CN109554758A - One kind, which is held, burns device and preparation method thereof - Google Patents
One kind, which is held, burns device and preparation method thereof Download PDFInfo
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- CN109554758A CN109554758A CN201811597599.6A CN201811597599A CN109554758A CN 109554758 A CN109554758 A CN 109554758A CN 201811597599 A CN201811597599 A CN 201811597599A CN 109554758 A CN109554758 A CN 109554758A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0006—Composite supporting structures
Abstract
It is held the present invention relates to one kind and burns device and preparation method thereof, belong to refractory kiln preparation technical field.In order to overcome existing hold to burn the device technical problem that there is impurity is more, easily-deformable, the service life is short, load is small, energy consumption is high, the present invention, which provides one kind and holds, burns device and preparation method thereof, this holds burning device and is only made of the signle crystal alumina of 99.99% or more purity, and the big crystal that is integrally formed, impurity are negligible.Signle crystal alumina of the invention holds burning device and is unlikely to deform through multiple high temp roasting, and the service life is longer；Since the hardness of signle crystal alumina has reached Mohs' hardness 9, while there is high intensity again, so the load for holding burning device is bigger, what can be done is thinner, reduces energy consumption.Disclosed by the invention is widely suitable to have wide industrial applications prospect in the roasting apparatus such as various kilns, annealing furnace.
Description
Technical field
It is held this application involves refractory kiln preparation technical field more particularly to one kind and burns device and preparation method thereof.
Background technique
As a kind of kiln furnitures, holds burning device and be widely used in the roasting apparatus such as various kilns, annealing furnace, as branch
Support, conveying, support pad are effectively prevent gas and harmful substance to the destruction of green body and are stained by the carrier of sintering briquette body.Industry
On generally it is plate-like be known as load bearing board, box shaped uncovered is known as saggar.And existing hold burns the use of the device overwhelming majority
Ceramics or mullite (3Al2O3·2SiO2) be made, the burning device that holds of this prior art has the following deficiencies:
1, purity is low, impurity is more.Impurity composition volatilizees under high temperature, is attached to by sintering briquette body, forms stain or stain, wave
Send out component easily with generated by elements such as (such as electronic component of magnetic material) contains in sintering briquette body iron, oxygen, manganese, zinc it is anti-
It answers, causes the pollution of magnetic material；
2, easy buckling deformation, cracking, rough surface, service life are short.Holding to burn device and be deformed easily makes to be produced by sintering briquette body
Change shape, breakage, poor response；
3, load is small, load-bearing is low.Tradition burns device since the rigidity of ceramic material is low by holding for ceramic making, leads to load
Ability is limited, and load-bearing is lower；
4, energy consumption is high.Traditional ceramics hold burn device since thickness is larger, it is thermally conductive to need to consume a large amount of thermal energy.
However, the alternative materials of these defects can be overcome by no means easy in vast as the open sea Material Field searching, direct face
The difficulty faced is after only carrying out related experiment comparison to the product of alternative materials, could really to know its performance advantage.
Summary of the invention
The application, which provides one kind and holds, burns device and preparation method thereof, with solve it is existing hold burn device there is impurity it is more,
Technical problem easily-deformable, the service life is short, load is small, energy consumption is high.
Technical solution provided by the present application is:
In order to reach the technical purpose to solve the above problems, the application's in a first aspect, providing one kind holds burning device, described
It holds burning device to be made of signle crystal alumina, holds signle crystal alumina purity >=99.99% in the component for burning device, the purity is matter
Measure percentage fractional.
