CN105862128B - A kind of preparation method of normal-temperature high-strength mechanical property aluminum oxide wafer for being suitable for screen material and its obtained product - Google Patents
A kind of preparation method of normal-temperature high-strength mechanical property aluminum oxide wafer for being suitable for screen material and its obtained product Download PDFInfo
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- CN105862128B CN105862128B CN201610385336.3A CN201610385336A CN105862128B CN 105862128 B CN105862128 B CN 105862128B CN 201610385336 A CN201610385336 A CN 201610385336A CN 105862128 B CN105862128 B CN 105862128B
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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
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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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention is a kind of preparation method of normal-temperature high-strength mechanical property aluminum oxide wafer for being suitable for screen material and its obtained product, and using kyropoulos technology, the uniform Al of dopant profile is prepared first with atmosphere doping of the graphite stay-warm case under elevated temperature in vacuo2O3:C crystal；Then, by the Al of growth2O3:The cleaved polishing of C crystal is into Al2O3:After C chips, Al is realized using the annealing of special process2O3:The Strengthening and Toughening of C chips.Be made aluminum oxide wafer under normal temperature condition four-point bending intensity up to 2000Mpa and more than, 380~2500nm wide range domain transmitance up to 82%, be applicable to high-end screen material.Process of the present invention has the advantages of technique is simple, green, energy-saving, therefore has significant economic benefit.
Description
Technical field
The invention belongs to transparent optical material manufacturing technology field, and in particular to a kind of normal temperature for being suitable for screen material is high
The preparation method of strong mechanical property aluminum oxide wafer and its obtained product.
Background technology
Aluminum oxide wafer is because of its excellent anti-wear performance, corrosion resistance, high temperature resistant, wide range domain high-permeability energy, Yi Jiyuan
Expect asepsis environment-protecting, abundance, the advantages such as physical and chemical performance is stable, be widely used for dome material, optical window material and
The critical material of the modern national defenses such as high-end screen material and civilian technology apparatus field.
However, the defects of aluminum oxide wafer maximum, is that the flexural strength of chip is not high and fracture toughness is very low, not
Through under disposition, the flexural strength of aluminum oxide wafer even not as good as the intensity of safety glass, fracture toughness is only 1.8~
2MPa·m1/2, the defects of these mechanics flexural strengths are not high and fracture toughness is extremely low is always to restrict aluminum oxide wafer to enter one
Step development and the bottleneck of application.The report of presently disclosed aluminum oxide wafer Strengthening and Toughening is mainly that three aspects are studied：1）Surface
The research of Ion Implantation Strengthening；2）Surface the second phase approach Investigation on intensification；3）The research that ion doping is strengthened；These disclosed opinions
Text report, the defects of in the majority and deficiency in application process also be present, and these papers report majority is oxygen under hot conditions
Change the Investigation on intensification of aluminium chip, and under normal temperature application conditions, the research to the Strengthening and Toughening of aluminum oxide wafer is rarely reported, research
It is adapted to the process urgent need to resolve of aluminum oxide wafer Strengthening and Toughening under normal temperature.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of technique it is simple, green, energy-saving be suitable for shielding
The preparation method of the normal-temperature high-strength mechanical property aluminum oxide wafer of curtain material and its obtained product.
The present invention is achieved by the following technical programs：A kind of normal-temperature high-strength mechanical property oxygen for being suitable for screen material
Change the preparation method of aluminium chip, it is characterised in that comprise the following steps：
Step 1：Al is prepared using kyropoulos technology2O3:C crystal, adulterated by graphite atmosphere to grow to obtain dopant profile
Uniform Al2O3:C crystal；
Step 2：By Al made from step 12O3:The cleaved polishing of C crystal is into Al2O3:After C chips, at annealing
Science and engineering skill, realizes Al2O3:The normal temperature Strengthening and Toughening of C chips.
