CN116427017A - Laser heating base method for growing Al 2 O 3 Method for producing YAG eutectic optical fiber - Google Patents
Laser heating base method for growing Al 2 O 3 Method for producing YAG eutectic optical fiber Download PDFInfo
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- CN116427017A CN116427017A CN202310124557.5A CN202310124557A CN116427017A CN 116427017 A CN116427017 A CN 116427017A CN 202310124557 A CN202310124557 A CN 202310124557A CN 116427017 A CN116427017 A CN 116427017A
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- 230000005496 eutectics Effects 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 52
- 229910018072 Al 2 O 3 Inorganic materials 0.000 title claims abstract description 38
- 238000004093 laser heating Methods 0.000 title claims abstract description 26
- 239000013307 optical fiber Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000013078 crystal Substances 0.000 claims abstract description 72
- 239000000835 fiber Substances 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 239000003570 air Substances 0.000 claims description 6
- 229910003460 diamond Inorganic materials 0.000 claims description 5
- 239000010432 diamond Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 description 10
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000010587 phase diagram Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000003280 down draw process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
-
- 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
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
- 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
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
Abstract
The invention relates to a laser heating base method for growing Al 2 O 3 -a method of YAG eutectic optical fiber comprising: (1) Al is added with 2 O 3 The crystal and YAG crystal are cut into long strips of Al 2 O 3 And the long-strip YAG are combined into a whole to be used as a source rod and fixed on a laser heating base feeding device; (2) Al is added with 2 O 3 The seed crystal or YAG seed crystal is fixed on the laser heating base lifting device; (3) Al by laser heating of the susceptor 2 O 3 -growth of YAG eutectic fiber.
Description
Technical Field
The invention relates to a laser heating base method for growing Al 2 O 3 Method for YAG eutectic optical fiber, in particular to a method for directly growing Al from crystal 2 O 3 A method for YAG eutectic optical fiber, which belongs to the technical field of crystal growth and devices.
Background
Compared with Al 2 O 3 Single crystal and YAG single crystal, al 2 O 3 The YAG eutectic ceramic material has an irregular network eutectic structure, has mechanical properties close to room temperature at high temperature, is a typical aluminum oxide-based binary eutectic system, has higher strength, excellent thermal shock resistance and excellent high-temperature creep resistance, and is considered as one of candidate materials for long-term operation in an ultra-high-temperature strong-oxidizing environment. At present, al is prepared 2 O 3 The method of YAG eutectic ceramic material mainly comprises sintering method, bridgman method, boundary epitaxial growth method, micro-downdraw method, laser zone melting method, etc.
However, the existing preparation methods (sintering method, bridgman method, boundary epitaxial growth method, micro-downdraw method, laser zone melting method, etc.) are all to make Al 2 O 3 Powder and Y 2 O 3 The powder is mixed in a certain proportion and then melted to grow eutectic. The eutectic morphology is changed by changing the growth conditions such as growth atmosphere, growth speed and the like. In addition, the mixing process needs to strictly follow Al in the phase diagram 2 O 3 -Y 2 O 3 The eutectic formation point is dosed to prevent the occurrence of other phases, so that it is difficult to adjust the eutectic morphology to a large extent.
Disclosure of Invention
To solve the existing Al 2 O 3 Preparation of YAG eutectic optical fiber composite materialIn the process, when powder is used as raw material, defects such as pollution, cracks and the like possibly exist, and Al in eutectic is difficult to change 2 O 3 And Y is equal to 2 O 3 The invention provides a method for growing Al by a laser heating base method 2 O 3 -a method of YAG eutectic optical fiber comprising:
(1) Al is added with 2 O 3 The crystal and YAG crystal are cut into long strips of Al 2 O 3 And the long-strip YAG are combined into a whole to be used as a source rod and fixed on a laser heating base feeding device;
(2) Al is added with 2 O 3 The seed crystal or YAG seed crystal is fixed on the laser heating base lifting device;
(3) Al by laser heating of the susceptor 2 O 3 -growth of YAG eutectic fiber.
The invention provides a method for directly growing Al from crystal 2 O 3 The method of YAG single crystal optical fiber composite material, firstly, proposes to grow eutectic optical fiber by using crystal as raw material. By the technique, al which has no obvious crack and is uniformly distributed can be obtained 2 O 3 YAG eutectic optical fiber composite material improves the uniformity and crystallinity of the eutectic optical fiber.