In order to reach the technical purpose for holding burning device prepared and solved the above problems, the second aspect of the application is provided
It is a kind of to hold the preparation method for burning device, comprising the following steps:
Seed crystal is mounted on the shadoof of crystal growing furnace, shadoof is mounted in the cavity of crystal growing furnace；
The alumina raw material that purity is 4N is packed into crucible, then crucible is packed into the cavity of the crystal growing furnace, is closed
It is vacuumized after closed chamber body, vacuum degree in cavity is made to reach 1e-4pa；
The material power for selecting the crystal growing furnace is 5~10kW/h, and power is risen to target power by initial power 0
70~120kW, the continuous heating under target power make crystal growth in-furnace temperature up to 2050~2200 DEG C；
After liquid stream is stablized in the crystal growing furnace, the seed crystal is transferred, in decentralization process, if seed crystal lower end is baked
Circle, is lifted up 20~30mm of shadoof, while reducing by 0.3~1kW of power；If seed crystal lower end by roasting circle, does not transfer seed persistently
Crystalline substance, seed crystal are inserted into 5~20mm of liquid level or less after contacting liquid level；Stop decentralization seed crystal at this time, is lifted up shadoof, makes pulling rate
0.5~2mm/h；
When crystal growth to diameter is 60~100mm, stopping is lifted up shadoof, makes pulling rate 0, while controlling under power
Drop, the range of decrease are 20~80W/h；
When the crystal weight reaches the 8~15% of charge, by control power decline, the range of decrease is 10~80W/h, is made
Rate of crystalline growth < 2kg/h；
When the crystal weight is the 80~95% of charge, it is lifted up shadoof, makes pulling rate up to 0.5~3mm/h, when
When crystal weight is without fluctuation and close to charge, 10~20h of state is maintained；
So that power is at the uniform velocity down to 0 in 100~180h, obtains signle crystal alumina crystal ingot；
Bubble-free, free from admixture, dislocation-free crystal ingot part in the signle crystal alumina crystal ingot are cut into and hold burning device.
Optionally, the seed crystal is rectangular or round α-Al2O3Monocrystalline, length are 150mm~200mm, and wide or diameter is 15
~25mm, seed crystal roughness Ra≤0.8 μm.
Optionally, the crucible is tungsten crucible or molybdenum crucible or tungsten-molybdenum alloy crucible.
Optionally, if floating crystalline substance occurs in liquid level during before seed crystal contact liquid level, power is improved；When floating crystalline substance disappears
It loses, decentralization seed crystal and molten soup welding when liquid level stabilizing.
Optionally, during the stopping decentralization seed crystal is 60~100mm to diameter to the crystal growth, every 1~
10min wink mentions 0.5~2mm, mentions altogether 20~50 times.
Optionally, mention 2~5mm in wink when the crystal weight reaches the 8~15% of charge, by power improve 300~
800W。
Optionally, method used in the cutting is diamond cut.
Optionally, the flawless crystal ingot be cut into plate, saggar shape or abnormity hold burning device.
Optionally, the burning device that holds is placed in annealing furnace, is evacuated to 1e-4pa, is made in-furnace temperature in 20~30h
1300~1600 DEG C are risen to, 20~36h of this temperature is maintained, heater power is uniformly then down to 0 in 65~75h, cooling
To room temperature.
Beneficial effect by adopting the above technical scheme is:
1, purity is higher, impurity is few.It is chemical up to 99.99% or more to hold signle crystal alumina in the material composition for burning device
Stability is good, and paint having no volatile substances generate in hot environment, ensure that atmosphere degree of purity, that is, is used in the roasting of electronic component
It will not pollute by sintering briquette body；
2, be unlikely to deform, be cracked, hold burn device hardness it is high, intensity is big, characteristic resistant to high temperature was actually using it
Service life in journey has very big extension than conventional products, and crystal can be cut very smooth, and high temperature use for a long time will not go out
The phenomenon that existing rough surface；
3, load is big, load-bearing is high.Since the hardness of signle crystal alumina has reached Mohs' hardness 9, while intensity is again very big, can
To bear bigger energy consumption weight and charge, same stove, which holds burning device using signle crystal alumina, can have more 30%-
50% charge；
4, low energy consumption.It burns device compared to holding for traditional ceramics matter and can be thinned to original 10%, volume is much smaller than normal
Product is advised, thus heating conduction is more preferable, reduces energy consumption.