Kyropoulos prepare Al in the step 12O3:The concrete technology step of C crystal includes：
Step 1.1：Crystal growth raw material is put into tungsten and molybdenum crucible, Kyropoulos furnace uses tungsten cage heater, and liner stay-warm case is adopted
With graphite material, 1~10 × 10 are evacuated to-4Pa, persistently overheating to 2100~2150 DEG C, constant temperature is complete to raw material after 4~8 hours
It is complete to melt；
Step 1.2：Temperature is adjusted to 2050 DEG C of fusing points and is nearby gradually reduced seed crystal, seed crystal end is at 10~20mm of liquid level
Rotated with 1~10 rev/min of speed, seeding after preheating 10~60 minutes；Output voltage is adjusted to drop with 0.1~1 DEG C/h speed
Temperature, while seed crystal is lifted with 0.05~2mm/h speed, the now isometrical bubble growth of crystal, until crystal mass reaches raw material matter
Amount, Al2O3:Prepared by C crystal terminates.
The concrete technology step of annealing treating process in the step 2 includes：
The high fiery insulation annealing of step 2.1：Annealing furnace is evacuated to 1~10 × 10-4Pa, it is persistently overheating to 1700~1900
DEG C, Al is taken in insulation 4~8h annealings, realization apart2O3The dislocation solid matter cable architecture that chip is formed during melt method for growing；
Step 2.2 moderate heat fast cooling is annealed：Adjust parameter and annealing, be filled with the air pressure of hydrogen atmosphere for 1atm+1~
5Kpa, from high fiery 1700~1900 DEG C of moderate heat temperature with 30~120 DEG C/h speed slow cooling to 1400~1600 DEG C of temperature
Afterwards, with 180~600 DEG C/h fast coolings, realize and improve and regulate and control Al2O3Dislocation density in lattice；
The low fiery long-time heat preservation annealing of step 2.3：Parameter and annealing is adjusted again, it is fast from the moderate heat temperature of second stage
Speed is cooled to 1000~1200 DEG C of low fiery temperature, is incubated 8~16h, at the same keep the air pressure of hydrogen atmosphere for 1atm+1~
5Kpa, realize Al2O3:C chips accumulate the release of thermal stress, then with 30~120 DEG C/h slow coolings to room temperature, complete annealing
Handling process.
Growth raw material in the step 1.1 is the Al that purity is 99.999%2O3Crystal block material or sintering feed, liner stay-warm case
The high purity graphite material for being 99.9% for purity.
Seed crystal in the step 1.2 is the aluminum oxide list in [11-20] or [10-10] or [1-102] or [0001] direction
Crystalline substance, Al is made2O3:The carbon dope amount of C crystal is 100~1000ppm.
Al made from above-mentioned preparation method2O3:C chips, it is characterised in that：The Al2O3:It is crisp in the absence of causing in C chips
Property cracking dislocation solid matter cable architecture.
Al made from above-mentioned preparation method2O3:C chips, it is characterised in that：The Al2O3:C chips Dislocations are in detached island
Shape disperses, and dislocation density is up to 0.5~5.0 × 104/cm2。
Al made from above-mentioned preparation method2O3:C chips, it is characterised in that：The Al2O3:Lower 4 points of C chip normal temperature conditions
Bending strength up to 2000MPa and more than, and 380~2500nm wide ranges domain transmitance up to 82%.
Al made from above-mentioned preparation method2O3:C chips, it is characterised in that：The Al2O3:C chips can be applied to high-end screen
Curtain material.
The present invention prepares Al using kyropoulos technology first2O3:C crystal, using high purity graphite stay-warm case in high-temperature vacuum bar
Atmosphere doping under part prepares the uniform Al of dopant profile2O3:C crystal；Then, kyropoulos Al2O3:The cleaved polishing of C crystal adds
Work is into Al2O3:After C chips, Al is realized using the annealing of special process2O3:The Strengthening and Toughening of C chips：Pass through first stage height
Fiery insulation annealing, reaches and takes Al apart2O3:The dislocation solid matter cable architecture formed in C chips during melt method for growing（Class is intrinsic
Defect）, annealed by second stage moderate heat fast cooling, reality improves and regulates and controls Al2O3:The purpose of C chip middle position dislocation densities,
Annealed by phase III low fiery long-time heat preservation, promote Al2O3:The release of thermal stress is accumulated in C chips.This final annealing
The Al that PROCESS FOR TREATMENT obtains2O3:C chips, under normal temperature condition, four-point bending intensity up to 2000Mpa and more than, and 380~
The transmitance in 2500nm wide ranges domain is applied to high-end aluminum oxide wafer screen material up to 82%, has wide market empty
Between.
