CN110160570B - Optical fiber sensor based on sapphire and optical fiber ferrule bonding and preparation method - Google Patents
Optical fiber sensor based on sapphire and optical fiber ferrule bonding and preparation method Download PDFInfo
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- CN110160570B CN110160570B CN201910395635.9A CN201910395635A CN110160570B CN 110160570 B CN110160570 B CN 110160570B CN 201910395635 A CN201910395635 A CN 201910395635A CN 110160570 B CN110160570 B CN 110160570B
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/26—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light
- G01D5/32—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light
- G01D5/34—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells
- G01D5/353—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre
- G01D5/3537—Optical fibre sensor using a particular arrangement of the optical fibre itself
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/32—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in transmittance, scattering or luminescence in optical fibres
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
- G01L1/242—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet the material being an optical fibre
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding, wherein the optical fiber sensor comprises an optical fiber ferrule and a single crystal sapphire sensing unit, and during preparation, the single crystal sapphire sensing unit and the optical fiber ferrule are bonded through high-temperature bonding to enable interface materials to be in diffusion bonding connection. The direct bonding method based on the atomic diffusion principle is obtained by performing interface material diffusion bonding connection between the single crystal sapphire sensing unit and the optical fiber insertion core at high temperature and high pressure, so that stable connection sensing can be realized between the optical fiber insertion core and the single crystal sapphire sensing unit, the problem of unmatched thermal expansion coefficients is avoided, the stability of a bonding interface in a high-temperature environment is high, and high-precision alignment packaging of the optical fiber and the sapphire sensing unit can be realized.
Description
Technical Field
The invention belongs to the technical field of optical fiber sensors, and particularly relates to an optical fiber sensor based on sapphire and optical fiber ferrule bonding and a preparation method thereof.
Background
The temperature and pressure measuring technology under the high-temperature environment has very wide application in the fields of military, aerospace, automobile industry, metallurgy and chemical industry and the like. For example, inside the combustion chamber of an automobile engine, the temperature can reach over 600 ℃; the temperature can reach more than 1000 ℃ in the aviation turbine engine; and in the combustion chamber of the rocket engine, the temperature can even reach more than 1700 ℃. At such high temperatures, conventional semiconductor sensors, capacitive sensors, etc. have been unable to meet the demands. The optical fiber sensor has the characteristics of small volume, light weight, no electromagnetic interference, high measurement precision, high temperature resistance and the like, so that the optical fiber sensor is widely used for sensing in a high-temperature environment. Sapphire has The characteristics of high melting point (2045 ℃), high hardness, chemical corrosion resistance, high light transmittance and The like, and is very suitable for preparing temperature and pressure sensitive elements in high-temperature environments (reference document (1) Lally EM, YongX, WangA. sapphire direct connecting as adapting form for compressing Sensing at extreme high temperatures [ J ]. Proceedings of SPIE-The International Society for Optical Engineering,2009,7316(5) 73160Y-73160Y-10.(2) Yi J, Lally E, WangA, et. Destrongton Al-sapphire fiber-P of robust fiber-P of proper porosity for electrical Engineering [ J ]. IEEE ] technique, 23-11, sapphire and The like, and has The advantages of high temperature and pressure resistance, long-term magnetic resistance, long-term stability, high temperature resistance, long-term stability and The like in combination with The temperature and pressure resistance of sapphire, and The like.
Currently, there are some documents that use sapphire and fiber to make sensors, such as:
1. patent application CN201711323719.9 discloses a preparation process of a sapphire photonic crystal fiber grating ultra-high temperature distributed sensor, which comprises the following steps: producing a special sapphire material rod body and a sleeve by using a special sapphire material rod preparation process and technology; secondly, based on the sapphire special material rod and the sleeve provided in the first step, the sapphire photonic crystal special optical fiber is produced by means of a photonic crystal special optical fiber preparation process and technology; thirdly, based on the sapphire photonic crystal special optical fiber provided in the second step, preparing a distributed fiber grating sensing unit in the sapphire photonic crystal special optical fiber by means of an ultrafast femtosecond laser engraving fiber grating preparation process and technology; and step four, adopting high-temperature sensor packaging technology based on a boron carbide high-temperature structure ceramic sleeve and high-temperature sensor packaging technology based on a sapphire capillary tube to package and protect the sapphire photonic crystal special optical fiber with the distributed fiber grating sensing unit provided based on the step three, and preparing the sapphire photonic crystal fiber grating ultra-high temperature distributed sensor.
