CN107557862B - Zirconia single crystal optical fiber and preparation method and application thereof - Google Patents
Zirconia single crystal optical fiber and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a zirconia single crystal optical fiber and a preparation method and application thereof. The crystal has a molecular formula of ZrO2，ZrO2The single crystal optical fiber is fibrous ZrO having an extremely large aspect ratio2Single crystal of at least ZrO2Single crystal ZrO2Advantages of polycrystalline fibers. Diameter range: 0.5-1mm in length>15 cm. The invention adopts a laser heating pedestal method (LHPG) to grow ZrO2A single crystal optical fiber. The melting point of the single crystal fiber is up to 2715 ℃, and compared with the prior art, the single crystal fiber of the zirconium oxide has excellent physicochemical properties such as high thermal conductivity, high hardness, high strength, high toughness, extremely high wear resistance, chemical corrosion resistance and the like, and can be used for preparing novel high-temperature sensors.
Description
Technical Field
The invention relates to a novel single crystal optical fiber and a preparation method and application thereof, in particular to a zirconia single crystal optical fiber and a preparation method and application thereof, belonging to the technical field of crystals and devices.
Background
The high-temperature sensor is mainly applied to the fields of aerospace, weapon manufacturing, nuclear industry, metallurgy, chemical industry, heat treatment and the like, and can measure thousands of high temperatures. At present, high-temperature thermocouples and tungsten-rhenium thermocouples are commonly used for contact type high-temperature tests at home and abroad, and the requirements of the medium-low temperature field are basically met. However, with the continuous development of research technology, the temperature of the combustion chamber needs to be measured, especially in some special combustion fields, such as the temperature of the gas jet of rockets and missiles, the temperature of the combustion chamber of a scramjet engine, the detonation pressure and the detonation temperature, and the like. The traditional temperature measurement method cannot meet the requirement, and a high-temperature single crystal optical fiber is required.
The high-temperature single crystal optical fiber commonly used at present mainly comprises Tm, YAG and Al2O3. The Tm is YAG which is a fluorescence lifetime type optical fiber sensor, can measure the temperature of about 1200 ℃, but the fluorescence efficiency is very low at high temperature, so the temperature cannot be measured. Sapphire crystalThe body optical fiber is a black body cavity type optical fiber sensor, is not limited by fluorescence efficiency, can carry out high-temperature measurement, but is limited by the melting point (2050 ℃) thereof, and cannot carry out higher-temperature measurement.
Chinese patent document CN102212874A (application No. 201110139624.8) discloses a method for manufacturing a sapphire tapered optical fiber. The method comprises the steps of using a laser heating base method growth device, firstly melting the top end of a sapphire crystal source rod with a circular cross section to form a stable melting zone, and then dropping a sapphire optical fiber seed crystal into the melting zone at the top end of the sapphire crystal source rod to form a sapphire optical fiber growth melting zone; the sapphire fiber seed is then pulled up while the sapphire crystal source rod is fed up until stable growth forms the butt end of the sapphire tapered fiber. The pulling speed of the sapphire fiber seed crystal is changed under the condition that the feeding speed Vs of the sapphire crystal source rod is kept unchanged until the thin end of the sapphire conical fiber is formed, so that a sapphire fiber conical area is formed between the thick end and the thin end of the sapphire fiber. And when the grown sapphire optical fiber reaches the required length, finishing the growth of the sapphire tapered optical fiber, and cutting and polishing two ends of the sapphire tapered optical fiber to obtain the sapphire tapered optical fiber. However, the sapphire crystal fiber cannot be measured at a high temperature of 2000 ℃ or higher because of its limitation of melting point (2050 ℃).
