and makes crystallization processOccur that crystalline substance shakes phenomenon and forming section crystal dislocation, cause quality to decline. Even Growth by Temperature Gradient TechniqueSapphire, also there will be the deviation of crucible angles in heating process, makes calandria for crucibleHeating inhomogeneous, easily there is non-homogeneous nucleus in the sapphire that grows.
[summary of the invention]
In order to overcome the deficiency in background technology, the temperature while the invention discloses a kind of grown crystal materialGradient control device and method thereof, the present invention by by jacket casing the outside at crucible, crucible bottom withThe vertical shaft height of sleeve bottom is higher, and vertical shaft is also higher in the bottom level of sleeve, is passing into inertiaAfter gas, the area of dissipation of described vertical shaft also obviously strengthens, make bottom in crucible bottom and sleeve itBetween form low-temperature space, also form low-temperature space below the bottom of described sleeve; Further support that the present invention obtainsGet the demand of heating-up temperature gradient.
In order to realize the object of foregoing invention, the present invention adopts following technical scheme:
Thermograde control device when grown crystal material, comprise furnace chamber, heater, sleeve,Crucible and cooling medium cooling mechanism are provided with crucible in furnace chamber, the bottom of crucible in sleeve,Sleeve outside is provided with heater; Cooling medium cooling mechanism is arranged on the bottom in sleeve; By cooling mediumCooling mechanism forms the thermograde control at the bottom of the high temperature of lower of crucible upper temp.
Thermograde control device when described grown crystal material, described cooling medium cooling mechanism bagDraw together lower shaft, sleeve, in described lower shaft, be provided with cooling medium capable of circulation, cold in sleeve in described lower shaftBut medium forms the thermograde control of crucible, and the bottom of described crucible is connected with the upper end of lower shaft.
Thermograde control device when described grown crystal material is established in the outside furnace chamber of heaterThere is stay-warm case.
Thermograde control device when described grown crystal material, upper cartridge is provided with upwards extensionPoint, above the outside of the described crucible of inner side, upwards extension parcel of sleeve.
Thermograde control device when described grown crystal material, described lower shaft top is empty to lower endCore structure is provided with pipeline in the lower shaft of hollow-core construction, and the inside of described pipeline is cooling medium path,Cooling medium refluxes behind upper reaches in pipeline between pipeline and the hollow-core construction of lower shaft, forms crucibleBottom cooling structure; Or outside between described pipeline and the hollow-core construction of lower shaft is that cooling medium is logicalRoad, cooling medium refluxes behind upper reaches outside pipeline and between the hollow-core construction of lower shaft in pipeline, shapeBecome the bottom of crucible another replacing structure of lowering the temperature.
Thermograde control device when described grown crystal material, outside the junction of crucible and lower shaftEdge face is provided with crucible fixed cover, is formed the anti-structure that slants of crucible by crucible fixed cover; Or lower shaft is upperEnd arranges the depression that corresponding crucible bottom is protruded downwards, by the anti-structure that slants that is recessed to form crucible.
Thermograde control device when described grown crystal material, the bottom faces of sleeve is provided with fixingHole, described fixing hole is enclosed within the top of lower shaft.
Thermograde control device when described grown crystal material is provided with on the lower shaft of lower cartridgeSleeve fixed cover, the fixing hole place of described sleeve is placed on sleeve fixed cover top.
Thermograde control device when described grown crystal material, the exterior face of described sleeve and crucibleBetween be provided with the medial surface of gap or sleeve and the exterior face of crucible for to be closely connected.
Thermograde control device when described grown crystal material, between sleeve and the top of crucibleIn gap, be placed with bezel ring,, form the support of sleeve to crucible by described bezel ring.
Thermograde control device when described grown crystal material, the inner side suitable for reading of described sleeve is provided withStep, bezel ring, outer rim is placed on described step, is formed the anti-slip structure of bezel ring, by step.
Thermograde control device when described grown crystal material, on the exterior face of the middle part of sleeve betweenEvery being provided with multiple inside and outside openings that connect, form heater by opening the part of crucible is directly heated.
Thermograde control device when described grown crystal material, the top of described sleeve is to suitable for reading establishingThere is top necking down.
Thermograde control device when described grown crystal material, the bottom of described sleeve is set to put downFace.
Thermograde control device when described grown crystal material, under the bottom of described sleeve is provided withThe additional cylinder of portion, a cooling medium that forms lower shaft bottom by the additional cylinder in the bottom low-temperature space non-proliferation forming of lowering the temperatureStructure.
Thermograde control device when described grown crystal material, between lower cartridge and base planeLinkage section be arc-shaped transition.
Thermograde control device when described grown crystal material, lower cartridge and base plane are for fallingTaper surface transition.
Thermograde control device when described grown crystal material, establish the bottom of described sleeve to bottomBe set to arc-shaped transition.
Thermograde control device when described grown crystal material, the bottom of described sleeve be set toA few necking segment.
Thermograde control device when described grown crystal material, sleeve is set to long tubular construction,In the sleeve of the lower shaft of crucible and bottom in long tubular construction.
Thermograde control device when described grown crystal material, described sleeve is set to the cylinder lengtheningShape structure, is provided with bearing plate at the interior middle part of tubular construction sleeve, and the middle part of described bearing plate is provided with cruciblePutting hole is provided with multiple cooling medium pod apertures on the bearing plate around crucible putting hole, under sleeve is interiorThe furnace chamber of portion is provided with at least one inert gas hand-hole, forms cooling medium by inert gas hand-holeAnother replacing structure of cooling mechanism, is formed the thermograde control of crucible bottom by cooling medium cooling mechanismSystem.