Specific embodiment
The application's in a first aspect, providing one kind holds burning device, and described hold is burnt device and be made of signle crystal alumina, holds burning dress
Signle crystal alumina purity >=99.99% in the component set, the purity are mass fraction percentage.Why aoxidized using monocrystalline
The big crystal of aluminium is in addition to use purity because signle crystal alumina has the characteristic that hardness is high, intensity is big, high temperature resistant, thermal conductivity are good
>=99.99% signle crystal alumina is further reduced the influence of impurity, has ensured the excellent properties for holding and burning device, has been not easily susceptible to
Interference.
The second aspect of the application provides a kind of preparation method held and burn device.
Below by embodiment, the second aspect of the application is described in further detail.
Embodiment 1
The present embodiment hold burn device the preparation method is as follows:
It prepares one kind and holds burning device, this, which holds, burns device for signle crystal alumina load bearing board, prepares signle crystal alumina with melt method
Big crystal is integrally formed through cutting, obtains the signle crystal alumina load bearing board of 99.99% or more purity, preparation method is as follows:
Prepare: getting rectangular α-Al2O3Monocrystalline, length 150mm, wide 15mm, seed crystal roughness Ra=0.4 μm.Then with inclined
Light microscopic and strong photoelectricity check seed crystal, whether there is bubble, wrappage, crystal boundary, twin and crackle etc. inside observation seed crystal
Defect, qualified seed crystal is under polarized light without obvious NOL ring.If it was found that the qualified seed crystal of the unqualified timely replacement of seed crystal, to avoid seed
Transgranular there are excessive defects to be genetic in grown crystal, influences crystal quality, selects qualified seed crystal, seed crystal is mounted on crystal
On the shadoof of growth furnace, shadoof is mounted in the cavity of crystal growing furnace；It uses purity for the high-purity mangesium oxide aluminum feedstock of 4N, fills
Enter in tungsten-molybdenum alloy crucible, then crucible is packed into the cavity of crystal growing furnace.Check thermal field, heat protection screen, temperature sensor etc.
It is whether normal, it closes chamber lid and vacuumizes, when vacuum degree reaches 1e-4pa in furnace, vacuumize completion.
The alumina raw material that 4N purity is used in this step, tentatively ensure that the degree of purity for preparing product from source, control
The content of impurity.Tungsten-molybdenum alloy crucible has both the good characteristic of tungsten crucible and molybdenum crucible, has fusing point height, elevated temperature strength good, anti-
Grind that corrosion-resistant, pyroconductivity is big, thermal expansion coefficient is small, harden ability is good without internal fissure, the advantage that size is accurate, inside and outside wall is bright and clean,
Crystal pulling quality is controlled and de- brilliant viscous pot has remarkable result.Condition of high vacuum degree guarantees the atmosphere clean degree of combinations environment, reduces empty
Adverse effect of the gas to crystallization.
Material: the material power of selected crystal growing furnace is 5kW/h, and power is risen to target power by initial power 0
70kW, the continuous heating under target power make in-furnace temperature up to 2050 DEG C, are completely melt raw material in furnace.
This step makes in-furnace temperature reach 2050 DEG C, has been more than the fusing point of alumina raw material, has reached what raw material was completely melt
Purpose.
Seeding: after liquid stream is stablized in furnace, transferring seed crystal, in decentralization process, if seed crystal lower end is lifted up and is mentioned by roasting circle
Bar 20mm, while reducing power 1kW；If seed crystal lower end by roasting circle, does not transfer seed crystal persistently, is inserted into liquid after seed crystal contact liquid level
5mm below face；It is lifted up shadoof at this time, makes pulling rate 0.5mm/h, up to crystal growth to diameter is 60mm.
Experiment is found, during seeding, since the volatilization of tungsten in the impurity and furnace in alumina raw material easily makes to melt
There is floating crystalline substance in soup, if floating crystalline substance occurs in liquid level in seed crystal decentralization process, will increase seeding difficulty, reduces crystal quality.At this point, passing through
Power is improved, increase in-furnace temperature, the floating crystalline substance of removal maintains power at this time when floating brilliant disappearance in furnace, when liquid stream is stablized, under
Put seed crystal and molten soup welding；
Experiment also found, since in dislocation easily heredity to crystal, mentioning in wink during seeding can pole above seed crystal
Big reduction dislocation heredity, promotes crystal quality.Therefore every 1min wink mentions 0.5mm, mentions altogether 20 times, until crystal diameter is 60mm.
