CN110257919A - A kind of uniform diameter single crystal fiber processing method - Google Patents
A kind of uniform diameter single crystal fiber processing method Download PDFInfo
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- CN110257919A CN110257919A CN201910424254.9A CN201910424254A CN110257919A CN 110257919 A CN110257919 A CN 110257919A CN 201910424254 A CN201910424254 A CN 201910424254A CN 110257919 A CN110257919 A CN 110257919A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
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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
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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
- 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
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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
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
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- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
Abstract
The present invention provides a kind of uniform diameter single crystal fiber processing methods, the crystal of length 30-300mm is obtained by czochralski method or other growing methods, pass sequentially through orientation, cutting, crystal bar is obtained after round as a ball processing method processing, it is (1.5-3.5) that crystal bar, which is soaked in molar ratio: in 1 concentrated sulfuric acid and concentrated phosphoric acid, wherein the concentration of concentrated sulfuric acid solution is 90%~99.8%, the concentration of concentrated phosphoric acid is 60%~90%, it is put into togerther again and is heated to boil in Muffle furnace, under the process conditions for setting right times and temperature, obtain the single crystal fiber of uniform diameter, diameter dimension is more uniformly and accurate, this method has easy to operate, feature easy to process, it is suitble to industrialization production.
Description
Technical field
The invention belongs to field of crystal processing, in particular to a kind of uniform diameter single crystal fiber processing method.
Background technique
Crystal fibre is since its brilliant performance obtains extensive research in recent years, in general, fiber refers to diameter in micron
To the elongated pole of millimeter magnitude diameter, the material for meeting this condition can be known as fiber, for transmitting optical signal
Fiber is referred to as optical fiber.
The fiber of different crystal materials has been widely used in each different application field, such as sapphire fibre, by
It is only second to diamond in the hardness (Mohs degree 9) of sapphire crystal, its high, wear-resistant, heat-resisting ability with hardness and strength
Strong feature and chemical property are stablized, the series of characteristics such as acid-alkali-corrosive-resisting, so sapphire fibre is used on aircraft industry
Make metal based reinforcement material；Sapphire crystal has good through performance in visible light to 5.6um spectral region, in military affairs
The upper electric light that is used as aims at；Medically with 2.94 μm of laser for being used to transmit Er:YAG laser；Due to sapphire Gao Rong
Point and optical property, industrially may be used as high temperature measurement.
The rear-earth-doped oxide crystal optical fibre as high power fibre laser becomes a new research hotspot recently.
As long as high purity quartz optical fiber has been used 40 years, due to quartz glass thermal coefficient very little, only 1.4-1.6Wm-1K-1,
Small thermal coefficient to heat-radiation belt come huge adverse effect, therefore optical fiber laser high power operate when still for refrigeration have compared with
High requirement limits continuing to lift up for its power.For monocrystalline laser gain medium, common laser crystal yttroalumite
Garnet (YAG) crystal thermal coefficient~14W/m.K, the thermal coefficient of yttrium aluminate (YAP) crystal are higher than also above~11W/m.K
Quartz glass several times；Accordingly it is contemplated that the matrix using monocrystalline as Active Optical Fiber, improves optical fiber sheet using its high thermal conductivity coefficient
The heat dissipation performance of body reduces requirement of the system for refrigeration, simplifies the complexity of system, the power and light beam matter of improving laser device
The output performances indexs such as amount.
Oxide monocrystal optical fiber is widely applied in linear and device for non-linear optical.Transfer element can be made, swashed
Element and nonlinear optical element etc. living.Manufacturing these, component requirements single crystal fiber is of uniform size, it is few to include defect.Diameter 25
μm, the single crystal fiber of long 5cm, 1% diameter fluctuation by cause 25% optical transmission loss.Make the monocrystalline light of non-linear element
Fibre, diameter fluctuation require < 0.1~1%.It is well known that the light loss of monocrystal is mainly lacked by diameter fluctuation and various crystal
Caused by falling into.Bulk-shaped monocrystal can choose of uniform size, bar that defect is seldom by machining etc., and single crystal fiber due to
Diameter very little (usually < 500 μm), it is difficult to the single crystal fiber that diameter is less than 2mm is processed by the methods of machining, especially
When fiber lengths > 100mm, machining yield is lower than 60%.Crystal optical fibre of the diameter less than 2mm generallys use the side of crystal growth
Method obtains, and the common method of existing growth oxide crystal optical fibre has micro- glass tube down-drawing, laser heated pedestal method and EFG technique all
It is faced with the big problem of fibre diameter fluctuations.Therefore, the crystalline substance for how obtaining uniform diameter is fine as important research topic.