Thermograde control device when described grown crystal material, described sleeve is tungsten or molybdenum or graphiteAny one in material; Or tungsten and molybdenum combination; Or molybdenum and graphite combination; Or tungsten and graphite are combined to formTwo-layer composite bed; Or three layers of composite bed of tungsten and molybdenum and graphite composition; Or inside and outside be that molybdenum layer middle part is tungsten layer;Or inside and outside be that tungsten layer middle part is molybdenum layer; Or inside and outside be that graphite linings middle part is tungsten layer; Or inside and outside be tungsten layer middle partFor graphite linings; Or inside and outside be that graphite linings middle part is molybdenum layer; Or inside and outside be that molybdenum layer middle part is graphite linings formation threeLayer composite bed.
Thermograde control device when described grown crystal material, at tungsten described in the composite bed of sleeveIn layer and molybdenum layer and graphite linings, add zirconia layer or alumina layer; Or arbitrary in tungsten or molybdenum or graphite materialOr wherein two replace with zirconia or aluminium oxide.
Thermograde control device when described grown crystal material, the section of described bezel ring, is square sectionFace.
Thermograde control device when described grown crystal material, in the outer edge surface bottom of described bezel ring,Be provided with the lower necking down in outside.
Thermograde control device when described grown crystal material, the medial surface of described bezel ring, and outer rimBasifacial is respectively equipped with and expands warp and necking down, forms " protruding " tee section structure.
Thermograde control device when described grown crystal material, establish the medial surface bottom of described bezel ring,There is the lower neck that expands in inner side.
Thermograde control device when described grown crystal material is provided with ripple on the medial surface of bezel ring,Shape wave face or the annular flank of tooth or inwardly casting lug thereon.
Thermograde control device when described grown crystal material, in arranging on bezel ring, medial surfaceCasting lug thereon is at least two.
Thermograde control device when described grown crystal material is provided with multiple in the upper side of bezel ring,Several perforation to the hole of bezel ring, bottom surfaces.
Thermograde control device when described grown crystal material, described inert gas is helium, neonAny one in gas, argon gas, Krypton, xenon, nitrogen, freon or radon gas.
Thermograde control method when grown crystal material, in furnace chamber, crucible is arranged on lower shaftUpper end, the bottom in crucible is provided with seed crystal, places crystal crushed aggregate on seed crystal, by crucible in cylinderIn the nigger of shape structure, the outside of the nigger of described tubular construction is provided with heater, describedHot body connects respectively the both positive and negative polarity of power supply, the nigger radiation heating of heater to tubular construction, tubularHeat is evenly passed to crucible by the nigger of structure, passes into cooling medium, institute in described lower shaft simultaneouslyState lower shaft surrounding and form low-temperature space; At this moment the crystal crushed aggregate in crucible melts, when the crystal in described crucibleWhen particle all melts, the upper end head of described seed crystal also beginning melts, due to cooling Jie in lower shaftThe effect of matter, seed crystal melts the thawing that is obviously later than crystal crushed aggregate; Then reduce jacket temperature, low temperatureThe low temperature in district passes to crucible, makes described crucible start the slow uniform decrease in temperature to top by bottom, forms temperatureDegree gradient, the crystalline material melting in crucible starts by seed crystal place, bottom the crystallization of growing, and obtains crystalline materialPiece.
Thermograde control method when grown crystal material, in furnace chamber, crucible is arranged on lower shaftUpper end, the bottom in crucible is provided with seed crystal, places crystal crushed aggregate on seed crystal, by crucible in coverIn cylinder, the fixing hole of lower cartridge is enclosed within the middle part of lower shaft, and the outside of described sleeve is provided with heater, instituteState the both positive and negative polarity that heater connects respectively power supply, heater is to sleeve radiation heating, and sleeve is even by heatPass to crucible, pass into cooling medium simultaneously in described lower shaft, described lower shaft surrounding forms low-temperature space; ThisTime crystal crushed aggregate in crucible melt, in the time that the crystal crushed aggregate in described crucible all melts, described seed crystalUpper end head also melt beginning, due to the effect of cooling medium in lower shaft, seed crystal melts obviously eveningIn the thawing of crystal crushed aggregate, then reduce jacket temperature, the lower shaft surrounding that described sleeve inner is divided formsLow-temperature space, the low temperature of low-temperature space passes to crucible, described crucible is started slowly even to top by bottomCooling, formation temperature gradient, the crystalline material melting in crucible starts by seed crystal place, bottom the crystallization of growing,Obtain crystalline material piece.
Thermograde control method when described grown crystal material, is provided with bottom in the bottom of sleeve attachedAdd cylinder, the cooling medium that enters lower shaft in lower shaft surrounding formation low-temperature space, is overlapping in described sleeveThe lower shaft surrounding of the bottom of cylinder also forms low-temperature space simultaneously, and add cylinder by bottom low temperature is assembled, described inThe low temperature of assembling forms the cooling of auxiliary socket bottom, and the low temperature of described gathering has been guaranteed other ground in furnace chamberThe least possible heat in side runs off.
Thermograde control method when grown crystal material, in furnace chamber, crucible is arranged on sleeve and holdsOn the crucible putting hole of heavy plate, the bottom in crucible is provided with seed crystal, and in crucible, seed crystal place is exposed at sleeveBearing plate bottom, on described seed crystal, place crystal crushed aggregate, the outside of described sleeve is provided with heater,Described heater connects respectively the both positive and negative polarity of power supply, and heater is to sleeve radiation heating, and sleeve is equal by heatThe even crucible that passes to, simultaneously by the inert gas hand-hole that is arranged on the furnace chamber described in bottom in sleeve, willInert gas is filled with sleeve, and then inert gas enters via the multiple cooling medium pod apertures on bearing plateSleeve, makes crucible bottom temperature lower than top; At this moment the crystal crushed aggregate in crucible melts, when described crucibleWhen interior crystal crushed aggregate all melts, the upper end head of described seed crystal also beginning melts, and is subject to inertiaThe effect of gas, the seed crystal of crucible bottom melts the thawing speed that is obviously later than crystal crushed aggregate, then reducesJacket temperature, makes to benefit from first seed crystal in the crucible of inert gas cooling, force described crucible byBottom starts to top slow uniform decrease in temperature, formation temperature gradient, and the crystalline material melting in crucible is the end of bySeed crystal place of portion starts the crystallization of growing, and obtains crystalline material piece.