Brief description of the drawings
Fig. 1 is the Al of embodiment 12O3:The through performance of C chip visible-near-infrared spectrums；
Fig. 2 is the Al of embodiment 12O3:The typical cleavage tear type looks of C chip four-point bending fracture cracks；
Fig. 3 is the Al of embodiment 12O3:C chip Dislocation Morphology features.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Preferred embodiment, the present invention is described in detail：
Embodiment 1：
（1）Step 1：Al is prepared using kyropoulos technology2O3:C crystal, adulterated by graphite atmosphere to grow to obtain admixture
The Al being evenly distributed2O3:C crystal, specific steps include：
Step 1.1：The aluminum oxide crystal block material that 30kg purity is 99.999% is loaded into tungsten and molybdenum crucible, liner stay-warm case is selected
Purity is 99.9% graphite material, is evacuated to 3.0 × 10-4Pa, persistently overheating to 2100 DEG C, constant temperature 6 hours is complete to raw material
Melt;
Step 1.2：Temperature is adjusted to 2050 DEG C of fusing points and is nearby gradually reduced seed crystal, seed crystal end sentences 8 in liquid level 12mm
Rev/min speed rotates, seeding after preheating 20 minutes；Output voltage is adjusted with 0.3 DEG C/h speed to cool, while with 0.1~
1mm/h speed lifting seed crystal, the now isometrical bubble growth of crystal, until crystal mass reaches material quality, Al2O3:C crystal
Growth terminates;
（2）Step 2：Kyropoulos Al2O3:The cleaved polishing of C crystal is into Al2O3:After C chips, using specific annealing
Handling process, realize Al2O3:The normal temperature Strengthening and Toughening of C chips, specific steps include：
The high fiery insulation annealing of step 2.1:Annealing furnace is evacuated to 5.0 × 10-4Pa, persistently overheating to 1800 DEG C, insulation
6h is made annealing treatment, and Al is taken apart to realize2O3The dislocation solid matter cable architecture that chip is formed during melt method for growing（Class is intrinsic to be lacked
Fall into）, it is to solve to restrict Al2O3:The basis of C chip mechanical properties；
Step 2.2 moderate heat fast cooling is annealed:Parameter and annealing is adjusted, the air pressure for being filled with hydrogen atmosphere is 1atm+
2.1Kpa, it is quick with 240 DEG C/h after high fiery 1800 DEG C of moderate heat temperature with 30 DEG C/h speed slow cooling to 1500 DEG C of temperature
Cooling.Realize and improve and regulate and control Al2O3Lattice dislocation density, it is further raising Al2O3The key of chip mechanical property；
The low fiery long-time heat preservation annealing of step 2.3:Parameter and annealing is adjusted again, it is fast in the moderate heat temperature of second stage
Speed is cooled to 1200 DEG C of low fiery temperature, is incubated 10h, while it is 1atm+2.1Kpa to keep the air pressure of hydrogen atmosphere.Realize
Al2O3:C chips accumulate the release of thermal stress（The thermal stress of main release second stage fast cooling accumulation）, then 60 DEG C/h delay
It is slow to be cooled to room temperature, complete annealing Strengthening and Toughening and handle whole technical process, finally give the normal-temperature high-strength mechanical property of annealing
The Al of energy2O3:C chips.