Expand shoulder growth: stopping is lifted up shadoof, makes pulling rate 0, while controlling power decline, and range of decrease 20W/h works as crystalline substance
Body weight reaches the 8% of charge, completes to expand shoulder；Wink mentions 2mm at this time, and power is improved 300W.
This step reduces in-furnace temperature by control power decline indirectly, makes to continue crystalline growth in furnace.
Test discovery, crystal turns to melt the easily viscous pot of soup at shoulder, if not mended warm processing, crystal turn shoulder it is endless hologony it is viscous
Pot phenomenon, will lead to crystal cleavage, influences crystal quality.The present invention mentions crystal wink when turning shoulder, while improving power, is promoted
Crucible peripheral temperature prevents molten soup from gluing pot, completes crystal and turns shoulder.
Isodiametric growth: by control power decline, range of decrease 10W/h controls long speed < 2kg/h.
This step reduces range of decrease value, makes crystal growth in the long speed of control by adjusting the range of decrease.
Finishing phase: when crystal weight is the 80% of charge, it is lifted up shadoof, makes pulling rate up to 0.5mm/h, works as crystalline substance
When body weight is without fluctuation and close to charge, state 10h is maintained, ending is completed.
The purpose for being lifted up shadoof in this step and maintaining pulling rate state is to prevent viscous pot.
Annealing stage: incision cycle of annealing makes power at the uniform velocity be reduced to 0, obtains signle crystal alumina crystal ingot in 100h.
Delay drop by the power of 100h, prevents crystal cleavage, reduce in-furnace temperature.
Excision forming: assessing obtained signle crystal alumina crystal ingot with laser pen, by bubble-free, free from admixture, without position
The flawless crystal ingot part such as mistake is cut into plate using diamond cutting and holds burning device, i.e. signle crystal alumina load bearing board.
The benefit of this step diamond cut is that cutting is regular, not easy damaged crystal.
Additional step: when roasting has the sheet parts of high-precision requirement to flatness, for the plane for avoiding load bearing board
Degree is not high to cause adverse effect to green body, needs to increase high temperature Shape correction step to load bearing board.
High temperature Shape correction step are as follows: will be placed in high-temperature annealing furnace, and vacuumize to shaping signle crystal alumina load bearing board
To 1e-4pa, it is warming up to 1300~1600 DEG C in 20~30h, maintains 20~36h of this temperature, it then will heating in 65~75h
Device power is uniformly down to 0, is cooled to room temperature, and bell is opened after vacuum breaker and takes out load bearing board.
Following table is sufficiently verified by carrying out durability test comparison to signle crystal alumina pilot sample and traditional conventional products
The beneficial effect of the technical program.
1 durability test contrast table A of table
2 durability test contrast table B of table
By above-mentioned table 1, table 2 it is found that compared with traditional ceramics hold and burn device, signle crystal alumina provided by the present application holds burning dress
The durability set is more preferably: more resistant to high temperature, being not easy warpage, cracking, resistance to cracking is more preferable, and no discoloration shows that stability is stronger, is not easy
It being reacted at high temperature with roasting green body, atmosphere degree of purity is higher, and thinner, the load of unit volume is bigger, while volume
Diminution advantageously reduces energy consumption.