Preferably, in step (1), the Al is in the form of long strips prior to combination 2 O 3 Polishing and cleaning one side of the long length multiplied by the width of the long-strip YAG;
the polishing is carried out for 10-20 min by utilizing diamond grinding paste with the granularity number of W5-W16;
the cleaning is ultrasonic cleaning, preferably ultrasonic cleaning for 10-20 min under the power of 60-120W.
Preferably, in the step (1), the elongated Al 2 O 3 The length of the steel is 10-100 mm, the width is 0.5-2 mm, and the thickness is 0.5-1 mm;
the length of the long-strip YAG is 10-100 mm, the width is 0.5-2 mm, and the thickness is 0.5-1 mm.
Preferably, in step (1), in order to ensure the mechanical properties of the eutectic fiber, the long strips of Al 2 O 3 And the thickness ratio z of the elongated YAG is 0.9-2, preferably 0.9.ltoreq.z <Z is more than 1.2 and less than or equal to 1.2 (1.2 is Al in the phase diagram on the premise of the same length and width) 2 O 3 Volume ratio to YAG, also Y in the phase diagram 2 O 3 And Al 2 O 3 Eutectic point of the phases). In the present invention, the thickness ratio can grow at the eutectic point, and then the liquid can grow from the eutectic point, namely the invention can grow from the eutectic point, which is innovative.
Preferably, in the step (2), the Al 2 O 3 The diameter of the seed crystal or YAG seed crystal is 0.5-1 mm.
Preferably, in the step (3), the growing atmosphere is nitrogen, oxygen or air; the atmosphere pressure of the growth is lower than one atmosphere pressure by 0.01-0.02 MPa.
Preferably, in step (3), the growth parameters include: the power of laser heating is 20-60W; seed crystal pulling speed V f 20-80 mm/min; the feed speed Vs of the source rod is 10-30 mm/min; control of Al 2 O 3 The diameter of the YAG eutectic optical fiber is 0.5-1.5 mm.
In yet another aspect, the present invention also provides an Al grown according to the above method 2 O 3 -YAG eutectic fiber.
The beneficial effects are that:
this patent uses Al 2 O 3 The crystal and YAG crystal are used as raw materials, and Al is directly grown by using a laser heating base method 2 O 3 YAG eutectic material, the ratio of the two crystals can be conveniently regulated by the method, the uniformity and crystallinity of the grown eutectic material are improved, and the growth process is simpler. Meanwhile, the crystal is taken as a raw material and has good crystallization performance, so that defects such as cracks and the like do not occur.
Drawings
FIG. 1 shows an elongated Al strip combined together 2 O 3 Crystals and YAG crystals;
FIG. 2 shows the grown Al 2 O 3 -YAG eutectic fiber composite;
FIG. 3 is Al 2 O 3 Eutectic morphology at/yag=8/7;
FIG. 4 is Al 2 O 3 Eutectic morphology at/yag=2.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
The present invention provides a method for directly growing Al from crystal 2 O 3 Method for adjusting long-strip Al by structural design of YAG eutectic optical fiber composite material 2 O 3 The thickness of the crystal and YAG crystal can accurately adjust the proportion of different components in the eutectic, and meanwhile, the crystal is used as a raw material, and the uniform distribution of all parts of the eutectic can be ensured by utilizing Montgomery convection in the growth process. Avoid the prior Al 2 O 3 In the preparation process of the YAG eutectic optical fiber composite material, the possible defects of pollution, cracks and the like exist when the powder is used as a raw material, so that the thermal shock resistance and the high-temperature creep resistance of the oxide eutectic optical fiber composite material under high temperature and high stress are greatly reduced. Meanwhile, the method has the advantages of large temperature gradient, high growth speed and simpler growth process.