By Al made from embodiment 12O3:C chips, it is processed into detection sample（The processing dimension and surface finish of sample
For：120mm×55.7mm×0.6mm；Surface roughness 0.4nm, edge roughness 70nm, bevelling 0.1mm × 45 °, 4 points of sample
Bending strength test result is 2076.5MPa；Fig. 1 is Al prepared by embodiment 12O3:The transmission of C chip visible-near-infrared spectrums
The performance test results, show Al2O3:C chips 380~2500nm wide ranges domain transmitance up to 82%；Fig. 2 is prepared by embodiment 1
Al2O3:C chip four-point bending scission fragments and fracture crack analysis, show that it is broken pattern and is characterized as that typical cleavage is broken
Split；Fig. 3 is Al prepared by embodiment 12O3:C chips carry out Dislocation Morphology analysis, show that its Dislocation Morphology is characterized as isolated island
Shape uniform distribution features, almost without dislocation solid matter cable architecture, dislocation density is 1.9 × 104/cm2。
Embodiment 2
（1）Step 1：Al is prepared using kyropoulos technology2O3:C crystal, adulterated by graphite atmosphere to grow to obtain admixture
The Al being evenly distributed2O3:C crystal, specific steps include：
Step 1.1：The aluminum oxide crystal block material that 30Kg purity is 99.999% is loaded into tungsten and molybdenum crucible, liner stay-warm case is selected
Purity is 99.9% graphite material, is evacuated to 5.0 × 10-4Pa, persistently overheating to 2150 DEG C, constant temperature 4 hours is complete to raw material
Melt；
Step 1.2：Temperature is adjusted to 2050 DEG C of fusing points and is nearby gradually reduced seed crystal, seed crystal end sentences 4 in liquid level 17mm
Rev/min speed rotates, seeding after preheating 50 minutes；Output voltage is adjusted with 0.5 DEG C/h speed to cool, while with 0.15~
1.5mm/h speed lifting seed crystal, the now isometrical bubble growth of crystal, until crystal mass reaches material quality, Al2O3:C is brilliant
Body growth terminates；
（2）Step 2：Kyropoulos Al2O3:The cleaved polishing of C crystal is into Al2O3:After C chips, using specific annealing
Handling process, realize Al2O3:The normal temperature Strengthening and Toughening of C chips.Specific steps include：
The high fiery insulation annealing of step 2.1：Annealing furnace is evacuated to 6.0 × 10-4Pa, persistently overheating to 1750 DEG C, insulation
6.5h is made annealing treatment, and Al is taken apart to realize2O3The dislocation solid matter cable architecture that chip is formed during melt method for growing（Class is intrinsic
Defect）, it is to solve to restrict Al2O3:The basis of C chip mechanical properties；
Step 2.2 moderate heat fast cooling is annealed：Parameter and annealing is adjusted, the air pressure for being filled with hydrogen atmosphere is 1atm+
1.8Kpa, it is quick with 360 DEG C/h after high fiery 1750 DEG C of moderate heat temperature with 60 DEG C/h speed slow cooling to 1450 DEG C of temperature
Cooling.Realize and improve and regulate and control Al2O3Lattice dislocation density, it is further raising Al2O3The key of chip mechanical property；
The low fiery long-time heat preservation annealing of step 2.3：Parameter and annealing is adjusted again, it is fast in the moderate heat temperature of second stage
Speed is cooled to 1150 DEG C of low fiery temperature, is incubated 12h, while it is 1atm+1.8Kpa to keep the air pressure of hydrogen atmosphere.Realize
Al2O3:C chips accumulate the release of thermal stress（The thermal stress of main release second stage fast cooling accumulation）, then 80 DEG C/h delay
It is slow to be cooled to room temperature, complete annealing Strengthening and Toughening and handle whole technical process, finally give the normal-temperature high-strength mechanical property of annealing
The Al of energy2O3:C chips.
By Al made from embodiment 22O3:C chips, it is processed into detection sample（The processing dimension and surface finish of sample
For：120mm×55.7mm×0.6mm；Surface roughness 0.4nm, edge roughness 70nm, bevelling 0.1mm × 45 °, its 4 points curved
Qu Qiangdu reaches 2103.6MPa, and dislocation density is 2.1 × 104/cm2, 380~2500nm wide ranges domain transmitance up to 82%.