Embodiment 2
Holding for the present embodiment burns device for signle crystal alumina saggar, prepares the big crystal of signle crystal alumina through cutting with melt method
It is integrally formed, preparation method is as follows:
Prepare: round α-Al2O3Monocrystalline, length 150mm, diameter 15mm, seed crystal roughness Ra=0.8 μm.Then polarisation is used
Mirror and strong photoelectricity check seed crystal, whether there is bubble, wrappage inside observation seed crystal, and crystal boundary, twin and crackle etc. lack
It falls into, qualified seed crystal is under polarized light without obvious NOL ring.If it was found that the qualified seed crystal of the unqualified timely replacement of seed crystal, to avoid seed crystal
Inside there is excessive defect to be genetic in grown crystal, influence crystal quality and select qualified seed crystal, it is raw that seed crystal is mounted on crystal
On the shadoof of long furnace, shadoof is mounted in the cavity of crystal growing furnace；It uses purity for the high-purity mangesium oxide aluminum feedstock of 4N, is packed into
In tungsten crucible, then will be in the cavity of crucible loading crystal growing furnace.Check whether thermal field, heat protection screen, temperature sensor etc. are normal,
It closes chamber lid to vacuumize, when vacuum degree reaches 1e-4pa in furnace, vacuumizes completion.
Using the alumina raw material of 4N purity, the degree of purity for preparing product tentatively ensure that from source, control containing for impurity
Amount.Tungsten crucible have fusing point is high, elevated temperature strength is good, it is wear-resistant it is corrosion-resistant, pyroconductivity is big, thermal expansion coefficient is small and harden ability is good
Excellent properties.Condition of high vacuum degree guarantees the atmosphere clean degree of combinations environment, reduces adverse effect of the air to crystallization.
Material: the material power of selected crystal growing furnace is 10kW/h, and power is risen to target power by initial power 0
120kW, the continuous heating under target power make in-furnace temperature up to 2100 DEG C, are completely melt raw material in furnace.
This step makes in-furnace temperature reach 2100 DEG C, has been more than the fusing point of alumina raw material, has reached what raw material was completely melt
Purpose.
Seeding: after liquid stream is stablized in furnace, transferring seed crystal, in decentralization process, whenever seed crystal lower end is by roasting circle, is lifted up and mentions
Bar 30mm, while reducing power 0.3kW；If seed crystal lower end by roasting circle, is not transferred seed crystal persistently, is inserted into after seed crystal contact liquid level
20mm below liquid level；It is lifted up shadoof at this time, makes pulling rate 0.5mm/h, while every 10min wink mentions 2mm, mentions 50 times altogether, directly
To crystal growth to diameter be 60~100mm.
Expand shoulder growth: stopping is lifted up shadoof, makes pulling rate 0, while controlling power decline, and range of decrease 80W/h works as crystalline substance
Body weight reaches the 15% of charge, completes to expand shoulder；Wink mentions 5mm at this time, and power is improved 800W.
This step reduces in-furnace temperature by control power decline indirectly, makes to continue crystalline growth in furnace.
Isodiametric growth: by control power decline, range of decrease 80W/h controls long speed < 2kg/h.
This step reduces range of decrease value, makes crystal growth in the long speed of control by adjusting the range of decrease.
Finishing phase: when crystal weight is the 95% of charge, it is lifted up shadoof, makes pulling rate up to 3mm/h, works as crystal
When weight is without fluctuation and close to charge, state 20h is maintained, ending is completed.
The purpose for being lifted up shadoof in this step and maintaining pulling rate state is to prevent viscous pot.
Annealing stage: incision cycle of annealing makes power be reduced to 0, obtains signle crystal alumina crystal ingot in 180h.
Delay drop by the power of 180h, prevents crystal cleavage, reduce in-furnace temperature.
Excision forming: it is assessed with the crystal ingot that laser pen completes growth, by nothings such as bubble-free, free from admixture, dislocation-frees
Burning device is held as saggar shape using diamond cut in the crystal ingot part of defect.
The benefit of this step diamond cut is that cutting is regular, not easy damaged crystal.
The holding of above method preparation, which burns device, has purity is high, impurity few, is unlikely to deform, is cracked, and load is big and energy consumption
Low feature.
