CN104499042A - Growth method of microporous sapphire crystal - Google Patents
Growth method of microporous sapphire crystal Download PDFInfo
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- CN104499042A CN104499042A CN201410770787.XA CN201410770787A CN104499042A CN 104499042 A CN104499042 A CN 104499042A CN 201410770787 A CN201410770787 A CN 201410770787A CN 104499042 A CN104499042 A CN 104499042A
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- sapphire
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- molybdenum
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Abstract
The invention discloses a growth method of a microporous sapphire crystal, which comprises the following steps: S1. growing a sapphire plate, cooling and discharging; S2. taking out the sapphire plate grown in the step S1, cutting one or a plurality of troughs in the length direction of the plate along the tail of the sapphire plate, and fixing a molybdenum wire or tungsten wire with the diameter of 0.5mm below into the troughs of the sapphire plate; S3. by using the sapphire plate fixed with the molybdenum wire or tungsten wire in the step S2 as the seed crystal, carrying out crystal seeding so that the molybdenum wire or tungsten wire and the sapphire plate grow together; and S4. after processing the sapphire plate into the preset shape, putting into a muffle furnace, and sublimating the molybdenum wire or tungsten wire off in an air atmosphere, thereby forming the microporous sapphire. The method can process the micropores with the diameter of 0.5mm below and the length of 15mm above on the sapphire crystal, which can not be implemented by the common boring or laser boring process.
Description
Technical field
The present invention relates to sapphire production unit technical field, particularly relate to a kind of growth method of micropore sapphire crystal.
Background technology
Sapphire crystal has the optical window material that good through performance is used to many measurement and analysis instruments in visible ray to 5.6um spectral range.The anisotropy of sapphire crystal, is applied to waveguide laser cavity, Surface Acoustic Wave Filter, retarding line, ultrasonic wave transport element; The hardness (Mohs degree 9) of sapphire crystal is only second to diamond, he has hardness and intensity is high, resistance to wear, feature that heat-resisting ability is strong and stable chemical nature, the series of characteristics such as acid-alkali-corrosive-resisting, are widely used in high power laser light window, high temperature resistant, high pressure, resistance to high-speed friction, container or the viewing window of vacuum vessel and the heating panel etc. of optical window and projector such as to be able to bear strong corrosion; Sapphire crystal such as square, arc, trilateral, the ellipse of different shape are widely used in nonmagnetic bracing frame, high temperature insulating material, isolating frame, faceplate of scanner etc.
The main method of current sapphire crystal growth has: flame method, crystal pulling method, kyropoulos, heat-exchanging method, falling crucible method and EFG technique etc.In aforesaid method, flame method due to thermograde excessive and cannot growth diameter be greater than the monocrystalline of 50mm and the defect of crystal and inner-stress value higher, range of application is greatly limited.The methods such as crystal pulling method, kyropoulos, heat-exchanging method, falling crucible method can growing large-size sapphire crystal, but they need through repeatedly high rigidity cutting, shaping, after a series of heavy mechanical workouts such as grinding, can make applicable shape and size, operation is more complicated; Cost is high and consuming time; Crystalline material utilization ratio is lower, and working efficiency is not high, and cost remains high.
The hardness (Mohs degree 9) of sapphire crystal is only second to diamond, just because of its high rigidity and the characteristic of high strength, sapphire is difficult to processed, for the hole of below 0.5mm, when drilling depth is more than more than 15mm, drill bit intensity does not reach, after laser boring, micropore makes melt still be present in micropore due to capillarity, can not achieve the goal.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, a kind of growth method of micropore sapphire crystal is provided, below diameter 0.5mm can be processed on sapphire crystal, the micropore of length more than 15mm.
Technical solution of the present invention is as follows:
A growth method for micropore sapphire crystal, comprises the following steps:
S1, the sapphire plate of growth width 30mm ~ 300mm, thickness 4mm ~ 30mm, reaches the long 30mm ~ 50mm of equal-diameter part break away from moulds later, comes out of the stove after cooling;
S2, take out the sapphire plate of step S1 growth, cutting out along panel length direction the fluting that one or several diameter is 0.5 ~ 1mm at sapphire plate afterbody, is that molybdenum filament or the tungsten filament of below 0.5mm is fixed in the fluting of sapphire plate by diameter; Molybdenum filament or tungsten filament fusing point higher than sapphire fusing point, and get along well sapphire reaction.
S3, secures the sapphire plate of molybdenum filament or tungsten filament as seed crystal using step S2, continue to grow 5 ~ 30mm length and pull after carrying out seeding, and molybdenum filament or tungsten filament and sapphire plate grow together;
S4, takes out sapphire plate that step S3 obtains and after being worked into presetting shape, puts in retort furnace to burn 1100 DEG C ~ 1200 degrees Celsius under air atmosphere and molybdenum filament or tungsten filament distillation are fallen, and forms micropore sapphire.