Claims (8)
- A kind of 1. preparation method for the normal-temperature high-strength mechanical property aluminum oxide wafer for being suitable for screen material, it is characterised in that including Following steps：Step 1：Al is prepared using kyropoulos technology2O3:C crystal, adulterated by graphite atmosphere uniform to grow to obtain dopant profile Al2O3:C crystal；Step 2：By Al made from step 12O3:The cleaved polishing of C crystal is into Al2O3:After C chips, using annealing work Skill, realize Al2O3:The normal temperature Strengthening and Toughening of C chips；The concrete technology step of annealing treating process in the step 2 includes：The high fiery insulation annealing of step 2.1：Annealing furnace is evacuated to 1~10 × 10-4Pa, persistently overheating to 1700~1900 DEG C, 4~8h annealings are incubated, Al is taken in realization apart2O3The dislocation solid matter cable architecture that chip is formed during melt method for growing；Step 2.2 moderate heat fast cooling is annealed：Adjust parameter and annealing, be filled with the air pressure of hydrogen atmosphere for 1atm+1~ 5kPa, from high fiery 1700~1900 DEG C of moderate heat temperature with 30~120 DEG C/h speed slow cooling to 1400~1600 DEG C of temperature Afterwards, with 180~600 DEG C/h fast coolings, realize and improve and regulate and control Al2O3Dislocation density in lattice；The low fiery long-time heat preservation annealing of step 2.3：Parameter and annealing is adjusted again, from the fast prompt drop of moderate heat temperature of second stage Temperature is incubated 8~16h to 1000~1200 DEG C of low fiery temperature, while it be 1atm+1~5kPa to keep the air pressure of hydrogen atmosphere, reality Existing Al2O3:C chips accumulate the release of thermal stress, then with 30~120 DEG C/h slow coolings to room temperature, complete annealing work Skill.
- 2. preparation method according to claim 1, it is characterised in that：Kyropoulos prepare Al in the step 12O3:C crystal Concrete technology step include：Step 1.1：Crystal growth raw material is put into tungsten and molybdenum crucible, Kyropoulos furnace uses tungsten cage heater, and liner stay-warm case uses stone Ink material, it is evacuated to 1~10 × 10-4Pa, persistently overheating to 2100~2150 DEG C, constant temperature melts completely after 4~8 hours to raw material Change；Step 1.2：Temperature is adjusted to 2050 DEG C of fusing points and is nearby gradually reduced seed crystal, seed crystal end sentences 1 in 10~20mm of liquid level ~10 revs/min of speed rotate, seeding after preheating 10~60 minutes；Output voltage is adjusted with 0.1~1 DEG C/h speed to cool, Seed crystal is lifted with 0.05~2mm/h speed simultaneously, now the isometrical bubble growth of crystal, until crystal mass reaches material quality, Al2O3:Prepared by C crystal terminates.
- 3. preparation method according to claim 2, it is characterised in that：Growth raw material in the step 1.1 is that purity is 99.999% Al2O3Crystal block material or sintering feed, liner stay-warm case are the high purity graphite material that purity is 99.9%.
- 4. preparation method according to claim 2, it is characterised in that：Seed crystal in the step 1.2 for [11-20] or [10-10] or [1-102] or the alumina single crystal in [0001] direction, Al is made2O3:The carbon dope amount of C crystal be 100~ 1000ppm。
- 5. according to Al made from any preparation methods of claim 1-42O3:C chips, it is characterised in that：The Al2O3:C is brilliant The dislocation solid matter cable architecture for causing brittle cracking is not present in piece.
- 6. according to Al made from any preparation methods of claim 1-42O3:C chips, it is characterised in that：The Al2O3:C is brilliant Piece Dislocations are in that isolated island disperses, and dislocation density is up to 0.5~5.0 × 104/cm2。
- 7. according to Al made from any preparation methods of claim 1-42O3:C chips, it is characterised in that：The Al2O3:C is brilliant Under piece normal temperature condition four-point bending intensity up to 2000MPa and more than, and 380~2500nm wide ranges domain transmitance up to 82%.
- 8. according to Al made from any preparation methods of claim 1-42O3:C chips, it is characterised in that：The Al2O3:C is brilliant Piece can be applied to high-end screen material.
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| JPH05186297A (en) * | 1992-01-08 | 1993-07-27 | Tosoh Corp | Production of high-grade single crystal of titanium sapphire |
| CN100575566C (en) * | 2007-12-28 | 2009-12-30 | 中国科学院上海光学精密机械研究所 | The method of growing method of carbon-doped sapphire crystal by EFG |
| CN102703970A (en) * | 2012-07-11 | 2012-10-03 | 浙江特锐新能源有限公司 | Kyropous method growth of titanium doped sapphire crystals |
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