The ultrahigh-temperature transient test technology has great application value in the fields of nuclear reactor cores, aircraft engines, hypersonic aircrafts, spaceship nose cones and the like, the test fields generally need to work in severe environments such as extremely high temperature (2300 plus 2500 ℃), high oxidability, high corrosivity, strong electromagnetic interference, strong radiation and the like, the traditional noble metal contact temperature measurement and infrared non-contact temperature measurement cannot meet the requirement of ultrahigh-temperature transient temperature measurement, and the temperature measurement materials and the technology need to have the characteristics of higher melting point, oxidation resistance, good light transmission characteristic, thermal stability, chemical stability, mechanical strength and the like. The development of ultra-high temperature oxide single crystal optical fiber with high thermal conductivity, high hardness, high strength, high toughness, extremely high wear resistance, oxidation resistance and chemical corrosion resistance is a problem to be solved urgently.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a zirconia single crystal optical fiber and a preparation method and application thereof.
The technical scheme of the invention is as follows:
a zirconia single crystal optical fiber has a chemical composition of a zirconia single crystal.
According to the present invention, it is preferable that the optical fiber has a circular or square cross section.
According to the present invention, it is preferable that the optical fiber has a diameter of 0.4 to 0.9mm, further preferably 0.45 to 0.7 mm;
preferably, the length of the optical fiber is more than or equal to 15 cm.
According to the present invention, it is preferable that the aspect ratio (length to diameter ratio) of the zirconia single crystal optical fiber is not less than 150: 1.
According to the invention, the zirconia single crystal is preferably cubic, the melting point is 2715 ℃, and the density is 5.89g/cm3Coefficient of thermal expansion of 9.6X 10-6K, thermal conductivity (2.5-2.9) w/(m.k), refractive index (2.15-2.23), dispersion 0.06, mohs hardness (7.8-8.2).
According to the present invention, the method for producing a single crystal optical fiber of zirconia comprises:
preparing zirconium oxide seed crystals;
a step of laser melting of a zirconia raw material;
and (3) neck-collecting, shouldering, isodiametric growth and extraction-removal of the zirconia seed crystals in the zirconia molten material.
According to the method for manufacturing an optical fiber of the present invention, preferably, the crystal extraction step further includes a high temperature annealing step.
According to the method for preparing the optical fiber of the present invention, preferably, in the step of preparing the zirconia seed crystal, the zirconia polycrystalline material rod is cut into a square rod or a round rod as the seed crystal or the raw material; further preferably, the length of the square rod or the round rod is 10-200mm, and further preferably 20-150 mm; the diameter of the polycrystalline material is 1-5 mm;
preferably, drying treatment is carried out after cutting; further preferably, the drying temperature is 60 to 80 ℃ and the drying time is 4 to 6 hours.
According to the method for producing an optical fiber of the present invention, preferably, in the step of laser melting the zirconia raw material, the raw material is melted by placing the center of the raw material rod at the center of the laser;
preferably, the power of the laser is 250-400W.
According to the preparation method of the optical fiber, the neck power is preferably 180-240W. Shoulder-laying, equal-diameter growth power of 120-. The selection can be made according to the diameter of the polycrystalline material and the pulling speed.
Preferably, when the diameter of the seed crystal is narrowed to 0.3-0.5mm in the neck narrowing process, shoulder setting and equal-diameter growth are carried out;
preferably, in the process of constant diameter growth, the pulling speed is 0.4-1.5 mm/min;
preferably, the zirconia feedstock rods are fed simultaneously during the isodiametric growth at a feed rate of 0.1 to 0.5 mm/min.
According to the preparation method of the optical fiber of the present invention, preferably, when the crystal grows to the required size, the laser power is increased to 180-240W to lift off the crystal.
According to the preparation method of the optical fiber, preferably, in the high-temperature annealing step, the crystal is subjected to medium-high temperature annealing treatment in the air, the annealing temperature is 1000-1500 ℃, and the annealing time is 20-40 h. And naturally cooling after the annealing is finished so as to eliminate the thermal stress in the crystal.