2. Patent application CN201710213633.4 discloses an integrated optical fiber large pressure sensor and a manufacturing method thereof, comprising a sensing unit, a glass capillary, a sensor body, a welding point, a shell and a Fabry-Perot cavity; the sensing unit consists of a pressure sensing film, a glass substrate and a transmission optical fiber; a micro cavity is corroded in the middle of the upper surface of the glass substrate, the bottom of the micro cavity is used as a first reflecting surface of the Fabry-Perot cavity, and the corrosion depth of the micro cavity determines the initial length of the Fabry-Perot cavity; the glass substrate and the sensor body are connected into a whole in an anodic bonding mode; the glass capillary is attached to the bottom surface of the glass substrate; the sensor body and the shell are connected into a whole to provide protection for the sensing unit; the transmission optical fiber is inserted and fixed from the bottom hole of the glass capillary, and the upper end face of the transmission optical fiber is attached to the bottom face of the glass substrate. The sensor can avoid the defect that the traditional optical fiber Fabry-Perot sensor has glue packaging, has wider measuring range and can measure higher pressure.
However, how to stably connect the optical fiber and the sapphire sensitive element to realize sensing becomes a technical problem. The invention provides a method for manufacturing an optical fiber sensor based on sapphire and optical fiber ferrule bonding, which aims to solve the problems.
Disclosure of Invention
The invention provides an optical fiber sensor based on sapphire and optical fiber ferrule bonding and a preparation method thereof to solve the technical problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule and a single crystal sapphire sensing unit, wherein during preparation, the single crystal sapphire sensing unit and the optical fiber ferrule are connected by diffusion bonding of interface materials through high-temperature bonding; the single crystal sapphire sensing unit is one of a Fabry-Perot cavity temperature sensing unit formed by a single crystal sapphire sensing unit and a Fabry-Perot cavity pressure sensing unit formed by a plurality of single crystal sapphire sensing units.
Further, the optical fiber ferrule is one or more of zirconia, alumina, quartz glass and single crystal sapphire; the sizes of the optical fiber inserting core and the single crystal sapphire sensing unit can be selected according to actual requirements.
Further, a preparation method of the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
A. grinding and polishing treatment: respectively putting the optical fiber insertion cores into an automatic grinding machine for grinding and polishing;
B. cleaning: carrying out standard RCA cleaning on the polished single crystal sapphire sensing unit, simultaneously sending the polished optical fiber ferrule into an ultrasonic machine for ultrasonic treatment until no obvious foreign matter exists on the end face, wiping the end face with alcohol, and then cleaning the end face in a dilute sulfuric acid solution;
C. pre-bonding: putting a cleaned single crystal sapphire sensing unit on a flat but frosted zirconia rod, slowly sleeving a bonding fixture, aligning the flat end face of an optical fiber ferrule with the single crystal sapphire sensing unit, putting the optical fiber ferrule into the bonding fixture, and finally putting the optical fiber ferrule into a vacuum drying oven for drying to remove moisture between the single crystal sapphire sensing units and between the single crystal sapphire ferrules;
D. strong bonding: and taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with the flaring part of the optical fiber insertion core, applying a weight with the mass of 1.8-2.3 kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit and the optical fiber insertion core can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor.
Further, in the step A, after the grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule is controlled to be less than 1 μm; the surface roughness of the single crystal sapphire sensing unit is less than 0.1 nm.
Further, in step a, the specific process of grinding and polishing is as follows:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule or the single crystal sapphire sensing unit for 4-6 min, then taking down the optical fiber ferrule or the single crystal sapphire sensing unit, washing away residues of the end face of the optical fiber ferrule or the single crystal sapphire sensing unit in the grinding process by water flow, and wiping the residues clean by using dust-free paper;
secondly, finely grinding the optical fiber ferrule or the end face of the single crystal sapphire sensing unit by using 3 mu m grinding paper for 4-6 min, flushing the end face of the optical fiber ferrule or the single crystal sapphire sensing unit by using water flow, and wiping the end face by using dust-free paper;
and thirdly, polishing by using ADS polishing paper for 14-16 min, wherein the optical fiber core inserting hole after grinding and polishing is blocked by abrasive materials, and tungsten wires and the optical fiber are required to be used for sequentially processing the through hole.