More preferably, the sapphire plate of step S1 growth width 30 ~ 300mm, thickness 4 ~ 30mm specifically comprises the following steps:
101, shove charge: select M to or A be fixed on seed chuck to seed crystal, mould is loaded in molybdenum crucible fixing, loads molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
102, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
103, heat up: open heating power supply and be warmed up to 2100 ~ 2300 DEG C, mould mouth material grain is melted;
104, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
105, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed (20mm/h ~ 30mm/h), makes crystal middle to outgrowth along seed crystal from mould by shouldering;
106, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to (30mm/h ~ 50mm/h), when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
107, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
More preferably, step S3 specifically comprises the following steps:
301, shove charge: the sapphire plate securing molybdenum filament or tungsten filament is as seed crystal and be fixed on seed chuck, loads mould in molybdenum crucible fixing, loads molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
302, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
303, heat up: open heating power supply and be warmed up to 2100 ~ 2300 DEG C, mould mouth material grain is melted;
304, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
305, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed (20mm/h ~ 30mm/h), makes crystal middle to outgrowth along seed crystal from mould by shouldering;
306, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to (30mm/h ~ 50mm/h), when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
307, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
More preferably, described in step S2, by molybdenum filament or tungsten filament, the method be fixed in the fluting of sapphire plate is:
201, sapphire plate afterbody cuts out along panel length direction the fluting that one or several diameter is 0.5mm ~ 1mm;
202, arrange vertical fluting in the side of seed crystal, the bottom extended line of described vertical fluting is crossing with the extended line of the fluting place straight line of described sapphire plate afterbody;
203, by diameter be the molybdenum filament of below 0.5mm or tungsten filament be arranged on described sapphire plate afterbody fluting in and vertically in fluting;
204, the top of seed crystal arranges molybdenum filament or tungsten filament hole, and the molybdenum filament of dual-side or tungsten filament fix molybdenum filament or tungsten filament through molybdenum filament or the knotting of tungsten filament hole.
Compared with prior art, beneficial effect of the present invention has: the present invention is by the molybdenum filament of below diameter 0.5mm or tungsten filament progress sapphire sheet material, then by the method for distillation, molybdenum filament or tungsten filament distillation are fallen, to form micropore sapphire, below diameter 0.5mm can be processed on sapphire crystal, the micropore of more than length 15mm is that common drilling method and laser boring can not realize.
Accompanying drawing explanation
Fig. 1 is the growth method schematic flow sheet of a kind of micropore sapphire crystal of the present invention;
Fig. 2 is seed crystal of the present invention, sapphire plate fixes front view;
Fig. 3 is seed crystal, sapphire plate fixation side view;
Fig. 4 is sapphire plate upward view.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
As shown in Figure 1, a kind of growth method of micropore sapphire crystal, comprises the following steps:
S1, the sapphire plate of growth width parameter as shown in table 1, reaches the long 30mm ~ 50mm of equal-diameter part break away from moulds later, comes out of the stove after cooling; The present embodiment selects molybdenum filament to distil;
Table 1 sapphire plate.Fluting diameter and molybdenum filament diameter parameters (unit: mm)
| Sapphire plate width | Sapphire plate thickness | Fluting diameter | Molybdenum filament diameter |
| 30 | 4 | 0.5 | 0.4 |
| 200 | 20 | 0.8 | 0.3 |
[0043]
| 300 | 30 | 1 | 0.1 |
Step S1 grows width sapphire plate and specifically comprises the following steps:
101, shove charge: select M to or A be fixed on seed chuck to seed crystal, mould is loaded in molybdenum crucible fixing, loads molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
102, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
103, heat up: open heating power supply and be warmed up to 2100 ~ 2300 DEG C, mould mouth material grain is melted;
104, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
105, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed (it is 20mm/h ~ 30mm/h that the present embodiment shouldering limits speed), makes crystal middle to outgrowth along seed crystal from mould by shouldering;
106, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to 30mm/h ~ 50mm/h, when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
107, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
S2, take out the sapphire plate of step S1 growth, cutting out one or several fluting (the present embodiment all use a fluting) at sapphire plate afterbody along panel length direction according to table 1 parameter, is that the molybdenum filament of below 0.5mm is fixed in the fluting of sapphire plate by diameter;
The method be fixed on by molybdenum filament in the fluting of sapphire plate described in step S2 is:
201, as shown in Figure 2, Figure 3, Figure 4: sapphire plate 1 afterbody along panel length direction (along longer sides direction, general cutting parallel with long limit) cut out the fluting 2 (it is that the present embodiment is slotted, and diameter is with reference to table 1 parameter) that a diameter is 0.5mm ~ 1mm; Sapphire plate 1 afterbody refers to and is fixed on after on seed crystal head, the bottom surface of sapphire plate 1.
202, arrange vertically fluting 4 in the side of seed crystal 3, the bottom extended line of described vertical fluting 4 is crossing with the extended line of the fluting 2 place straight line of described sapphire plate afterbody;
203, in the fluting 2 that the molybdenum filament being below 0.5mm by diameter according to table 1 parameter is arranged on described sapphire plate afterbody and vertically in fluting 4;
204, the top of seed crystal 3 arranges molybdenum filament hole 5, and the molybdenum filament of dual-side is tied a knot through molybdenum filament hole 5 and fixed molybdenum filament.