According to the preparation method of the optical fiber, a preferable scheme comprises the following steps:
(1) selection and treatment of source rods and seed crystals
ZrO 2 is mixed with2Respectively cutting the polycrystalline material rod into two square rods or round rods with the lengths of 150mm and 20mm as raw materials and seed crystals, fixing the raw materials and the seed crystals on a corundum rod with a groove by using high-temperature ceramic glue, and drying the corundum rod for 4 to 6 hours at the temperature of between 60 and 80 ℃;
(2) crystal growth
a. Cleaning the furnace chamber and the laser reflector, fixing the prepared raw material rod on the feeding device, and fixing the prepared seed crystal on the upper pulling device; increasing the power of a laser to melt the material rod, adjusting the center of the material rod to be positioned at a laser reflection focus, continuously increasing the power to form a stable hemispherical melting zone, and keeping the temperature for 5-10 minutes;
b. descending the seed crystal to contact with the melting zone, adjusting the position of the seed crystal to be positioned at the center of the melting zone, adjusting the heating power until the diameter of the seed crystal is not enlarged or reduced, starting the pulling device, gradually increasing the power, and performing neck collection; when the diameter of the seed crystal is narrowed to 0.3-0.5mm, shoulder setting and equal-diameter growth are carried out; upper pulling speed in the growth process: 0.4-1.5 mm/min, lower feed rate: 0.1-0.5 mm/min; when the crystal grows to the required size, gradually increasing the power and lifting the crystal;
c. after the crystal growth is finished, reducing the laser power at the rate of 5-50W/min, turning off the laser, and then opening the growth furnace after flowing a flowing atmosphere for 5-15 min;
d. after the growth is finished, the crystal is subjected to medium-high temperature annealing treatment in the air to eliminate the thermal stress in the crystal.
ZrO of the invention2The melting point of the single crystal optical fiber is up to 2715 ℃, and the single crystal optical fiber is a cubic system, has higher strength, hardness, wear resistance and corrosion resistance, and is an ideal material for an ultrahigh-temperature detector.
According to the invention, the zirconia single crystal fiber is used as a high-temperature sensing material.
The invention has the following characteristics and beneficial effects:
1. the invention obtains ZrO by utilizing laser heating pedestal technology (LHPG)2The diameter of the single crystal optical fiber is within the range of 0.5-1mm, the length of the single crystal optical fiber reaches more than 15cm, the single crystal optical fiber has a great aspect ratio, the fluctuation of the crystal diameter is small, the surface is smooth, the crystal quality is high, and the single crystal optical fiber is a brand new high-temperature sensing material with excellent performance.
2. ZrO of the present invention with respect to other materials2The single crystal optical fiber has the following advantages: the melting point is up to 2715 ℃, and high-temperature measurement of 2000-2500 ℃ can be carried out; has excellent physical and chemical properties such as high thermal conductivity, high hardness, high strength, high toughness, extremely high wear resistance, chemical corrosion resistance and the like, and can work in severe environments such as high temperature, corrosive atmosphere and the like.
3. The inventionPreparation process of zirconia single crystal fiber by laser heating pedestal method to obtain ZrO2The melting point temperature solves the problem of obstruction caused by overhigh melting point, and the melting zone is more uniform, the optical fiber growth process is more stable, the fluctuation of the optical fiber diameter is smaller, and the high-quality ZrO can be obtained more easily by accurately controlling the laser power under different rod diameters and different pulling rate ratios2A single crystal optical fiber.
Drawings
FIG. 1 shows ZrO produced in example 12Photographs of single crystal fiber samples.
FIG. 2 shows ZrO produced in example 12Single crystal XRD test pattern, in which: the abscissa is the angle 2 θ in units of degrees and the ordinate is the intensity, arbitrary units.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Example 1
ZrO2The preparation method of the single crystal optical fiber comprises the following steps:
(1) selection and treatment of source rods and seed crystals
(2) Crystal growth
Cleaning a furnace chamber and a laser reflector, fixing the prepared raw material on a feeding device, and fixing the prepared seed crystal on an upper lifting device. And increasing the power of the laser to 100W to melt the material rod, adjusting the center of the material rod to be positioned at a laser reflection focus, continuously increasing the power to 140W to form a stable hemispherical melting zone, and keeping the temperature for 10 minutes.