Further, in step B, the standard RCA cleaning specifically includes the following steps:
(1) pretreatment of
Firstly, placing a single crystal sapphire sensing unit in a beaker, and cleaning for 3-5 times by using deionized water and ultrasonic waves until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit in concentrated sulfuric acid for 3.5-4.5 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 14-16 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 3-5 min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water to ammonia water to hydrogen peroxide of 4:1:1, and heating in a water bath at 74-76 ℃ for 4-5 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit with deionized water for 3-5 times;
thirdly, cleaning the mixture for 3-5 min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 74-76 ℃ for 3-4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit with deionized water for 3-5 times;
thirdly, cleaning the mixture for 3-5 min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit in a phosphoric acid (85%) solution, cleaning for 44-46 min at 148-152 ℃, and leaching the single crystal sapphire sensing unit with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
Further, in the step C, the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 55-65 min.
Further, in the step D, the temperature of the high-temperature bonding is 1150-1250 ℃, and the time is 115-130 min.
Further, hydrogen peroxide according to the mass ratio: the concentrated sulfuric acid was mixed at 1: 1.
Further, the concentration of the phosphoric acid solution was 85%.
The principle of the application is as follows: the optical fiber chip is based on the fact that materials such as sapphire wafers and optical fiber inserting cores are subjected to atomic diffusion in a high-temperature environment, so that strong connection is formed on a bonding interface, and the optical fiber inserting cores can fix and protect optical fibers.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) the invention adopts a direct bonding method without an intermediate bonding medium, the sensing unit and the optical fiber ferrule can be bonded and formed at one time, the method is simple and convenient, and the ferrule can play a role in fixing and protecting the optical fiber.
(2) According to the direct bonding method based on the atomic diffusion principle, the single crystal sapphire sensing unit and the optical fiber insertion core are connected through interface material diffusion bonding at high temperature and high pressure, the problem of unmatched thermal expansion coefficients is avoided, and the bonding interface has high stability in a high-temperature environment, so that stable connection sensing can be realized between the optical fiber insertion core and the single crystal sapphire sensing unit.
(3) The optical fiber core insert bonded by the invention is matched with the commercial standard optical fiber in outer diameter, so that the high-precision alignment packaging of the optical fiber and the sapphire sensing unit can be realized.
Drawings
In order to illustrate the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some examples of the present invention, and for a person skilled in the art, without inventive step, other drawings can be obtained according to these drawings:
FIG. 1 is a schematic structural diagram of an optical fiber sensor based on sapphire and fiber ferrule bonding according to the present application;
FIG. 2 is a schematic diagram of a single crystal sapphire sensor wafer bonded with a zirconia ferrule of the present application;
FIG. 3 is a sample object diagram after bonding of a single crystal sapphire sensor wafer and a zirconia ferrule of the present application;
FIG. 4 is a graph showing the wavelength of the optical fiber sensor manufactured by the method of example 1 of the present application as a function of pressure.
In the drawings: 1-optical fiber core insert; 2-a single crystal sapphire sensing unit; 3-corundum mould; 4-zirconia ferrule; 5-single crystal sapphire sheet; 6-zirconia rods; 7-external pressure.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
As shown in fig. 1, 2 and 3, the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule 1, a single crystal sapphire sensing unit 2, a corundum mold 3, a zirconia ferrule 4, a single crystal sapphire sheet 5, a zirconia rod 6 and an external pressure 7, wherein during preparation, the single crystal sapphire sensing unit 2 and the optical fiber ferrule 1 are connected through high-temperature bonding and interface materials are subjected to diffusion bonding; the single-crystal sapphire sensing unit 2 is a Fabry-Perot cavity pressure sensing unit formed by a single-chip multi-chip single-crystal sapphire sensing unit; the optical fiber ferrule 1 is made of zirconia and single crystal sapphire; the sizes of the optical fiber inserting core 1 and the single crystal sapphire sensing unit 2 can be selected according to actual requirements.
A preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
step 1: and (5) grinding and cleaning the inserting core. Even the flat-head zirconia lock pin, its terminal surface also has certain radian, does not satisfy the condition of bonding, needs to grind it, puts into the zirconia lock pin and grinds the polishing in the automatic grinding machine, and specific technology is:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 for 4min, then taking down the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2, washing away residues of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 in the grinding process by water flow, and wiping the residues clean by dust-free paper;
secondly, finely grinding the optical fiber ferrule 1 or the end face of the single crystal sapphire sensing unit 2 for 4min by using 3-micron grinding paper, and cleaning the end face by using dustless paper;
and thirdly, polishing by using ADS polishing paper for 14min, wherein the holes of the optical fiber ferrule 1 after grinding and polishing are blocked by abrasive materials, and tungsten wires and optical fibers are required to be used for sequentially processing through holes. After grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule 1 is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit 2 is below 0.1 nm. The core-inserting hole after grinding is blocked by abrasive, and a tungsten filament and an optical fiber are required to be sequentially subjected to through hole treatment. Then, the ferrule is subjected to ultrasonic treatment until no obvious foreign matters exist on the end face, and then the end face is wiped by alcohol and is placed into a dilute sulfuric acid solution.
Step 2: selection and cleaning of single crystal sapphire: the surface roughness of the single crystal sapphire wafer is selected to be below 0.1nm to achieve better bonding quality, and then standard RCA cleaning is carried out on the single crystal sapphire wafer, and the method comprises the following steps:
(1) pretreatment of
Putting the single crystal sapphire sensing unit 2 in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit 2 in concentrated sulfuric acid for 3.5 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 14 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 3min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water, ammonia water and hydrogen peroxide being 4:1:1, and heating in a water bath at 74 ℃ for 4 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 3-5 min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 74 ℃ for 3 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 3min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit 2 in a phosphoric acid solution, cleaning for 44min at 148 ℃ when the concentration of the phosphoric acid solution is 85%, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
And step 3: pre-bonding: FIG. 2 is a flow chart of bonding of a single crystal sapphire sensing wafer and a zirconia ferrule, wherein a cleaned single crystal sapphire sensing unit 2 is firstly placed on a zirconia rod with a flat end surface but frosted, then a bonding fixture is slowly sleeved, then the flat end surface of an optical fiber ferrule 1 is aligned with the single crystal sapphire sensing unit 2 and placed in the bonding fixture, and finally the bonding fixture is placed in a vacuum drying oven for drying, so that moisture between the single crystal sapphire sensing units 2 and between the single crystal sapphire sensing units and the optical fiber ferrule 1 is removed; the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 55 min.
And 4, step 4: strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with the flaring part of the optical fiber insertion core 1, applying a weight with the mass of 1.8kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit 2 and the optical fiber insertion core 1 can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor; the temperature of the high-temperature bonding is 1150 ℃ and the time is 115min, and as shown in fig. 3, the single crystal sapphire sheet and the zirconia ferrule can be firmly connected together.
The optical fiber sensor prepared in the embodiment 1 is subjected to a pressure experiment at normal pressure to 4MPa to obtain pressure sensitivity data, and a curve of wavelength variation with pressure is shown in fig. 4.
Example 2
As shown in fig. 1, 2 and 3, the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule 1, a single crystal sapphire sensing unit 2, a corundum mold 3, a zirconia ferrule 4, a single crystal sapphire sheet 5, a zirconia rod 6 and an external pressure 7, wherein during preparation, the single crystal sapphire sensing unit 2 and the optical fiber ferrule 1 are connected through high-temperature bonding and interface materials are subjected to diffusion bonding; the single crystal sapphire sensing unit 2 is a single crystal sapphire sensing unit to form a Fabry-Perot cavity temperature sensing unit; the optical fiber ferrule 1 is made of alumina, quartz glass and single crystal sapphire; the sizes of the optical fiber inserting core 1 and the single crystal sapphire sensing unit 2 can be selected according to actual requirements.
A preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
step 1: and (5) grinding and cleaning the inserting core. Even the flat-head zirconia lock pin, its terminal surface also has certain radian, does not satisfy the condition of bonding, needs to grind it, puts into the zirconia lock pin and grinds the polishing in the automatic grinding machine, and specific technology is:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 for 6min, then taking down the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2, washing away residues of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 in the grinding process by water flow, and wiping the residues clean by dust-free paper;
secondly, finely grinding the optical fiber ferrule 1 or the end face of the single crystal sapphire sensing unit 2 for 6min by using 3-micron grinding paper, and cleaning the end face by using dustless paper;
and thirdly, polishing by using ADS polishing paper for 16min, wherein the holes of the optical fiber ferrule 1 after grinding and polishing are blocked by abrasive materials, and tungsten wires and optical fibers are required to be used for sequentially processing through holes. After grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule 1 is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit 2 is below 0.1 nm. The core-inserting hole after grinding is blocked by abrasive, and a tungsten filament and an optical fiber are required to be sequentially subjected to through hole treatment. Then, the ferrule is subjected to ultrasonic treatment until no obvious foreign matters exist on the end face, and then the end face is wiped by alcohol and is placed into a dilute sulfuric acid solution.
Step 2: selection and cleaning of single crystal sapphire: the surface roughness of the single crystal sapphire wafer is selected to be below 0.1nm to achieve better bonding quality, and then standard RCA cleaning is carried out on the single crystal sapphire wafer, and the method comprises the following steps:
(1) pretreatment of
Putting the single crystal sapphire sensing unit 2 in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit 2 in concentrated sulfuric acid for 4.5 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 16 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 5min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water to ammonia water to hydrogen peroxide of 4:1:1, and heating in a water bath at 76 ℃ for 5 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 76 ℃ for 4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit 2 in a phosphoric acid solution, cleaning for 46min at 152 ℃ when the concentration of the phosphoric acid solution is 85%, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
And step 3: pre-bonding: FIG. 2 is a flow chart of bonding of a single crystal sapphire sensing wafer and a zirconia ferrule, wherein a cleaned single crystal sapphire sensing unit 2 is firstly placed on a zirconia rod with a flat end surface but frosted, then a bonding fixture is slowly sleeved, then the flat end surface of an optical fiber ferrule 1 is aligned with the single crystal sapphire sensing unit 2 and placed in the bonding fixture, and finally the bonding fixture is placed in a vacuum drying oven for drying, so that moisture between the single crystal sapphire sensing units 2 and between the single crystal sapphire sensing units and the optical fiber ferrule 1 is removed; the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 65 min.
And 4, step 4: strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with the flaring part of the optical fiber insertion core 1, applying a weight with the mass of 2.3kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit 2 and the optical fiber insertion core 1 can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor; the temperature of the high-temperature bonding is 1250 ℃, the time is 130min, and as shown in figure 3, the single crystal sapphire sheet and the zirconia ferrule can be firmly connected together.
Example 3
As shown in fig. 1, 2 and 3, the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule 1, a single crystal sapphire sensing unit 2, a corundum mold 3, a zirconia ferrule 4, a single crystal sapphire sheet 5, a zirconia rod 6 and an external pressure 7, wherein during preparation, the single crystal sapphire sensing unit 2 and the optical fiber ferrule 1 are connected through high-temperature bonding and interface materials are subjected to diffusion bonding; the single crystal sapphire sensing unit 2 is a single crystal sapphire sensing unit to form a Fabry-Perot cavity temperature sensing unit; the optical fiber ferrule 1 is made of zirconia, alumina and single crystal sapphire; the sizes of the optical fiber inserting core 1 and the single crystal sapphire sensing unit 2 can be selected according to actual requirements.
A preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
step 1: and (5) grinding and cleaning the inserting core. Even the flat-head zirconia lock pin, its terminal surface also has certain radian, does not satisfy the condition of bonding, needs to grind it, puts into the zirconia lock pin and grinds the polishing in the automatic grinding machine, and specific technology is:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 for 4min, then taking down the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2, washing away residues of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 in the grinding process by water flow, and wiping the residues clean by dust-free paper;
secondly, finely grinding the optical fiber ferrule 1 or the end face of the single crystal sapphire sensing unit 2 for 4min by using 3-micron grinding paper, and cleaning the end face by using dustless paper;
and thirdly, polishing by using ADS polishing paper for 14min, wherein the holes of the optical fiber ferrule 1 after grinding and polishing are blocked by abrasive materials, and tungsten wires and optical fibers are required to be used for sequentially processing through holes. After grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule 1 is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit 2 is below 0.1 nm. The core-inserting hole after grinding is blocked by abrasive, and a tungsten filament and an optical fiber are required to be sequentially subjected to through hole treatment. Then, the ferrule is subjected to ultrasonic treatment until no obvious foreign matters exist on the end face, and then the end face is wiped by alcohol and is placed into a dilute sulfuric acid solution.