Summary of the invention
The purpose of the present invention is to solve being difficult to the problem of obtaining uniform diameter oxide monocrystal optical fiber in the prior art,
In order to achieve the above objectives, the present invention provides a kind of uniform diameter single crystal fiber processing methods, easy to operate, easy to process, can
Obtain the crystal optical fibre specific method step of the uniform diameter of different oxide monocrystals are as follows:
(1) crystal of length 30-300mm is obtained by the growing method of czochralski method；(2) it passes sequentially through orientation, cut
It cuts, the crystal bar of uniform diameter of the round as a ball processing method acquisition diameter in 1.5-4.5mm or so；(3) crystal bar after will be round as a ball is put
It is placed in the quartz or glassware with cover of matching length；(4) the certain density concentrated sulfuric acid and concentrated phosphoric acid are successively poured into dress
Have in the above-mentioned vessel of crystal bar, it is 1cm-10cm that the height that acid solution is arranged, which exceeds the height on crystal bar top,；(5) will equipped with crystal bar and
The vessel of acid solution are put into togerther in Muffle furnace, and the heating rate of 100-300 DEG C/h is heated to 300-380 DEG C, constant temperature；In constant temperature
It period interval 5-15 minutes, takes out crystal bar and measures diameter, until stopping measurement after reaching required fibre diameter, measurement diameter is drawn
It is made as diameter and changes over time curve, the foundation as the control of later period production process.
As an improvement, the concentration of concentrated sulfuric acid solution described in step (4) uses 90%~99.8%, the concentrated phosphoric acid
Concentration use 60%~90%, the concentrated sulfuric acid and concentrated phosphoric acid molar ratio are (1.5-3.5): 1.
As an improvement, the optical fiber is sapphire or garnet optical fiber.
The utility model has the advantages that uniform diameter single crystal fiber processing method provided by the invention, by being by crystal bar immersion molar ratio
(1.5-3.5): in 1 concentrated sulfuric acid and concentrated phosphoric acid, wherein the concentration of concentrated sulfuric acid solution is 90%~99.8%, concentrated phosphoric acid
Concentration is 60%~90%, is placed in Muffle furnace together, under the right times of setting and the process conditions of temperature, is obtained straight
The uniform single crystal fiber of diameter, diameter dimension is more uniformly and accurate, easy to operate, easy to process.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is 800 μm of diameter of the optical fiber scanning electron microscope that the present invention obtains.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
A kind of uniform diameter single crystal fiber processing method, first passes through czochralski method or other growing methods obtain length
The crystal of 30-300mm；Pass sequentially through orientation, cutting, round as a ball processing method obtain diameter in the diameter of 1.5-4.5mm or so
Uniform crystal bar；Crystal bar after will be round as a ball is placed in the quartz or glassware with cover of matching length；It will be certain density
The concentrated sulfuric acid and concentrated phosphoric acid are successively poured into the above-mentioned vessel equipped with crystal bar, and the height that acid solution is arranged is beyond the height on crystal bar top
1cm-10cm；Vessel equipped with crystal bar and acid solution are put into togerther in Muffle furnace, the heating rate of 100-300 DEG C/h is heated to
300-380 DEG C, constant temperature；It is spaced 5-15 minutes during constant temperature, takes out crystal bar and measure diameter, until after reaching required fibre diameter
Stop measurement, measurement diameter is plotted as diameter and changes over time curve, diameter change rate can be obtained by drawing curve, to use in the future
In the accurate control corrosion rate time.
Preferably, the concentration of the concentrated sulfuric acid, the concentration of concentrated phosphoric acid acid solution, the concentrated sulfuric acid etching time according to be processed
The material category of optical fiber and the diameter of optical fiber and the diameter for preparing optical fiber determine.
Embodiment 1
The crystal of length 30-100mm is obtained by czochralski method；Pass sequentially through orientation, cutting, round as a ball processing method acquisition
Crystal bar of the diameter in the uniform diameter of 1.5-2.5mm or so；Crystal bar after will be round as a ball is placed in the quartz with cover of matching length
Or in glassware；It is that 90% concentrated sulfuric acid and 60-75% concentrated phosphoric acid are successively poured into the above-mentioned vessel equipped with crystal bar by concentration,
The molar ratio of the middle concentrated sulfuric acid and concentrated phosphoric acid is (1.5-2): 1.
It is 1cm-10cm that the height that acid solution is arranged, which exceeds the height on crystal bar top,；Together by the vessel equipped with crystal bar and acid solution
It is put into Muffle furnace, with 100-220 DEG C/h heating rate, is heated to 300-340 DEG C, constant temperature；9-15 points are spaced during constant temperature
Clock takes out crystal bar and measures diameter, until stopping measurement after reaching 800 μm of required fibre diameter, measurement diameter is plotted as diameter
Curve is changed over time, diameter change rate can be obtained by drawing curve, and to be used for the accurate control corrosion rate time in the future, wherein diameter becomes
Rate is the fit slope value of change curve.
Embodiment 2
The crystal of length 120-300mm is obtained by czochralski method；Pass sequentially through orientation, cutting, round as a ball processing method obtain
Diameter is obtained in the crystal bar of the uniform diameter of 2.5-4.5mm or so；Crystal bar after will be round as a ball is placed in the stone with cover of matching length
In English or glassware；It is that the 97-99% concentrated sulfuric acid and concentration 75-90% concentrated phosphoric acid are successively poured into equipped with the above-mentioned of crystal bar by concentration
In vessel, wherein the molar ratio of the concentrated sulfuric acid and concentrated phosphoric acid is (2-3.5): 1.
