CN108239789A - A kind of heat treatment process of large-size sapphire optical crystal - Google Patents
A kind of heat treatment process of large-size sapphire optical crystal Download PDFInfo
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- CN108239789A CN108239789A CN201810275048.1A CN201810275048A CN108239789A CN 108239789 A CN108239789 A CN 108239789A CN 201810275048 A CN201810275048 A CN 201810275048A CN 108239789 A CN108239789 A CN 108239789A
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- temperature
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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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- 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
Abstract
The present invention discloses a kind of heat treatment process of large-size sapphire optical crystal, belongs to crystalline material manufacture field：After large-size sapphire blank carries out superfine grinding or the mechanical processings such as single-sided polishing grinding and twin polishing grinding, its surface can generate residual stress, the present invention is using the six heating rate stages and four cooling rate stages for including annealing and drawing process so that large-size sapphire is heated evenly, internal difference in temperature is small, can effectively reduce the residual stress of sapphire surface；And step heat preservation different time can reduce the dislocation density of large-size sapphire, help to improve the integrality of sapphire surface, so as to promote sapphire total quality.
Description
Technical field
The present invention relates to the processing technique field of crystalline material, at the heat of particularly a kind of large-size sapphire optical crystal
Science and engineering skill.
Background technology
Sapphire crystal is because of its unique crystal structure, excellent mechanical performance, dielectric properties, chemical stability and height
Surface smoothness as a kind of important functional material, plays an important role, such as in the fields such as substrate material and laser technology
Using lattice integrity degree is high, suface processing quality is excellent sapphire crystal as the GaN base LED of substrate, laser diode and big
Scale integrated circuit；It mixes the sapphire uniquenesses of Ti and is embodied in it in addition to amplifying spectrum with roomy wave band, femtosecond can be obtained
Other than pulse, there is big induction excitation section.Meanwhile as a kind of important structural material, national defence has been widely used in it
Industry and civil field particularly have irreplaceable status and work in fields such as military affairs, aerospace, high-grade daily necessities
With the middle infrared window and radome fairing being such as prepared by sapphire crystal, it has also become airborne, spaceborne, carrier-borne and latent base, land
Base optoelectronic device, especially in High Mach number guided missile dome；Sapphire crystal can be used for making medical operation apparatus, precision machinery
Bearing and clock and watch watchcase, jewellery and various cup vessel, Transparent lamp set and screening glass.
As sapphire application is more and more extensive, a large amount of small size sapphire is not only needed, to large-sized blue precious
Stone demand is also higher and higher, and either sapphire is carried out at superfine grinding, single side grinding and polishing and Two sides milling and polishing
Reason can all cause sapphire surface to generate residual stress, and the residual stress of small size sapphire surface is easy to by annealing
Control, but large-size sapphire is easy to since volume is bigger, in annealing process due to heating, cooling speed and heat preservation
The remnants that time control is bad and sapphire surface generation is caused to rupture or can not be effectively reduced sapphire surface are answered
Power.The problem of for being susceptible in above-mentioned annealing process, the invention discloses a kind of heat of large-size sapphire optical crystal
Treatment process can effectively reduce the residual stress on large-size sapphire surface, improve sapphire crystal block quality.
Invention content
The main object of the present invention is to be to provide a kind of heat treatment process processing side of large-size sapphire optical crystal
Method, can be to avoid for large-size sapphire crystal block after the processing of superfine grinding, single side grinding and polishing and Two sides milling and polishing
Sapphire surface is cracked because uneven heating is even in annealing process, and the remnants that can effectively reduce sapphire surface should
Power improves crystal quality.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
A kind of heat treatment process of large-size sapphire optical crystal, to superfine grinding, single side grinding and polishing and double
Large-size sapphire crystal block, which make annealing treatment, after the grinding and polishing processing of face includes following ten stages；
First stage：Temperature is heated up in -200 DEG C of room temperature with 3 DEG C/min speed.
Second stage：Temperature is heated up at 200 DEG C -1100 DEG C with 4 DEG C/min speed.
Phase III：Temperature is heated up with 3 DEG C/min speed, is protected when being increased to 1300 DEG C at 1100 DEG C -1300 DEG C
Warm 60min.
Fourth stage：Temperature is heated up at 1300 DEG C -1500 DEG C with 1-2 DEG C/min speed.