The invention uses laser heating base method to directly grow Al with crystal as raw material 2 O 3 -YAG eutectic fiber composite. Can conveniently control Al 2 O 3 The ratio of the crystal to YAG crystal, and under the proper laser power and growth speed, obtaining the crack-free Al 2 O 3 -YAG eutectic fiber composite. The method uses Al 2 O 3 Compared with the method that powder is used as the raw material, the method can conveniently adjust the proportion of the two crystals in the eutectic crystal, and simultaneously ensures the uniformity of the grown eutectic material. The following exemplary description of laser heated susceptor method for directly growing Al from crystals 2 O 3 -YAG eutectic fiber.
Al is added with 2 O 3 And YAG crystals are cut into long strips. Al is cut by an inner circle or a wire cutting machine 2 O 3 And YAG crystals are cut into long strips, and the two crystals should be kept to have the same width and length during the cutting process. Preferably, the dimensions thereof are maintainedThe range is 10-100 mm in length, 0.5-2 mm in width and 0.5-1 mm in thickness. Al for growth 2 O 3 The YAG crystal has the same length and width, which is beneficial to the subsequent fitting.
Will take the shape of long strips of Al 2 O 3 And YAG crystals are combined together as a source rod. Specifically, cut long strips of Al 2 O 3 And polishing one side of YAG crystal with the length multiplied by the width for 10-20 min by using diamond grinding paste with the granularity number of W5-W16, and ensuring that the parallelism is unchanged in the polishing process. Preferably, ultrasonic cleaning is performed for 10 to 20 minutes after polishing is completed. The polished long Al strips with the same length and width 2 O 3 And polished surfaces of YAG crystals are adhered to each other and fixed to a laser heating susceptor feed unit.
To ensure that it forms eutectic, al is in the form of long strips of equal length and width 2 O 3 And YAG crystals according to Y 2 O 3 And Al 2 O 3 The thickness ratio of the two crystals obtained by the phase diagram is Al 2 O 3 YAG=0.97-1.17, but the method can deviate the phase diagram to lead Al 2 O 3 /YAG＝0.9～2。
By using Al with a diameter of 0.5-1 mm 2 O 3 Or YAG is used as seed crystal to be fixed on the laser heating base lifting device.
The growth is container-free, so that the growth can be performed under the conditions of nitrogen, oxygen, air and the like. In order to ensure the removal of bubbles, the air pressure in the growth process is lower than one atmosphere pressure by 0.01-0.02 MPa.
Adjusting the position of the laser heating base feeding device to enable the top ends of the two crystals to be positioned at the laser heating center and form a hemispherical melting zone, slowly placing the seed crystals into the melting zone, and then growing the eutectic optical fiber at a proper speed. Assume that an elongated Al with the same width D 2 O 3 And YAG crystal of thickness L 1 +L 2 Pulling speed V f Feeding speed Vs, the eutectic fiber radius r satisfies 4 Vs/pi vf=r 2 /D(L 1 +L 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Whereby by adjusting the proper pulling-up speed and feeding speedSelection of Al 2 O 3 The diameter of the YAG eutectic optical fiber composite material is in the range of 0.5-1.5 mm.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
(1) Al is cut by an internal circle or a wire cutting machine 2 O 3 And YAG crystals cut into a long strip with a length of 40mm and a width of 1.5mm, wherein Al 2 O 3 The thickness of the crystal is 0.8mm, and the thickness of the YAG crystal is 0.7mm;
(2) Will take the shape of long strips of Al 2 O 3 And YAG crystal length x width, polishing for 15min by using diamond grinding paste with particle size of W7, and ensuring parallelism in polishing process. Ultrasonic cleaning for 15min, and collecting long Al strips 2 O 3 The polished surface of the YAG crystal is mutually adhered to and fixed on a laser heating base feeding device;
(3) By means of Al with a diameter of 1mm 2 O 3 The crystal is used as seed crystal and is fixed on a laser heating base lifting device;
(4) The growth is carried out under an air atmosphere of 0.01MPa below one atmosphere. And then adjusting the position of the feeding device to enable the top end of the spliced square rod to be positioned at the laser focusing and heating position. Slowly lifting the power to 40W until the top end of the square rod is melted, slowly placing the seed crystal into a melting zone after a hemispherical melting zone is formed, lifting the seed crystal upwards by 28.6mm/h after the melting zone is stable, and feeding the spliced square rod upwards by 10mm/h to perform eutectic optical fiber growth. The diameter of the obtained eutectic optical fiber is about 1mm, and the eutectic morphology is shown in fig. 2 and 3.