Step 2: selection and cleaning of single crystal sapphire: the surface roughness of the single crystal sapphire wafer is selected to be below 0.1nm to achieve better bonding quality, and then standard RCA cleaning is carried out on the single crystal sapphire wafer, and the method comprises the following steps:
(1) pretreatment of
Putting the single crystal sapphire sensing unit 2 in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit 2 in concentrated sulfuric acid for 3.5 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 14 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 3min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water, ammonia water and hydrogen peroxide being 4:1:1, and heating in a water bath at 74 ℃ for 4 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 76 ℃ for 4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit 2 in a phosphoric acid solution, cleaning for 44min at 149 ℃ when the concentration of the phosphoric acid solution is 85%, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
And step 3: pre-bonding: FIG. 2 is a flow chart of bonding of a single crystal sapphire sensing wafer and a zirconia ferrule, wherein a cleaned single crystal sapphire sensing unit 2 is firstly placed on a zirconia rod with a flat end surface but frosted, then a bonding fixture is slowly sleeved, then the flat end surface of an optical fiber ferrule 1 is aligned with the single crystal sapphire sensing unit 2 and placed in the bonding fixture, and finally the bonding fixture is placed in a vacuum drying oven for drying, so that moisture between the single crystal sapphire sensing units 2 and between the single crystal sapphire sensing units and the optical fiber ferrule 1 is removed; the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 58 min.
And 4, step 4: strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with a flaring part of the optical fiber insertion core 1, applying a weight with the mass of 1.8-2.3 kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit 2 and the optical fiber insertion core 1 can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor; the temperature of the high-temperature bonding is 1180 ℃, the time is 118min, and as shown in fig. 3, the monocrystalline sapphire sheet and the zirconia ferrule can be firmly connected together.
Example 4
As shown in fig. 1, 2 and 3, the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule 1, a single crystal sapphire sensing unit 2, a corundum mold 3, a zirconia ferrule 4, a single crystal sapphire sheet 5, a zirconia rod 6 and an external pressure 7, wherein during preparation, the single crystal sapphire sensing unit 2 and the optical fiber ferrule 1 are connected through high-temperature bonding and interface materials are subjected to diffusion bonding; the single crystal sapphire sensing unit 2 is a plurality of single crystal sapphire sensing units which form a Fabry-Perot cavity pressure sensing unit; the optical fiber ferrule 1 is made of quartz glass and single crystal sapphire; the sizes of the optical fiber inserting core 1 and the single crystal sapphire sensing unit 2 can be selected according to actual requirements.
A preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
step 1: and (5) grinding and cleaning the inserting core. Even the flat-head zirconia lock pin, its terminal surface also has certain radian, does not satisfy the condition of bonding, needs to grind it, puts into the zirconia lock pin and grinds the polishing in the automatic grinding machine, and specific technology is:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 for 6min, then taking down the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2, washing away residues of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 in the grinding process by water flow, and wiping the residues clean by dust-free paper;
secondly, finely grinding the optical fiber ferrule 1 or the end face of the single crystal sapphire sensing unit 2 for 5min by using 3-micron grinding paper, and cleaning the end face by using dustless paper;
and thirdly, polishing by using ADS polishing paper for 14min, wherein the holes of the optical fiber ferrule 1 after grinding and polishing are blocked by abrasive materials, and tungsten wires and optical fibers are required to be used for sequentially processing through holes. After grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule 1 is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit 2 is below 0.1 nm. The core-inserting hole after grinding is blocked by abrasive, and a tungsten filament and an optical fiber are required to be sequentially subjected to through hole treatment. Then, the ferrule is subjected to ultrasonic treatment until no obvious foreign matters exist on the end face, and then the end face is wiped by alcohol and is placed into a dilute sulfuric acid solution.