Thermograde control method when described grown crystal material, described crystal crushed aggregate is crystal powderEnd, crystal chunk or crystal grain.
By above-mentioned disclosure, the invention has the beneficial effects as follows:
Thermograde control device and method thereof when grown crystal material of the present invention, by by sleeveBe enclosed within the outside of crucible, first heater heats jacket casing, and jacket casing is again to crucible heating, because the present invention existsThe vertical shaft height of crucible bottom and sleeve bottom is higher, and vertical shaft is also higher in the bottom level of sleeve,Passing into after inert gas, the area of dissipation of described vertical shaft also obviously strengthens, and makes crucible bottom and sleeveIn bottom between form low-temperature space, also form low-temperature space below the bottom of described sleeve, sleeve bottomFurther cooling among a small circle in auxiliary socket of low-temperature space; So not only minimized take away sleeve at the bottom ofThe heat at the periphery place of portion, makes heat that the present invention takes away be significantly less than the crucible of prior art complete aroundThe loss of portion's heat, due to heat run off less, in having reduced use cost, the present invention also obtainsGet preferably thermograde, further supported the present invention to obtain the demand of heating-up temperature gradient; ThisInvention, by the independent action of jacket casing and bezel ring, or jacket casing, can not slant crucible, further crucible fourObtain in week and add comparatively uniformly thermal temperature field; Due to the effect of jacket casing, also can guarantee that the few appearance of crucible is non-allUniform grain core.
[brief description of the drawings]
Fig. 1 is structural representation of the present invention;
Fig. 2 is that crucible of the present invention and sleeve upper oral part add bezel ring, structural representation;
Fig. 3 is the lower curved transition structure schematic diagram of sleeve of the present invention;
Fig. 4 is that the upper oral part inner side of sleeve of the present invention arranges step example structure schematic diagram;
Fig. 5 is that the middle part of sleeve of the present invention arranges opening and comprises the lower curved transition embodiment of bottomStructural representation;
Fig. 6 is the bottom back taper face transition example structure schematic diagram of sleeve of the present invention;
Fig. 7 is that the bottom of sleeve of the present invention arranges a necking segment example structure schematic diagram;
Fig. 8 is that the bottom of sleeve of the present invention arranges multiple necking segment example structure schematic diagrames;
Fig. 9 is top necking down, the lower curved transition example structure schematic diagram of crucible of the present invention;
Figure 10 is bezel ring, square cross schematic diagram of the present invention;
Figure 11 is the lower necking down example structure schematic diagram in bezel ring, of the present invention outside;
Figure 12 is " protruding " tee section example structure schematic diagram of bezel ring, of the present invention;
Figure 13 is the lower neck example structure schematic diagram that expands in bezel ring, of the present invention inner side;
Figure 14 is the example structure schematic diagram that bezel ring, inside face of the present invention arranges waveform face;
Figure 15 is the example structure schematic diagram that bezel ring, of the present invention arranges up/down perforation hole;
Figure 16 is outer molybdenum layer middle part, the two sides of sleeve of the present invention tungsten layer structural representation;
Figure 17 is that tungsten layer two sides, the middle part skin of sleeve of the present invention arranges respectively graphite linings, molybdenum layer embodimentStructural representation;
Figure 18 is the structural representation that tungsten layer two sides, the middle part skin of sleeve of the present invention arranges respectively graphite linings;
Figure 19 is the structural representation that graphite linings two sides, the middle part skin of sleeve of the present invention arranges respectively tungsten layer;
Figure 20 is the structure that molybdenum layer two sides, the middle part skin of sleeve of the present invention arranges respectively tungsten layer, graphite liningsSchematic diagram;
Figure 21 is the structure that graphite linings two sides, the middle part skin of sleeve of the present invention arranges respectively tungsten layer, molybdenum layerSchematic diagram;
Figure 22 is a tungsten layer another side molybdenum layer structural representation of sleeve of the present invention;
Figure 23 is a molybdenum layer another side tungsten layer structural representation of sleeve of the present invention;
Figure 24 is a tungsten layer another side graphite linings structural representation of sleeve of the present invention;
Figure 25 is the structural representation that lower cartridge of the present invention arranges the additional cylinder in bottom;
Figure 26 arranges cooling medium pod apertures structural representation on 25 bearing plate;
Figure 27 is the structural representation at the bottom of sleeve of the present invention does not arrange tin;
In the drawings: 1, furnace chamber; 2, stay-warm case; 3, heater; 4, sleeve; 5, crucible; 6, crystalline substanceBody material; 7, seed crystal; 8, crucible fixed cover; 9, lower shaft; 10, sleeve fixed cover; 11, pipeline;12, cooling medium path; 13, bezel ring; 14, fixing hole; 15, necking segment; 16, top necking down;17, arc-shaped transition; 18, square-section; 19, necking down under outside; 20, under inner side, expand neck; 21, platformRank; 22, back taper face; 23, tungsten layer; 24, molybdenum layer; 25, graphite linings; 26, " protruding " shape is cutFace; 27, opening; 28, waveform face; 29, hole; 30, the additional cylinder in bottom; 31, crucible putting hole;32, cooling medium pod apertures; 33, bearing plate.