Example 2
(1) Al is cut by an internal circle or a wire cutting machine 2 O 3 And YAG crystals cut into a long strip with a length of 40mm and a width of 1.5mm, wherein Al 2 O 3 The thickness of the crystal is 1mm, and the thickness of the YAG crystal is 0.5mm;
(2) Will take the shape of long strips of Al 2 O 3 And YAG crystal length x width, polishing for 15min by using diamond grinding paste with particle size of W7, and ensuring parallelism in polishing process. Ultrasonic cleaning for 15min, and collecting long Al strips 2 O 3 The polished surface of the YAG crystal is mutually adhered to and fixed on a laser heating base feeding device;
(3) By means of Al with a diameter of 1mm 2 O 3 The crystal is used as seed crystal and is fixed on a laser heating base lifting device;
(4) The growth is carried out under an air atmosphere of 0.01MPa below one atmosphere. And then adjusting the position of the feeding device to enable the top end of the spliced square rod to be positioned at the laser focusing and heating position. Slowly lifting the power to 40W until the top end of the square rod is melted, slowly placing the seed crystal into a melting zone after a hemispherical melting zone is formed, lifting the seed crystal upwards at 57.2mm/h after the melting zone is stable, and feeding the spliced square rod upwards at 20mm/h to perform eutectic optical fiber growth. The diameter of the obtained eutectic optical fiber is about 1mm, and the appearance of the eutectic optical fiber is shown in fig. 4.
Claims (8)
1. Laser heating base method for growing Al 2 O 3 -a method of YAG eutectic optical fiber, characterized by comprising:
(1) Al is added with 2 O 3 The crystal and YAG crystal are cut into long strips of Al 2 O 3 And the long-strip YAG are combined into a whole to be used as a source rod and fixed on a laser heating base feeding device;
(2) Al is added with 2 O 3 The seed crystal or YAG seed crystal is fixed on the laser heating base lifting device;
(3) Al by laser heating of the susceptor 2 O 3 -growth of YAG eutectic fiber.
2. The method of claim 1, wherein the steps areIn step (1), before the combination, the long Al is mixed 2 O 3 Polishing and cleaning one side of the long length multiplied by the width of the long-strip YAG; the polishing is carried out for 10-20 min by utilizing diamond grinding paste with the granularity number of W5-W16; the cleaning is ultrasonic cleaning, preferably ultrasonic cleaning for 10-20 min under the power of 60-120W.
3. The method according to claim 1, wherein in step (1), the elongated Al 2 O 3 The length of the steel is 10-100 mm, the width is 0.5-2 mm, and the thickness is 0.5-1 mm;
the length of the long-strip YAG is 10-100 mm, the width is 0.5-2 mm, and the thickness is 0.5-1 mm.
4. A method according to claim 3, wherein in step (1), the elongated Al 2 O 3 And the thickness ratio z of the elongated YAG is 0.9-2, preferably 0.9 < z < 1.2 and 1.2 < z < 2.
5. The method according to claim 1, wherein in step (2), the Al 2 O 3 The diameter of the seed crystal or YAG seed crystal is 0.5-1 mm.
6. The method of claim 1, wherein in step (3), the growing atmosphere is nitrogen, oxygen or air; the atmosphere pressure of the growth is lower than one atmosphere pressure by 0.01-0.02 MPa.
7. The method according to any one of claims 1-6, wherein in step (3), the parameters of the growth comprise: the power of laser heating is 20-60W; seed crystal pulling speed V f 20-80 mm/min; the feed speed Vs of the source rod is 10-30 mm/min; control of Al 2 O 3 The diameter of the YAG eutectic optical fiber is 0.5-1.5 mm.
8. An Al grown according to the method of any one of claims 1-7 2 O 3 -YAG eutectic fiber.
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| CN202310124557.5A CN116427017A (en) | 2023-02-16 | 2023-02-16 | Laser heating base method for growing Al 2 O 3 Method for producing YAG eutectic optical fiber |
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| CN202310124557.5A CN116427017A (en) | 2023-02-16 | 2023-02-16 | Laser heating base method for growing Al 2 O 3 Method for producing YAG eutectic optical fiber |
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