b, descending the seed crystal to enable the seed crystal to be in contact with the melting zone, adjusting the position of the seed crystal to enable the seed crystal to be positioned in the center of the melting zone, adjusting the heating power until the diameter of the seed crystal is not enlarged or reduced, starting the pulling device, gradually increasing the power to 200W, and performing neck collection. When the diameter of the seed crystal is narrowed to 0.5mm, the power is adjusted to 160W for shouldering and equal-diameter growth. Upper pulling speed in the growth process: 0.4 mm/min, lower feed rate: 0.2 mm/min. When the crystal grows to the required size, the power is gradually increased to 200W, and the crystal is extracted.
c, after the crystal growth is finished, reducing the laser power at the rate of 20W/min, turning off the laser, and then opening the furnace after flowing a flowing atmosphere for 15 min.
d, after the growth is finished, carrying out medium-high temperature annealing treatment on the crystal in the air to eliminate the thermal stress in the crystal. The specific annealing procedure is as follows: ZrO to be grown2The single crystal fiber is heated to 1000 ℃ in a sintering furnace and is kept at the constant temperature for 30 hours, and then is slowly cooled to room temperature.
Example 2
ZrO2The preparation method of the single crystal optical fiber comprises the following steps:
(1) selection and treatment of source rods and seed crystals
(2) Crystal growth
Cleaning a furnace chamber and a laser reflector, fixing the prepared raw material on a feeding device, and fixing the prepared seed crystal on an upper lifting device. And increasing the power of the laser to 100W to melt the material rod, adjusting the center of the material rod to be positioned at a laser reflection focus, continuously increasing the power to 140W to form a stable hemispherical melting zone, and keeping the temperature for 10 minutes.
b, descending the seed crystal to enable the seed crystal to be in contact with the melting zone, adjusting the position of the seed crystal to enable the seed crystal to be positioned in the center of the melting zone, adjusting the heating power until the diameter of the seed crystal is not enlarged or reduced, starting the pulling device, gradually increasing the power to 200W, and performing neck collection. When the diameter of the seed crystal is narrowed to 0.5mm, the power is adjusted to 150W for shouldering and equal-diameter growth. Upper pulling speed in the growth process: 1.2 mm/min, lower feed rate: 0.5 mm/min. When the crystal grows to the required size, the power is gradually increased to 200W, and the crystal is extracted.
c, after the crystal growth is finished, reducing the laser power at the rate of 10W/min, turning off the laser, and then opening the furnace after flowing a flowing atmosphere for 15 min.
d, after the growth is finished, carrying out medium-high temperature annealing treatment on the crystal in the air to eliminate the thermal stress in the crystal. The specific annealing procedure is as follows: ZrO to be grown2The single crystal fiber is heated to 1200 ℃ in a sintering furnace and is kept at the constant temperature for 24 hours, and then is slowly cooled to the room temperature.
Example 3:
ZrO2the preparation method of the single crystal optical fiber comprises the following steps:
(1) selection and treatment of source rods and seed crystals
(2) Crystal growth
Cleaning a furnace chamber and a laser reflector, fixing the prepared raw material on a feeding device, and fixing the prepared seed crystal on an upper lifting device. And increasing the power of the laser to 100W to melt the material rod, adjusting the center of the material rod to be positioned at a laser reflection focus, continuously increasing the power to 140W to form a stable hemispherical melting zone, and keeping the temperature for 10 minutes.
b, descending the seed crystal to enable the seed crystal to be in contact with the melting zone, adjusting the position of the seed crystal to enable the seed crystal to be positioned in the center of the melting zone, adjusting the heating power until the diameter of the seed crystal is not enlarged or reduced, starting the pulling device, gradually increasing the power to 200W, and performing neck collection. When the diameter of the seed crystal is narrowed to 0.3mm, the power of 130W is adjusted to carry out shouldering and equal-diameter growth. Upper pulling speed in the growth process: 1.5 mm/min, lower feed rate: 0.3 mm/min. When the crystal grows to the required size, the power is gradually increased to 200W, and the crystal is extracted.
c, after the crystal growth is finished, reducing the laser power at the rate of 5W/min, turning off the laser, and then opening the furnace after flowing a flowing atmosphere for 15 min.
d, after the growth is finished, carrying out medium-high temperature annealing treatment on the crystal in the air to eliminate the thermal stress in the crystal. Concrete backThe fire program was as follows: ZrO to be grown2The single crystal fiber is heated to 1300 ℃ in a sintering furnace and is kept at the constant temperature for 24 hours, and then is slowly cooled to the room temperature.