5th stage：Temperature is heated up at 1500 DEG C -1550 DEG C with 1-2 DEG C/min speed.When being increased to 1550 DEG C
Keep the temperature 300min.
6th stage：Temperature is cooled down at 1550 DEG C -1400 DEG C with 1-2 DEG C/min speed.When cooling to 1400 DEG C
Keep the temperature 60min.
7th stage：Temperature from 1400 DEG C -1500 DEG C when, heated up with 1-2 DEG C/min speed.When being warming up to 1500 DEG C
Keep the temperature 120min.
8th stage：Temperature is cooled down from when dropping to 1300 DEG C for 1500 DEG C with 1-2 DEG C/min speed.
9th stage：Temperature is cooled down from when dropping to 1000 DEG C for 1300 DEG C with 4 DEG C/min speed.
Tenth stage：Temperature is from 1000 DEG C of Temperature falls to room temperature.
In the technical program, the heating rate, the cooling of four cooling temperature sections there is provided six warming temperature sections are fast
Degree and four holding stages, comprising annealing process and drawing process, can effectively reduce large size sapphire crystal surface
Residual stress, prevent from cracking because uneven heating is even, improve crystal quality.
A kind of heat treatment process of above-mentioned large-size sapphire optical crystal, wherein, annealing workpiece for superfine grinding,
The sapphire crystal block of single side grinding and polishing and Two sides milling and polishing.
A kind of heat treatment process of above-mentioned large-size sapphire optical crystal, wherein, heat treatment process includes annealing rank
Section and tempering stage.
A kind of heat treatment process of above-mentioned large-size sapphire optical crystal, wherein, the lifting of eight stage of fourth stage-the
Temperature, speed are no more than 1-2 DEG C/min.
A kind of heat treatment process of above-mentioned large-size sapphire optical crystal, wherein, the heat-treating atmosphere is lazy
Property gas, preferably argon gas.
A kind of heat treatment process of above-mentioned large-size sapphire optical crystal, wherein, the tenth section of temperature drops to 1000 DEG C
It is by cooling rate set to zero, cooled to room temperature to continue temperature-fall period later.
The method have the advantages that：The process of will heat up is divided into six temperature sections, controls the heating speed of each temperature section
Degree, is divided into four temperature sections by temperature-fall period, controls the cooling rate of each temperature section, so as to make sapphire in whole process
It is heated evenly, prevents sapphire surface from generating rupture, the residual stress of sapphire surface can be efficiently reduced；And ten ranks
Section includes annealing and is tempered two processes, and the purpose that tempering is set in annealing process is not only through heating and heat preservation of annealing
Mode accelerates surface layer atom and dislocation to transport to rebuild lattice surface structure by tempering cooling insulating process collective effect
Dynamic, dislocation and blocky boundary defect rearrangement discharge focused energy, make the reduction of damaging layer surface free energy, and skin-material is extensive
Multiple low-energy state so that lattice surface is more complete, so as to improve the total quality of crystal.
Description of the drawings
Fig. 1 is the graph of relation that processing time and temperature are answered in hot repair
Specific embodiment
A kind of heat treatment process processing method of large-size sapphire optical crystal, with reference to specific embodiment pair
The present invention is further described：
Large-size sapphire crystal block after the processing of superfine grinding, single side grinding and polishing or Two sides milling and polishing is put into interior go
In ionized water, with ultrasonic cleaning 15min, dried up and be put into heat-treatment furnace with air gun；
First stage：Temperature is heated up in -200 DEG C of room temperature with 3 DEG C/min speed.
Second stage：Temperature is heated up at 200 DEG C -1100 DEG C with 4 DEG C/min speed.
Phase III：Temperature is heated up with 3 DEG C/min speed, is protected when being increased to 1300 DEG C at 1100 DEG C -1300 DEG C
Warm 60min.
Fourth stage：Temperature is heated up at 1300 DEG C -1500 DEG C with 2 DEG C/min speed.
5th stage：Temperature is heated up at 1500 DEG C -1550 DEG C with 1 DEG C/min speed.It is protected when being increased to 1550 DEG C
Warm 300min.
6th stage：Temperature is cooled down at 1550 DEG C -1400 DEG C with 2 DEG C/min speed.It is protected when cooling to 1400 DEG C
Warm 60min.