Embodiment 3
The burning device that holds of the present embodiment is that signle crystal alumina abnormity holds burning device, prepares the big crystalline substance of signle crystal alumina with melt method
Body is integrally formed through cutting, and preparation method is as follows:
Prepare: round α-Al2O3Monocrystalline, length 150mm, diameter 15mm, seed crystal roughness Ra=0.6 μm.Then polarisation is used
Mirror and strong photoelectricity check seed crystal, whether there is bubble, wrappage inside observation seed crystal, and crystal boundary, twin and crackle etc. lack
It falls into, qualified seed crystal is under polarized light without obvious NOL ring.If it was found that the qualified seed crystal of the unqualified timely replacement of seed crystal, to avoid seed crystal
Inside there is excessive defect to be genetic in grown crystal, influence crystal quality, select qualified seed crystal, it is raw that seed crystal is mounted on crystal
On the shadoof of long furnace, shadoof is mounted in the cavity of crystal growing furnace；It uses purity for the high-purity mangesium oxide aluminum feedstock of 4N, is packed into
In molybdenum crucible, then will be in the cavity of crucible loading crystal growing furnace.Check whether thermal field, heat protection screen, temperature sensor etc. are normal,
It closes chamber lid to vacuumize, when vacuum degree reaches 1e-4pa in furnace, vacuumizes completion.
The alumina raw material that 4N purity is used in this step, tentatively ensure that the degree of purity for preparing product from source, control
The content of impurity.The good characteristic of molybdenum crucible has the advantages that no internal fissure, size are accurate, inside and outside wall is bright and clean, to crystal pulling quality
Control and de- brilliant viscous pot have remarkable result.Condition of high vacuum degree guarantees the atmosphere clean degree of combinations environment, reduces air to crystallization
It influences.
Material: the material power of selected crystal growing furnace is 5kW/h, and power is risen to target power by initial power 0
95kW, the continuous heating under target power make in-furnace temperature up to 2200 DEG C, are completely melt raw material in furnace.
This step makes in-furnace temperature reach 2200 DEG C, has been more than the fusing point of alumina raw material, has reached what raw material was completely melt
Purpose.
Seeding: after liquid stream is stablized in furnace, transferring seed crystal, in decentralization process, if seed crystal lower end is lifted up and is mentioned by roasting circle
Bar 25mm, while reducing power 0.6kW；If seed crystal lower end by roasting circle, is not transferred seed crystal persistently, is inserted into after seed crystal contact liquid level
15mm below liquid level；It is lifted up shadoof at this time, makes pulling rate 1.2mm/h, while every 5min wink mentions 1.2mm, mentions 35 times altogether, directly
To crystal growth to diameter be 80mm.
Expand shoulder growth: stopping is lifted up shadoof, makes pulling rate 0, while controlling power decline, and the range of decrease is 20~80W/h,
When crystal weight reaches the 11% of charge, shoulder is expanded in completion；Wink mentions 3.5mm at this time, and power is improved 550W.
This step reduces in-furnace temperature by control power decline indirectly, makes to continue crystalline growth in furnace.
Isodiametric growth: by control power decline, range of decrease 45W/h controls long speed < 2kg/h.
This step reduces range of decrease value, makes crystal growth in the long speed of control by adjusting the range of decrease.
Finishing phase: when crystal weight is the 90% of charge, it is lifted up shadoof, makes pulling rate up to 1.8mm/h, works as crystalline substance
When body weight is without fluctuation and close to charge, state 15h is maintained, ending is completed.
The purpose for being lifted up shadoof in this step and maintaining pulling rate state is to prevent viscous pot.
Annealing stage: incision cycle of annealing makes power be reduced to 0, obtains signle crystal alumina crystal ingot in 140h.
Delay drop by the power of 140h, prevents crystal cleavage, reduce in-furnace temperature.
Excision forming: it is assessed with the crystal ingot that laser pen completes growth, by nothings such as bubble-free, free from admixture, dislocation-frees
The crystal ingot part of defect becomes abnormity using diamond cut and holds burning device.The benefit of this step diamond cut is cutting rule
It is whole, not easy damaged crystal.
The holding of above method preparation, which burns device, has purity is high, impurity few, is unlikely to deform, is cracked, and load is big and energy consumption
Low feature.