[detailed description of the invention]
Below in conjunction with embodiment, the present invention is further detailed; The following examples be not forRestriction of the present invention, only realizes mode of the present invention as supporting, at technological frame disclosed in this inventionInterior any equivalent structure is replaced, and is protection scope of the present invention;
Thermograde control device when a kind of grown crystal material described in 1,2 by reference to the accompanying drawings, bagDraw together furnace chamber 1, heater 3, sleeve 4, crucible 5 and cooling medium cooling mechanism, in furnace chamber 1, be provided withCrucible 5, the bottom of crucible 5 is in sleeve 4, and sleeve 4 tops are provided with upwards extension, sleeveThe outside upper part of 4 the described crucible 5 of inner side, upwards extension parcel, cover described in 2 by reference to the accompanying drawingsBetween cylinder 4 and the exterior face of crucible 5, be provided with the medial surface of gap or sleeve 4 and the exterior face of crucible 5 isClosely connect; Be provided with heater 3 in sleeve 4 outsides, in the outside furnace chamber 1 of heater 3, be provided with guarantorTemperature cover 2, it should be noted that: add man-hour at single crucible 5, the tool of furnace chamber 1 own as the present invention usesThere is heat insulation function, add man-hour if use at multiple crucibles 5 simultaneously, just need to use stay-warm case 2 to eachCrucible 5 is incubated; Cooling medium cooling mechanism is arranged on the bottom in sleeve 4; Fallen by cooling mediumTemperature mechanism forms the thermograde control at the bottom of the high temperature of lower of crucible 5 upper temp.
Between sleeve 4 and the top of crucible 5, in gap, be placed with bezel ring, 13, by described bezel ring, 13 shapesBecome the support of sleeve 4 to crucible 5; 4 in order to place described bezel ring, 13 by reference to the accompanying drawings, sleeve 4 suitable for readingInner side is provided with step 21, and bezel ring, 13 outer rims are placed on described step 21, form bezel ring, by step 2113 anti-slip structure; 5 the present invention are interval with multiple on the exterior face of the middle part of sleeve 4 by reference to the accompanying drawingsThe inside and outside opening 27 connecting, forms heater 3 by opening 27 part of crucible is directly heated; In conjunction withDescribed in accompanying drawing 9, the top of sleeve 4 is provided with top necking down 16 to suitable for reading, is formed by described top necking down 16To the support of crucible; 3～9 because the variation of described sleeve 4 is more by reference to the accompanying drawings, provides several belowVersion, but following variation is not for restriction of the present invention, and the bottom of described sleeve 4 is set toPlane; Be provided with the additional cylinder 30 in bottom in the bottom of described sleeve 4, form lower shaft by the additional cylinder 30 in bottomThe low-temperature space non-proliferation structure that the cooling medium cooling of 9 bottoms forms; Sleeve 4 bottoms and base plane itBetween linkage section be arc-shaped transition 17; Sleeve 4 bottoms and base plane are 22 transition of back taper face; InstituteBottom to the bottom of stating sleeve 4 is set to arc-shaped transition 17; Or the bottom of described sleeve 4 is set at leastA necking segment 15.
Described cooling medium cooling mechanism is divided into two kinds of cooling forms, and wherein the first is specially described coolingMedium cooling mechanism comprises lower shaft 9, sleeve 4, in described lower shaft 9, is provided with cooling medium capable of circulation,Cooling medium in the interior described lower shaft 9 of sleeve 4 forms the thermograde control of crucible 5, described crucible 5Bottom be connected with the upper end of lower shaft 9; By reference to the accompanying drawings 3～9 or the bottom faces of accompanying drawing 25 sleeves 4 on establishHave fixing hole 14, described fixing hole 14 is enclosed within the top of lower shaft 9; Described lower shaft 9 tops to lower end areHollow-core construction is provided with pipeline 11 in the lower shaft 9 of hollow-core construction, and the inside of described pipeline 11 is coolingMedium channel 12, pipeline 11 connects cooling medium, cooling medium behind the interior upper reaches of pipeline 11 along pipeBetween the hollow-core construction of road 11 and lower shaft 9, reflux, form the bottom cooling structure of crucible 5; Or described inOutside between the hollow-core construction of pipeline 11 and lower shaft 9 is cooling medium path 12, cooling medium alongBetween the outer hollow-core construction with lower shaft 9 of pipeline 11 behind upper reaches along the interior backflow of pipeline 11, formation crucible 5Bottom another replacing structure of lowering the temperature; On the junction outer edge surface of crucible 5 and lower shaft 9, be provided with crucible solidSurely overlap 8, formed the anti-structure that slants of crucible by crucible fixed cover 8; Or the upper end of lower shaft 9 arranges correspondenceThe depression that crucible bottom is protruded downwards, by the anti-structure that slants that is recessed to form crucible;
On the lower shaft 9 of sleeve 4 bottoms, be provided with sleeve fixed cover 10, the fixing hole 14 of described sleeve 4Place is placed on sleeve fixed cover 10 tops; Certainly support that the structure of this method can also be at lower shaft 9Sleeve fixed cover 10 positions convex hole is set, in the time that convex hole is set, just that sleeve is set is solid with the present inventionSurely overlap 10 formation and be equal to replacing structure.
27 the present invention consider that lower shaft 9 is directly connected with crucible 5 and has omitted sleeve 4 by reference to the accompanying drawingsThe cylinder end, can realize equally, so sleeve 4 is set to long tubular construction, the cylinder end of sleeve 4 is supported on stoveIn 1 bottom faces of chamber, in the sleeve 4 of the lower shaft 9 of crucible 5 and bottom in long tubular construction.
By reference to the accompanying drawings 26, described sleeve 4 is set to the tubular construction lengthening, at tubular construction sleeve 4Interior middle part be provided with bearing plate 33, the middle part of described bearing plate 33 is provided with crucible putting hole 31, crucible is putOn crucible putting hole 31, on the bearing plate 33 around crucible putting hole 31, be provided with multiple cooling JieMatter pod apertures 32, the furnace chamber 1 of sleeve 4 interior bottoms is provided with at least one inert gas hand-hole, by lazyProperty gas injection hole form another replacing structure of cooling medium cooling mechanism, by cooling medium cooling mechanismForm the thermograde control of crucible 5 bottoms; Described inert gas be helium, neon, argon gas, Krypton,Any one in xenon, nitrogen, freon or radon gas.