7th stage：Temperature from 1400 DEG C -1500 DEG C when, heated up with 1 DEG C/min speed.It is protected when being warming up to 1500 DEG C
Warm 120min.
8th stage：Temperature is cooled down from when dropping to 1300 DEG C for 1500 DEG C with 2 DEG C/min speed.
9th stage：Temperature is cooled down from when dropping to 1000 DEG C for 1300 DEG C with 4 DEG C/min speed.
Tenth stage：Temperature takes out sapphire from 1000 DEG C of Temperature falls to room temperature.
Claims (5)
1. a kind of heat treatment process of large-size sapphire optical crystal, it is characterized in that, to by superfine grinding, grinding, throwing
Large-size sapphire crystal block is heat-treated after light, and heating, cooling process is divided into ten stages, until temperature is down to room temperature；
First stage：Temperature is heated up in -200 DEG C of room temperature with 3 DEG C/min speed；
Second stage：Temperature is heated up at 200 DEG C -1100 DEG C with 4 DEG C/min speed；
Phase III：Temperature is heated up with 3 DEG C/min speed, is kept the temperature when being increased to 1300 DEG C at 1100 DEG C -1300 DEG C
60min；
Fourth stage：Temperature is heated up at 1300 DEG C -1500 DEG C with 1-2 DEG C/min speed；
5th stage：Temperature is heated up at 1500 DEG C -1550 DEG C with 1-2 DEG C/min speed.It is kept the temperature when being increased to 1550 DEG C
300min；
6th stage：Temperature is cooled down at 1550 DEG C -1400 DEG C with 1-2 DEG C/min speed.It is kept the temperature when cooling to 1400 DEG C
60min；
7th stage：Temperature from 1400 DEG C -1500 DEG C when, heated up with 1-2 DEG C/min speed.It is kept the temperature when being warming up to 1500 DEG C
120min；
8th stage：Temperature is cooled down from when dropping to 1300 DEG C for 1500 DEG C with 1-2 DEG C/min speed；
9th stage：Temperature is cooled down from when dropping to 1000 DEG C for 1300 DEG C with 4 DEG C/min speed；
Tenth stage：Temperature is from 1000 DEG C of Temperature falls to room temperature.
2. the heat treatment process of a kind of large-size sapphire optical crystal according to claim 1, which is characterized in that at heat
Science and engineering part is superfine grinding or the sapphire crystal block of single side grinding and polishing and Two sides milling and polishing.
3. the heat treatment process of a kind of large-size sapphire optical crystal according to claim 1, which is characterized in that at heat
Reason process includes annealing stage and tempering stage.
4. the heat treatment process of a kind of large-size sapphire optical crystal according to claim 1, which is characterized in that described
Heat-treating atmosphere for inert gas, preferred argon gas.
5. the heat treatment process of a kind of large-size sapphire optical crystal according to claim 1, which is characterized in that the tenth
It is by cooling rate set to zero, cooled to room temperature that Duan Wendu continues temperature-fall period after dropping to 1000 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110528076A (en) * | 2019-10-08 | 2019-12-03 | 四川大学 | A kind of sapphire and graphene doping generate sapphire method |
| CN110744732A (en) * | 2019-09-03 | 2020-02-04 | 福建晶安光电有限公司 | Manufacturing process of high-performance substrate |
| CN111155173A (en) * | 2018-11-07 | 2020-05-15 | 中科钢研节能科技有限公司 | Sapphire and annealing method of sapphire crystal |
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| JP2015182944A (en) * | 2014-03-26 | 2015-10-22 | 住友金属鉱山株式会社 | Production method of sapphire single crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155173A (en) * | 2018-11-07 | 2020-05-15 | 中科钢研节能科技有限公司 | Sapphire and annealing method of sapphire crystal |
| CN111155173B (en) * | 2018-11-07 | 2021-07-23 | 国宏中晶集团有限公司 | Sapphire and annealing method of sapphire crystal |
| CN110744732A (en) * | 2019-09-03 | 2020-02-04 | 福建晶安光电有限公司 | Manufacturing process of high-performance substrate |
| CN110744732B (en) * | 2019-09-03 | 2022-04-15 | 福建晶安光电有限公司 | Manufacturing process of high-performance substrate |
| CN110528076A (en) * | 2019-10-08 | 2019-12-03 | 四川大学 | A kind of sapphire and graphene doping generate sapphire method |
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Application publication date: 20180703 |
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