It is 1cm-10cm that the height that acid solution is arranged, which exceeds the height on crystal bar top,；Together by the vessel equipped with crystal bar and acid solution
It is put into Muffle furnace, with 220-300 DEG C/h heating rate, is heated to 350-380 DEG C, constant temperature；5-10 points are spaced during constant temperature
Clock takes out crystal bar and measures diameter, until stopping measurement after reaching 820 μm of required fibre diameter, measurement diameter is plotted as diameter
Curve is changed over time, diameter change rate can be obtained by drawing curve, and to be used for the accurate control corrosion rate time in the future, wherein diameter becomes
Rate is the fit slope value of change curve.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (3)
1. a kind of uniform diameter single crystal fiber processing method, it is characterised in that: specific method step are as follows:
(1) crystal of length 30-300mm is obtained by czochralski method；(2) orientation is passed sequentially through, cutting, round as a ball processing method obtain
Diameter is obtained in the crystal bar of the uniform diameter of 1.5-4.5mm or so；(3) crystal bar after will be round as a ball lies against the with cover of matching length
In quartz or glassware；(4) the certain density concentrated sulfuric acid and concentrated phosphoric acid are successively poured into the above-mentioned vessel equipped with crystal bar, if
It is 1cm-10cm that the liquid level for setting acid solution, which exceeds the height of upper end crystal bar,；(5) vessel one of crystal bar and mix acid liquor will be housed
It rises and is put into Muffle furnace, with the heating rate of 100-300 DEG C/h, be heated to 300-380 DEG C, 5-15 points are spaced during constant temperature
Clock takes out crystal bar and measures diameter, until stopping measurement after reaching required fibre diameter, measurement diameter is plotted as diameter at any time
Change curve, the foundation as the control of later period production process.
2. uniform diameter single crystal fiber processing method according to claim 1, it is characterised in that: dense described in step (4)
The concentration of sulfuric acid solution uses 90%~99.8%, and the concentration of the concentrated phosphoric acid uses 60%~90%, the concentrated sulfuric acid and dense
Phosphoric acid molar ratios are (1.5-3.5): 1.
3. uniform diameter single crystal fiber processing method according to claim 1, it is characterised in that: the optical fiber is sapphire
Or garnet optical fiber or other oxide crystal optical fiber.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910424254.9A CN110257919A (en) | 2019-05-21 | 2019-05-21 | A kind of uniform diameter single crystal fiber processing method |
| PCT/CN2020/084443 WO2020233279A1 (en) | 2019-05-21 | 2020-04-13 | Method for processing single crystal optical fiber with uniform diameter |
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| CN201910424254.9A CN110257919A (en) | 2019-05-21 | 2019-05-21 | A kind of uniform diameter single crystal fiber processing method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111501104A (en) * | 2020-04-14 | 2020-08-07 | 中国科学院上海光学精密机械研究所 | Rare earth doped YAG crystal fiber core with hundred-micron diameter and preparation method thereof |
| WO2020233279A1 (en) * | 2019-05-21 | 2020-11-26 | 南京同溧晶体材料研究院有限公司 | Method for processing single crystal optical fiber with uniform diameter |
| CN112195517A (en) * | 2020-06-10 | 2021-01-08 | 眉山博雅新材料有限公司 | Method for preparing doped YAG single crystal optical fiber core |
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| CN1460573A (en) * | 2003-04-25 | 2003-12-10 | 中国科学院上海光学精密机械研究所 | Surface processing method of titanium-doped sapphire crystal laser rod |
| JP2007123486A (en) * | 2005-10-27 | 2007-05-17 | Sumitomo Metal Mining Co Ltd | Surface treatment method of sapphire substrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020233279A1 (en) * | 2019-05-21 | 2020-11-26 | 南京同溧晶体材料研究院有限公司 | Method for processing single crystal optical fiber with uniform diameter |
| CN111501104A (en) * | 2020-04-14 | 2020-08-07 | 中国科学院上海光学精密机械研究所 | Rare earth doped YAG crystal fiber core with hundred-micron diameter and preparation method thereof |
| CN112195517A (en) * | 2020-06-10 | 2021-01-08 | 眉山博雅新材料有限公司 | Method for preparing doped YAG single crystal optical fiber core |
| US11136690B1 (en) | 2020-06-10 | 2021-10-05 | Meishan Boya Advanced Materials Co., Ltd. | Method for preparing doped yttrium aluminum garnet single crystal fiber by performing a cylindrical surface polishing operation and growing a cladding layer |
| CN112195517B (en) * | 2020-06-10 | 2022-03-01 | 眉山博雅新材料股份有限公司 | Method for preparing doped YAG single crystal optical fiber core |
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