The material that described in 16～24, sleeve 4 uses by reference to the accompanying drawings in tungsten or molybdenum or graphite material arbitrarilyA kind of; Or tungsten and molybdenum combination; Or molybdenum and graphite combination; Or tungsten and graphite are combined to form two-layer composite bed;Or three layers of composite bed of tungsten and molybdenum and graphite composition; Or inside and outside be that molybdenum layer middle part is tungsten layer; Or inside and outside be tungstenLayer middle part is molybdenum layer; Or inside and outside be that graphite linings middle part is tungsten layer; Or inside and outside be that tungsten layer middle part is graphite linings;Or inside and outside be that graphite linings middle part is molybdenum layer; Or inside and outside be that molybdenum layer middle part is three layers of composite bed of graphite linings formation;In tungsten layer and molybdenum layer and graphite linings described in the composite bed of sleeve 4, add zirconia layer or alumina layer;In tungsten or molybdenum or graphite material arbitrary or wherein two replace with zirconia or aluminium oxide; For sleeve 4The material the present invention who uses has provided above several preferably matching structures, due to taking of above several materialsFormula formula is too much, and therefore the present invention does not give to describe in detail one by one, and the random variation that comprises above-mentioned material is allProtection scope of the present invention.
The structure providing in 10～15 by reference to the accompanying drawings, the present invention provides the distressed structure of several bezel ring,s 13:The section of described bezel ring, 13 is square-section 18; Be provided with under outside in the outer edge surface bottom of described bezel ring, 13Necking down 19; The medial surface of described bezel ring, 13 and outer edge surface bottom are respectively equipped with expands warp and necking down, forms and" protruding " tee section 26 structures; The medial surface bottom of described bezel ring, 13 is provided with the lower neck 20 that expands in inner side; At lidThe medial surface of ring 13 is provided with waveform face 28 or the annular flank of tooth or inside casting lug thereon; In bezel ring, 13Projecting inward that on side, arranges is at least two; In the upper side of bezel ring, 13, be provided with a plurality of perforationsTo the hole 29 of bezel ring, 13 bottom surfaces.
Provide following preferred embodiment in conjunction with institute's drawings attached:
Implement one:
Thermograde control method when grown crystal material, under the interior crucible 5 of furnace chamber 1 is arranged onThe upper end of axle 9, the bottom in crucible 5 is provided with seed crystal 7, places crystal crushed aggregate 6 on seed crystal 7,Described crystal crushed aggregate 6 is crystal powder, crystal chunk or crystal grain, by crucible 5 in tubular constructionNigger 4 in, the outside of the nigger 4 of described tubular construction is provided with heater 3, describedHot body 3 connects respectively the both positive and negative polarity of power supply, nigger 4 radiation heatings of heater 3 to tubular construction,Heat is evenly passed to crucible 5 by the nigger 4 of tubular construction, passes into cold in described lower shaft 9 simultaneouslyBut medium, described lower shaft 9 surroundings form low-temperature space; At this moment the crystal crushed aggregate 6 in crucible 5 melts, whenWhen crystal crushed aggregate 6 in described crucible 5 all melts, the also beginning of upper end head of described seed crystal 7Melt, due to the effect of lower shaft 9 interior cooling mediums, seed crystal 7 melts and is obviously later than melting of crystal crushed aggregate 6Change; Then reduce jacket temperature, the low temperature of low-temperature space passes to crucible 5, makes described crucible 5 end of byPortion starts the slow uniform decrease in temperature to top, formation temperature gradient, and the crystalline material of crucible 5 interior thawings is the end of byPortion's seed crystal 7 places start the crystallization of growing, and obtain crystalline material piece.
Implement two:
Thermograde control method when grown crystal material, under the interior crucible 5 of furnace chamber 1 is arranged onThe upper end of axle 9, the bottom in crucible 5 is provided with seed crystal 7, places crystal crushed aggregate 6 on seed crystal 7,Described crystal crushed aggregate 6 is crystal powder, crystal chunk or crystal grain, by crucible 5 in sleeve 4,The fixing hole 14 of sleeve 4 bottoms is enclosed within the middle part of lower shaft 9, and the outside of described sleeve 4 is provided with heater 3,Described heater 3 connects respectively the both positive and negative polarity of power supply, and heater 3 is to sleeve 4 radiation heatings, sleeve 4Heat is evenly passed to crucible 5, in described lower shaft 9, pass into cooling medium, described lower shaft 9 four simultaneouslyWeek forms low-temperature space; At this moment the crystal crushed aggregate 6 in crucible 5 melts, when the crystal in described crucible 5 brokenWhen material 6 all melts, the upper end head of described seed crystal 7 also beginning melts, because lower shaft 9 is interior coldBut the effect of medium, seed crystal 7 melts the thawing that is obviously later than crystal crushed aggregate 6, then reduces heating jacket temperatureDegree, lower shaft 9 surroundings of described sleeve 4 interior parts form low-temperature space, and the low temperature of low-temperature space passes to crucible5, make described crucible 5 start the slow uniform decrease in temperature to top, formation temperature gradient, crucible 5 by bottomThe crystalline material of interior thawing starts by bottom seed crystal 7 places the crystallization of growing, and obtains crystalline material piece.
Thermograde control method when described grown crystal material, is provided with bottom in the bottom of sleeve 4Additional cylinder 30, the cooling medium that enters lower shaft 9 forms low-temperature spaces in interior lower shaft 9 surroundings of described sleeve 4Meanwhile, also form low-temperature space simultaneously in lower shaft 9 surroundings of the bottom of sleeve 4, add tins 30 by bottomLow temperature is assembled, and the low temperature of described gathering forms the cooling of auxiliary socket 4 bottoms, the low temperature of described gatheringGuarantee that in furnace chamber 1, other local the least possible heat runs off.