Example 4:
ZrO2the preparation method of the single crystal optical fiber comprises the following steps:
(1) selection and treatment of raw materials
(2) Crystal growth
Cleaning a furnace chamber and a laser reflector, fixing the prepared raw material on a feeding device, and fixing the prepared seed crystal on an upper lifting device. And increasing the power of the laser to 120W to melt the material rod, adjusting the center of the material rod to be positioned at a laser reflection focus, continuously increasing the power to 180W to form a stable hemispherical melting zone, and keeping the temperature for 20 minutes.
b, descending the seed crystal to enable the seed crystal to be in contact with the melting zone, adjusting the position of the seed crystal to enable the seed crystal to be positioned in the center of the melting zone, adjusting the heating power until the diameter of the seed crystal is not enlarged or reduced, starting the pulling device, gradually increasing the power to 220W, and performing neck collection. When the diameter of the seed crystal is narrowed to 0.3mm, the power is adjusted to 180W for shouldering and equal-diameter growth. Upper pulling speed in the growth process: 1.35 mm/min, lower feed rate: 0.15 mm/min. When the crystal grows to the required size, the power is gradually increased to 220W, and the crystal is extracted.
c, after the crystal growth is finished, reducing the laser power at the rate of 5W/min, turning off the laser, and then opening the furnace after flowing a flowing atmosphere for 15 min.
d, after the growth is finished, carrying out medium-high temperature annealing treatment on the crystal in the air to eliminate the thermal stress in the crystal. The specific annealing procedure is as follows: ZrO to be grown2The single crystal fiber is heated to 1400 ℃ in a sintering furnace and is kept at the constant temperature for 24 hours, and then is slowly cooled to room temperature.
Comparative example 1
As described in example 1, except that:
the upper part pulling speed in the growth process in the step (2) b is as follows: 2 mm/min. Too high pulling speed can cause too large internal stress of the crystal, easily generate defects and influence the quality of the crystal
Comparative example 2
As described in example 1, except that:
the upper part pulling speed in the growth process in the step (2) b is as follows: 0.2 mm/min. The pulling rate is relatively too small, resulting in an excessively large diameter of the resulting optical fiber crystal.
Comparative example 3
As described in example 1, except that:
the feeding speed of the lower part in the growth process in the step (2) b is as follows: 0.04 mm/min. The ratio of the upward pulling to the downward pulling is more than 9:1, the stability of a melting zone is reduced, the diameter fluctuation of the optical fiber is large, and the crystal quality is influenced.
Test example 1
The products obtained in examples 1 to 4 and comparative examples 1 to 3 were tested for physical properties as shown in Table 1.
TABLE 1
| Melting Point | Cross-sectional shape | Diameter of | Length of | |
| Example 1 | 2750 | Circular shape | 0.70mm | 19.5cm |
| Example 2 | 2720 | Circular shape | 0.65mm | 15.0cm |
| Example 3 | 2705 | Circular shape | 0.45mm | 18.0cm |
| Example 4 | 2719 | Circular shape | 0.66mm | 16.0cm |
| Comparative example 1 | 2730 | Circular shape | 0.30mm | 5.0cm |
| Comparative example 2 | 2742 | Circular shape | 1.05mm | 12cm |
| Comparative example 3 | 2721 | Circular shape | 0.30mm | 3.5cm |
As can be seen from Table 1, the single-crystal optical fibers of zirconia prepared in examples 1 to 4 of the present invention have uniform diameters, lengths of 15cm or more, and aspect ratios of 230 or more.
Comparative examples 1 to 3 were not properly controlled in preparation parameters, and the obtained zirconia single crystal optical fiber was poor in quality and short in length.