The above is only the specific embodiment of the application, make skilled artisans appreciate that or realization the application.It is right
A variety of modifications of these embodiments will be apparent to one skilled in the art, general original as defined herein
Reason can be realized in other embodiments without departing from the spirit or scope of the application.Therefore, the application will not
Be intended to be limited to the embodiments shown herein, and be to fit to it is consistent with the principles and novel features disclosed in this article most
Wide range.
Claims (10)
1. one kind holds burning device, which is characterized in that the burning device that holds is made of signle crystal alumina, is held single in the component for burning device
Crystal alumina purity >=99.99%, the purity are mass fraction percentage.
2. a kind of hold the preparation method for burning device, which comprises the following steps:
Seed crystal is mounted on the shadoof of crystal growing furnace, shadoof is mounted in the cavity of crystal growing furnace；
The alumina raw material that purity is 4N is packed into crucible, then crucible is packed into the cavity of the crystal growing furnace, closes chamber
It is vacuumized after body, vacuum degree in cavity is made to reach 1e-4pa；
Select the crystal growing furnace material power be 5~10kW/h, by power by initial power 0 rise to target power 70~
120kW, the continuous heating under target power make crystal growth in-furnace temperature up to 2050~2200 DEG C；
After liquid stream is stablized in the crystal growing furnace, transfer the seed crystal, in decentralization process, if seed crystal lower end by roasting circle, to
Upper promotion 20~30mm of shadoof, while reducing by 0.3~1kW of power；If seed crystal lower end by roasting circle, does not transfer seed crystal, seed persistently
5~20mm of liquid level or less is inserted into after crystalline substance contact liquid level；At this time stop decentralization seed crystal, be lifted up shadoof, make pulling rate 0.5~
2mm/h；
When crystal growth to diameter is 60~100mm, stopping is lifted up shadoof, makes pulling rate 0, while controlling power decline,
The range of decrease is 20~80W/h；
When the crystal weight reaches the 8~15% of charge, by control power decline, the range of decrease is 10~80W/h, makes crystal
Speed of growth < 2kg/h；
When the crystal weight is the 80~95% of charge, it is lifted up shadoof, makes pulling rate up to 0.5~3mm/h, works as crystal
When weight is without fluctuation and close to charge, 10~20h of state is maintained；
So that power is at the uniform velocity down to 0 in 100~180h, obtains signle crystal alumina crystal ingot；
Bubble-free, free from admixture, dislocation-free crystal ingot part in the signle crystal alumina crystal ingot are cut into and hold burning device.
3. preparation method as claimed in claim 2, which is characterized in that the seed crystal is rectangular or round α-Al2O3Monocrystalline, length
For 150mm~200mm, wide or diameter is 15~25mm, seed crystal roughness Ra≤0.8 μm.
4. preparation method as claimed in claim 2, it is characterised in that the crucible is tungsten crucible or molybdenum crucible or tungsten-molybdenum alloy earthenware
Crucible.
5. preparation method as claimed in claim 2, which is characterized in that if liquid level goes out during before seed crystal contact liquid level
Crystalline substance is now floated, power is improved；Decentralization seed crystal and molten soup welding when floating brilliant disappearance, liquid level stabilizing.
6. preparation method as claimed in claim 2, which is characterized in that the stopping decentralization seed crystal to the crystal growth to diameter
During for 60~100mm, every 1~10min wink mentions 0.5~2mm, mentions altogether 20~50 times.
7. preparation method as claimed in claim 2, which is characterized in that the wink when crystal weight reaches the 8~15% of charge
2~5mm is mentioned, power is improved into 300~800W.
8. preparation method as claimed in claim 2, which is characterized in that method used in the cutting is diamond cut.
9. preparation method as claimed in claim 2, which is characterized in that the flawless crystal ingot is cut into plate, saggar shape
Or abnormity hold burning device.
10. preparation method as claimed in claim 2, which is characterized in that the burning device that holds is placed in annealing furnace, is evacuated to
So that in-furnace temperature is risen to 1300~1600 DEG C in 1e-4pa, 20~30h, 20~36h of this temperature is maintained, then in 65~75h
Heater power is uniformly down to 0, is cooled to room temperature.
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