Implement three:
Thermograde control method when grown crystal material, is arranged on cover at the interior crucible 5 of furnace chamber 1On the crucible putting hole 31 of cylinder 4 bearing plates 33, the bottom in crucible 5 is provided with seed crystal 7, crucible 5Interior seed crystal 7 places are exposed places crystal crushed aggregate 6 in bearing plate 33 bottoms of sleeve 4 on described seed crystal 7,Described crystal crushed aggregate 6 is crystal powder, crystal chunk or crystal grain, and the outside of described sleeve 4 is provided withHeater 3, described heater 3 connects respectively the both positive and negative polarity of power supply, and to sleeve, 4 radiation add heater 3Heat, heat is evenly passed to crucible 5 by sleeve 4, simultaneously by the stove being arranged on described in the interior bottom of sleeve 4The inert gas hand-hole of chamber 1, is filled with sleeve 4 by inert gas, and then inert gas is via bearing plateMultiple cooling medium pod apertures 32 on 33 enter sleeve 4, make crucible 5 bottom temps lower than top;At this moment the crystal crushed aggregate 6 in crucible 5 melts, in the time that the crystal crushed aggregate 6 in described crucible 5 all melts,The upper end head of described seed crystal 7 also beginning melts, and is subject to the effect of inert gas, crucible 5 bottomsSeed crystal 7 melt the thawing speed that is obviously later than crystal crushed aggregate 6, then reduce jacket temperature, makeFirst benefit from seed crystal 7 in the crucible 5 of inert gas cooling, force described crucible 5 to be started extremely by bottomThe slow uniform decrease in temperature in top, formation temperature gradient, the crystalline material of crucible 5 interior thawings is by bottom seed crystal 7Place starts the crystallization of growing, and obtains crystalline material piece.
Part not in the detailed description of the invention is prior art.
For open object of the present invention and the embodiment selecting in this article, current think suitable,But, will be appreciated that, the present invention is intended to comprise that all belong to the embodiment in this design and invention scopeAll changes and improvement.
Claims (35)
1. thermograde control device when grown crystal material, comprises furnace chamber (1), heater(3), sleeve (4), crucible (5) and cooling medium cooling mechanism, it is characterized in that: in furnace chamber (1)Inside be provided with crucible (5), the bottom of crucible (5) in sleeve (4), the bottom faces of sleeve (4)Be provided with fixing hole (14), described fixing hole (14) is enclosed within the top of lower shaft (9), in sleeve (4)Outside is provided with heater (3); Cooling medium cooling mechanism is arranged on the bottom in sleeve (4); By coldBut the thermograde control at the bottom of the high temperature of lower of medium cooling mechanism formation crucible (5) upper temp.
2. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: described cooling medium cooling mechanism comprises lower shaft (9), sleeve (4), in described lower shaft (9)Be provided with cooling medium capable of circulation, the cooling medium in sleeve (4) in described lower shaft (9) forms crucible(5) thermograde control, the bottom of described crucible (5) is connected with the upper end of lower shaft (9).
3. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: in the outside furnace chamber (1) of heater (3), be provided with stay-warm case (2).
4. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: sleeve (4) top is provided with upwards extension, inner side, the upwards extension bag of sleeve (4)Wrap up in above the outside of described crucible (5).
5. thermograde control device when grown crystal material according to claim 2, its spyLevy and be: described lower shaft (9) top is hollow-core construction to lower end, in the lower shaft (9) of hollow-core construction, establishHave pipeline (11), the inside of described pipeline (11) is cooling medium path (12), cooling medium alongBehind the interior upper reaches of pipeline (11), between pipeline (11) and the hollow-core construction of lower shaft (9), reflux, shapeBecome the bottom cooling structure of crucible (5); Or the hollow-core construction of described pipeline (11) and lower shaft (9) itBetween outside be cooling medium path (12), cooling medium outside pipeline (11) with lower shaft (9)Between hollow-core construction, behind upper reaches, in pipeline (11), reflux, the bottom cooling that forms crucible (5) is anotherOne replacing structure.
6. thermograde control device when grown crystal material according to claim 2, its spyLevy and be: on the junction outer edge surface of crucible (5) and lower shaft (9), be provided with crucible fixed cover (8), byCrucible fixed cover (8) forms the anti-structure that slants of crucible; Or the upper end of lower shaft (9) arranges corresponding crucibleThe depression that protrude downwards bottom, by the anti-structure that slants that is recessed to form crucible.
7. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: on the lower shaft (9) of sleeve (4) bottom, be provided with sleeve fixed cover (10), described sleeve (4)Fixing hole (14) locate to be placed on sleeve fixed cover (10) top.
8. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: between described sleeve (4) and the exterior face of crucible (5), be provided with gap or sleeve (4) inSide with the exterior face of crucible (5) for to be closely connected.
9. thermograde control device when grown crystal material according to claim 1, its spyLevy and be: between sleeve (4) and the top of crucible (5), in gap, be placed with bezel ring, (13), by instituteState bezel ring, (13) and form the support of sleeve (4) to crucible (5).
10. the thermograde control device during according to grown crystal material described in claim 1 or 8,It is characterized in that: the inner side suitable for reading of described sleeve (4) is provided with step (21), bezel ring, (13) outer rim is placedAt described step (21) above, formed the anti-slip structure of bezel ring, (13) by step (21).
11. thermograde control device during according to grown crystal material described in claim 1 or 8,It is characterized in that: on the middle part exterior face of sleeve (4), be interval with multiple inside and outside openings (27) that connect,Forming heater (3) by opening (27) directly heats the part of crucible.
12. temperature ladders during according to grown crystal material described in the arbitrary claim of claim 7 or 8Degree control device, is characterized in that: the top of described sleeve (4) is provided with top necking down (16) to suitable for reading.
Thermograde control device when 13. grown crystal material according to claim 12, itsFeature is: the bottom of described sleeve (4) is set to plane.