Claims (6)
1. The zirconia single crystal optical fiber is characterized in that the chemical composition of the optical fiber is zirconia single crystal, the diameter of the optical fiber is 0.4-0.9mm, and the length of the optical fiber is more than or equal to 15 cm; the zirconia single crystal is a cubic crystal system, the melting point is 2715 ℃, and the density is 5.89g/cm3Coefficient of thermal expansion of 9.6X 10-6K, thermal conductivity of 2.5-2.9 w/(m.K), refractive index of 2.15-2.23, dispersion of 0.06, Mohs hardness of 7.8-8.2;
the preparation method utilizes a laser heating pedestal method, and comprises the following steps:
preparing zirconium oxide seed crystals;
a step of zirconia raw material laser melting, which is to place the center of a raw material rod at the center of laser to melt the raw material, wherein the power of a laser is 250-400W;
the zirconium oxide seed crystal is subjected to neck collection, shouldering, isometric growth and extraction and removal in the zirconium oxide molten material; neck power of 180-; when the diameter of the seed crystal is narrowed to 0.3-0.5mm in the process of neck contraction, shoulder setting and equal-diameter growth are carried out; in the process of isometric growth, the pulling speed is 0.4-1.5 mm/min; the feeding speed of the zirconium oxide raw material rods is 0.1-0.5 mm/min during the equal-diameter growth process.
2. A method for producing a zirconia single-crystal optical fiber according to claim 1, which uses a laser heating susceptor method comprising:
preparing zirconium oxide seed crystals;
a step of zirconia raw material laser melting, which is to place the center of a raw material rod at the center of laser to melt the raw material, wherein the power of a laser is 250-400W;
the zirconium oxide seed crystal is subjected to neck collection, shouldering, isometric growth and extraction and removal in the zirconium oxide molten material; neck power of 180-; when the diameter of the seed crystal is narrowed to 0.3-0.5mm in the process of neck contraction, shoulder setting and equal-diameter growth are carried out; in the process of isometric growth, the pulling speed is 0.4-1.5 mm/min; the feeding speed of the zirconium oxide raw material rods is 0.1-0.5 mm/min during the equal-diameter growth process.
3. The method of manufacturing a zirconia single crystal optical fiber according to claim 2, further comprising a high temperature annealing step after the crystal is pulled out.
4. The method for producing a zirconia single-crystal optical fiber according to claim 2, wherein the zirconia seed crystal production step is a step of cutting a zirconia polycrystalline material rod into a square rod or a round rod as a seed crystal or a raw material.
5. The method for preparing a zirconia single-crystal optical fiber according to claim 4, wherein the length of the square or round rod in the step of preparing the zirconia seed crystal is 10 to 200mm, and the diameter of the polycrystalline material is 1 to 5 mm; and after cutting, drying at 60-80 ℃ for 4-6 hours.
6. The method for preparing a single crystal zirconia optical fiber as defined in claim 2, wherein in the high temperature annealing step, the crystal is annealed at 1000-1500 ℃ for 20-40h in air at medium-high temperature.
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| CN108330540B (en) * | 2018-04-12 | 2020-09-04 | 山东大学 | Hafnium oxide single crystal optical fiber and preparation method and application thereof |
| CN108977882B (en) * | 2018-08-31 | 2021-02-12 | 山东大学 | Sesquioxide single crystal optical fiber and preparation method and application thereof |
| CN110777429A (en) * | 2019-10-15 | 2020-02-11 | 山东大学 | Preparation device and method of crystal optical fiber |
| CN112095144A (en) * | 2020-09-02 | 2020-12-18 | 上海理工大学 | Method for preparing CeF3 single crystal optical fiber by laser heating pedestal method |
| CN112281213B (en) * | 2020-10-26 | 2022-04-26 | 山东大学 | Rare earth doping (Lu)aScbYc)2O3(a + b + c = 1) single crystal optical fiber, and preparation method and application thereof |
| CN112965162A (en) * | 2021-03-04 | 2021-06-15 | 山东大学 | High-sensitivity single crystal optical fiber temperature measurement method based on single crystal optical fiber acoustic anisotropy and doping modulation |
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