S3, secures the sapphire plate of molybdenum filament as seed crystal using step S2, continue to grow 5mm ~ 30mm length after carrying out seeding and pull, molybdenum filament and sapphire plate grow together;
Step S3 specifically comprises the following steps:
301, shove charge: the sapphire plate securing molybdenum filament is as seed crystal and be fixed on seed chuck, loads mould in molybdenum crucible fixing, loads molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
302, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
303, heat up: open heating power supply and be warmed up to 2100 ~ 2300 DEG C, mould mouth material grain is melted;
304, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
305, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed (20mm/h ~ 30mm/h), makes crystal middle to outgrowth along seed crystal from mould by shouldering cooling;
306, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to (30mm/h ~ 50mm/h), when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
307, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
S4, takes out sapphire plate that step S3 obtains and after being worked into presetting shape, puts in retort furnace to burn 1100 DEG C ~ 1200 DEG C under air atmosphere and molybdenum filament distillation fallen, and forms micropore sapphire.
Below be only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a growth method for micropore sapphire crystal, is characterized in that, comprises the following steps:
S1, the sapphire plate of growth width 30 mm ~ 300mm, thickness 4 mm ~ 30mm, reaches the long 30mm ~ 50mm of equal-diameter part break away from moulds later, comes out of the stove after cooling;
S2, takes out the sapphire plate of step S1 growth, and cutting out one along panel length direction or some diameters are the fluting of 0.5mm ~ 1mm at sapphire plate afterbody, is that molybdenum filament or the tungsten filament of below 0.5mm is fixed in the fluting of sapphire plate by diameter;
S3, secures the sapphire plate of molybdenum filament or tungsten filament as seed crystal using step S2, continue to grow 5 ~ 30mm length and pull after carrying out seeding, and molybdenum filament or tungsten filament and sapphire plate grow together;
S4, takes out sapphire plate that step S3 obtains and after being worked into presetting shape, puts in retort furnace to burn 1100 DEG C ~ 1200 DEG C under air atmosphere and molybdenum filament or tungsten filament distillation are fallen, and forms micropore sapphire.
2. the growth method of a kind of micropore sapphire crystal according to claim 1, is characterized in that, step S1 grows width 30mm ~ 300mm, the sapphire plate of thickness 4mm ~ 30mm specifically comprises the following steps:
101, shove charge: select M to or A be fixed on seed chuck to seed crystal, mould is loaded in molybdenum crucible fixing, loads molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
102, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
103, heat up: open heating power supply and be warmed up to 2100 DEG C ~ 2300 DEG C, mould mouth material grain is melted;
104, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
105, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed, makes crystal middle to outgrowth along seed crystal from mould by shouldering cooling;
106, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to 30 mm/h ~ 50mm/h, when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
107, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
3. the growth method of a kind of micropore sapphire crystal according to claim 1, it is characterized in that, step S3 specifically comprises the following steps:
301, shove charge: the sapphire plate securing molybdenum filament or tungsten filament is fixed on seed chuck as seed crystal, mould is loaded in molybdenum crucible fixing, load molybdenum crucible 5kg ~ 7kg flame melt method particle, seed rod is arranged on sapphire wafer growing die middle, mould mouth blowing grain;
302, vacuumize and applying argon gas: close fire door, open mechanical pump and vacuumize, close vacuum apparatus when vacuum tightness reaches 3Pa ~ 10Pa, applying argon gas is to standard atmospheric pressure;
303, heat up: open heating power supply and be warmed up to 2100 ~ 2300 DEG C, mould mouth material grain is melted;
304, seeding: turned down by seed crystal after the material grain fusing of mould mouth, start seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding also upwards lift seed crystal with the speed of 5mm/h ~ 20mm/h;
305, shouldering: the seed rod rate of pulling is adjusted to shouldering and limits speed, makes crystal middle to outgrowth along seed crystal from mould by shouldering cooling;
306, isodiametric growth: after shouldering terminates, carries out isodiametric growth, and improve pulling rate to 30 mm/h ~ 50mm/h, when warm field is stable, heating power during isodiametric growth and the rate of pulling remain unchanged;
307, cooling: pull crystal break away from moulds, starts cooling, drops to room temperature, come out of the stove after 10h.
4. the growth method of a kind of micropore sapphire crystal according to claim 1, is characterized in that, described in step S2, by molybdenum filament or tungsten filament, the method be fixed in the fluting of sapphire plate is:
201, sapphire plate afterbody cuts out along panel length direction the fluting that one or several diameter is 0.5mm ~ 1mm;
202, arrange vertical fluting in the side of seed crystal, the bottom extended line of described vertical fluting is crossing with the extended line of the fluting place straight line of described sapphire plate afterbody;
203, by diameter be the molybdenum filament of below 0.5mm or tungsten filament be arranged on described sapphire plate afterbody fluting in and vertically in fluting;
204, the top of seed crystal arranges molybdenum filament or tungsten filament hole, and the molybdenum filament of dual-side or tungsten filament fix molybdenum filament or tungsten filament through molybdenum filament or the knotting of tungsten filament hole.
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Application publication date: 20150408 |