Thermograde control device when 14. grown crystal material according to claim 12, itsFeature is: be provided with the additional cylinder in bottom (30) in the bottom of described sleeve (4), by the additional cylinder in bottom (30)Form the low-temperature space non-proliferation structure of the cooling medium cooling formation of lower shaft (9) bottom.
Thermograde control device when 15. grown crystal material according to claim 12, itsFeature is: the linkage section between sleeve (4) bottom and base plane is arc-shaped transition (17).
Thermograde control device when 16. grown crystal material according to claim 13, itsFeature is: sleeve (4) bottom and base plane are back taper face (22) transition.
17. temperature ladders during according to grown crystal material described in the arbitrary claim of claim 7 or 8Degree control device, is characterized in that: bottom to the bottom of described sleeve (4) is set to arc-shaped transition (17).
Thermograde control device when 18. grown crystal material according to claim 13, itsFeature is: the bottom of described sleeve (4) is set at least one necking segment (15).
Thermograde control device when 19. grown crystal material according to claim 1, its spyLevy and be: sleeve (4) is set to long tubular construction, the lower shaft (9) of crucible (5) and bottom inIn the sleeve (4) of long tubular construction.
Thermograde control device when 20. grown crystal material according to claim 1, its spyLevy and be: described sleeve (4) is set to the tubular construction lengthening, in tubular construction sleeve (4) interiorPortion is provided with bearing plate (33), and the middle part of described bearing plate (33) is provided with crucible putting hole (31), at earthenwareCrucible putting hole (31) bearing plate (33) is around provided with multiple cooling medium pod apertures (32), coverThe furnace chamber (1) of cylinder (4) interior bottom is provided with at least one inert gas hand-hole, is noted by inert gasHand-hole forms another replacing structure of cooling medium cooling mechanism, forms crucible by cooling medium cooling mechanism(5) the thermograde control of bottom.
21. according to claim 1,2,4,7,8,13,14,15,16,18,19 or 20Thermograde control device when grown crystal material described in one claim, is characterized in that: described coverCylinder (4) is any one in tungsten or molybdenum or graphite material; Or tungsten and molybdenum combination; Or molybdenum and graphite groupClose; Or tungsten and graphite are combined to form two-layer composite bed; Or three layers of composite bed of tungsten and molybdenum and graphite composition;Or inside and outside be that molybdenum layer middle part is tungsten layer; Or inside and outside be that tungsten layer middle part is molybdenum layer; Or inside and outside be graphite linings middle partFor tungsten layer; Or inside and outside be that tungsten layer middle part is graphite linings; Or inside and outside be that graphite linings middle part is molybdenum layer; Or inside and outsideFor molybdenum layer middle part is three layers of composite bed of graphite linings formation.
Thermograde control device when 22. grown crystal material according to claim 21, itsFeature is: adding zirconia layer in tungsten layer and molybdenum layer and graphite linings described in the composite bed of sleeve (4)Or alumina layer; In tungsten or molybdenum or graphite material arbitrary or wherein two replace with zirconia or oxidationAluminium.
Thermograde control device when 23. grown crystal material according to claim 9, its spyLevy and be: the section of described bezel ring, (13) is square-section (18).
Thermograde control device when 24. grown crystal material according to claim 9, its spyLevy and be: be provided with necking down (19) under outside in the outer edge surface bottom of described bezel ring, (13).
Thermograde control device when 25. grown crystal material according to claim 9, its spyLevy and be: the medial surface of described bezel ring, (13) and outer edge surface bottom are respectively equipped with expands warp and necking down, forms and" protruding " tee section (26) structure.
Thermograde control device when 26. grown crystal material according to claim 9, its spyLevy and be: the medial surface bottom of described bezel ring, (13) is provided with the lower neck (20) that expands in inner side.
Thermograde control device when 27. grown crystal material according to claim 9, its spyLevy and be: on the medial surface of bezel ring, (13), be provided with waveform face (28) or the annular flank of tooth or to projecting inwardPiece.
Thermograde control device when 28. grown crystal material according to claim 9, its spyLevy and be: projecting inward that on bezel ring, (13) medial surface, arranges is at least two.
Thermograde control device when 29. grown crystal material according to claim 9, its spyLevy and be: in the upper side of bezel ring, (13), be provided with a plurality of perforation to the hole (29) of bezel ring, (13) bottom surfaces.
Thermograde control device when 30. grown crystal material according to claim 20, itsFeature is: described inert gas is in helium, neon, argon gas, Krypton, xenon, nitrogen or radon gasAny one.
31. temperature ladders while implementing the claims 20～22 and 30 arbitrary described grown crystal materialDegree control device a kind of grown crystal material time thermograde control method, it is characterized in that: at stoveThe interior crucible in chamber (1) (5) is arranged on the upper end of lower shaft (9), and the bottom in crucible (5) arrangesThere is seed crystal (7), at the upper crystal crushed aggregate (6) of placing of seed crystal (7), crucible (5) is tied in tubularIn the nigger (4) of structure, the outside of the nigger (4) of described tubular construction is provided with heater(3), described heater (3) connects respectively the both positive and negative polarity of power supply, and heater (3) is to tubular constructionNigger (4) radiation heating, the nigger (4) of tubular construction evenly passes to heatCrucible (5) passes into cooling medium in described lower shaft (9) simultaneously, and described lower shaft (9) surrounding formsLow-temperature space; At this moment the crystal crushed aggregate (6) in crucible (5) melts, when the crystalline substance in described crucible (5)When body particle (6) all melts, the upper end head of described seed crystal (7) also beginning melts, byIn lower shaft (9) effect of cooling medium, seed crystal (7) melts and is obviously later than crystal crushed aggregate (6)Melt; Then reduce jacket temperature, the low temperature of low-temperature space passes to crucible (5), makes described crucible(5) start the slow uniform decrease in temperature to top by bottom, formation temperature gradient, melts in crucible (5)Crystalline material locate to start by bottom seed crystal (7) crystallization of growing, obtain crystalline material piece.
32. while implementing the claims 1,7,12～18,21～22 arbitrary described grown crystal materialThe another kind of grown crystal material of thermograde control device time thermograde control method, its spyLevy and be: crucible (5) is arranged on the upper end of lower shaft (9) in furnace chamber (1), in crucible (5)Bottom be provided with seed crystal (7), at the upper crystal crushed aggregate (6) of placing of seed crystal (7), by crucible (5)In sleeve (4), the fixing hole (14) of sleeve (4) bottom is enclosed within the middle part of lower shaft (9),The outside of described sleeve (4) is provided with heater (3), and described heater (3) connects respectively power supplyBoth positive and negative polarity, heater (3) is to sleeve (4) radiation heating, and sleeve (4) evenly passes to heatCrucible (5) passes into cooling medium in described lower shaft (9) simultaneously, and described lower shaft (9) surrounding formsLow-temperature space; At this moment the crystal crushed aggregate (6) in crucible (5) melts, when the crystalline substance in described crucible (5)When body particle (6) all melts, the upper end head of described seed crystal (7) also beginning melts, byIn lower shaft (9) effect of cooling medium, seed crystal (7) melts and is obviously later than crystal crushed aggregate (6)Melt, then reduce jacket temperature, in described sleeve (4), lower shaft (9) surrounding of part formsLow-temperature space, the low temperature of low-temperature space passes to crucible (5), makes described crucible (5) be started supreme by bottomThe slow uniform decrease in temperature of portion, formation temperature gradient, the crystalline material melting in crucible (5) is by bottom seed crystal(7) locate to start the crystallization of growing, obtain crystalline material piece.
Thermograde control method when 33. grown crystal material according to claim 32, itsFeature is: be provided with the additional cylinder in bottom (30) in the bottom of sleeve (4), enter the cooling of lower shaft (9)Medium lower shaft (9) surrounding in described sleeve (4) forms in low-temperature space, at sleeve (4)Lower shaft (9) surrounding of bottom also forms low-temperature space simultaneously, adds cylinder (30) low temperature is poly-by bottomCollection, the low temperature of described gathering forms the cooling of auxiliary socket (4) bottom, and the low temperature of described gathering is guaranteedIn furnace chamber (1) other local the least possible heat run off.
34. temperature ladders while implementing the claims 20～22 and 30 arbitrary described grown crystal materialDegree control device the third grown crystal material time thermograde control method, it is characterized in that:The interior crucible of furnace chamber (1) (5) is arranged on the crucible putting hole (31) of sleeve (4) bearing plate (33)Upper, the bottom in crucible (5) is provided with seed crystal (7), the interior seed crystal of crucible (5) (7) locate exposedBearing plate (33) bottom of sleeve (4), at the upper crystal crushed aggregate (6) of placing of described seed crystal (7),The outside of described sleeve (4) is provided with heater (3), and described heater (3) connects respectively power supplyBoth positive and negative polarity, heater (3) is to sleeve (4) radiation heating, and sleeve (4) evenly passes to heatCrucible (5) is noted by the inert gas that is arranged on the furnace chamber (1) described in interior the bottom of sleeve (4) simultaneouslyHand-hole, is filled with sleeve (4) by inert gas, then many via on bearing plate (33) of inert gasIndividual cooling medium pod apertures (32) enters sleeve (4), makes crucible (5) bottom temp lower than top;At this moment the crystal crushed aggregate (6) in crucible (5) melts, when the crystal crushed aggregate (6) in described crucible (5)While all thawing, the upper end head of described seed crystal (7) also beginning melts, and is subject to inert gasEffect, the seed crystal (7) of crucible (5) bottom melts the thawing speed that is obviously later than crystal crushed aggregate (6),Then reduce jacket temperature, make to benefit from first the interior seed crystal (7) of crucible (5) of inert gasCooling, force described crucible (5) to start the slow uniform decrease in temperature to top by bottom, formation temperature gradient,The crystalline material melting in crucible (5) locates to start by bottom seed crystal (7) crystallization of growing, and obtains crystalMaterial block.
35. according to temperature when arbitrary described grown crystal material in claim 31,32 or 34Gradient control method, described crystal crushed aggregate (6) is crystal powder, crystal chunk or crystal grain.
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| CN201210020279.0A CN103160934B (en) | 2011-12-18 | 2012-01-10 | Thermograde control device and method thereof when a kind of grown crystal material |
| PCT/CN2012/000268 WO2013104089A1 (en) | 2012-01-10 | 2012-03-02 | Temperature gradient control device for crystal growth and method thereof |
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| CN201210020279.0A CN103160934B (en) | 2011-12-18 | 2012-01-10 | Thermograde control device and method thereof when a kind of grown crystal material |
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| CN104695015B (en) * | 2013-12-05 | 2018-01-09 | 长春理工大学 | Grow CaF2Crystal adjusts the method and device of thermal field structure |
| CN104501595B (en) * | 2014-11-28 | 2016-06-15 | 张家港市华孚实业有限公司 | A kind of processing unit (plant) for insulation material |
| CN106422983A (en) * | 2016-11-10 | 2017-02-22 | 郑州磨料磨具磨削研究所有限公司 | Ultrahigh-pressure pressurizing and heating device |
| CN109321975B (en) * | 2018-11-19 | 2020-09-08 | 永平县泰达废渣开发利用有限公司 | Monocrystalline silicon directional solidification seeding module |
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Denomination of invention: Device and method of temperature gradient control in growth process of crystal material Effective date of registration: 20180110 Granted publication date: 20160518 Pledgee: Xin Rong investment Company limited by guarantee Pledgor: Luoyang Jinnuo Mechanical Engineering Co., Ltd. Registration number: 2017410000032 |
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Date of cancellation: 20190614 Granted publication date: 20160518 Pledgee: Xin Rong investment Company limited by guarantee Pledgor: Luoyang Jinnuo Mechanical Engineering Co., Ltd. Registration number: 2017410000032 |