Step 2: selection and cleaning of single crystal sapphire: the surface roughness of the single crystal sapphire wafer is selected to be below 0.1nm to achieve better bonding quality, and then standard RCA cleaning is carried out on the single crystal sapphire wafer, and the method comprises the following steps:
(1) pretreatment of
Putting the single crystal sapphire sensing unit 2 in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit 2 in concentrated sulfuric acid for 3.9 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 14 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 5min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water, ammonia water and hydrogen peroxide being 4:1:1, and heating in a water bath at 74 ℃ for 4.2 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 74 ℃ for 4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 5min by using hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit 2 in a phosphoric acid solution, cleaning for 44min at 151 ℃ when the concentration of the phosphoric acid solution is 85%, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
And step 3: pre-bonding: FIG. 2 is a flow chart of bonding of a single crystal sapphire sensing wafer and a zirconia ferrule, wherein a cleaned single crystal sapphire sensing unit 2 is firstly placed on a zirconia rod with a flat end surface but frosted, then a bonding fixture is slowly sleeved, then the flat end surface of an optical fiber ferrule 1 is aligned with the single crystal sapphire sensing unit 2 and placed in the bonding fixture, and finally the bonding fixture is placed in a vacuum drying oven for drying, so that moisture between the single crystal sapphire sensing units 2 and between the single crystal sapphire sensing units and the optical fiber ferrule 1 is removed; the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 62 min.
And 4, step 4: strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with the flaring part of the optical fiber insertion core 1, applying a weight with the mass of 2.1kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit 2 and the optical fiber insertion core 1 can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor; the temperature of the high-temperature bonding is 1230 ℃, the time is 125min, and as shown in figure 3, the monocrystalline sapphire sheet and the zirconia ferrule can be firmly connected together.
Example 5
As shown in fig. 1, 2 and 3, the optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises an optical fiber ferrule 1, a single crystal sapphire sensing unit 2, a corundum mold 3, a zirconia ferrule 4, a single crystal sapphire sheet 5, a zirconia rod 6 and an external pressure 7, wherein during preparation, the single crystal sapphire sensing unit 2 and the optical fiber ferrule 1 are connected through high-temperature bonding and interface materials are subjected to diffusion bonding; the single crystal sapphire sensing unit 2 is a single crystal sapphire sensing unit to form a Fabry-Perot cavity temperature sensing unit; the optical fiber ferrule 1 is made of aluminum oxide and single crystal sapphire; the sizes of the optical fiber inserting core 1 and the single crystal sapphire sensing unit 2 can be selected according to actual requirements.
A preparation method of an optical fiber sensor based on sapphire and optical fiber ferrule bonding comprises the following steps:
step 1: and (5) grinding and cleaning the inserting core. Even the flat-head zirconia lock pin, its terminal surface also has certain radian, does not satisfy the condition of bonding, needs to grind it, puts into the zirconia lock pin and grinds the polishing in the automatic grinding machine, and specific technology is:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 for 5min, then taking down the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2, washing away residues of the end face of the optical fiber ferrule 1 or the single crystal sapphire sensing unit 2 in the grinding process by water flow, and wiping the residues clean by dust-free paper;
secondly, finely grinding the optical fiber ferrule 1 or the end face of the single crystal sapphire sensing unit 2 for 5min by using 3-micron grinding paper, and cleaning the end face by using dustless paper;
and thirdly, polishing by using ADS polishing paper for 15min, wherein the holes of the optical fiber ferrule 1 after grinding and polishing are blocked by abrasive materials, and tungsten wires and the optical fibers are required to be used for sequentially processing through holes. After grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule 1 is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit 2 is below 0.1 nm. The core-inserting hole after grinding is blocked by abrasive, and a tungsten filament and an optical fiber are required to be sequentially subjected to through hole treatment. Then, the ferrule is subjected to ultrasonic treatment until no obvious foreign matters exist on the end face, and then the end face is wiped by alcohol and is placed into a dilute sulfuric acid solution.
Step 2: selection and cleaning of single crystal sapphire: the surface roughness of the single crystal sapphire wafer is selected to be below 0.1nm to achieve better bonding quality, and then standard RCA cleaning is carried out on the single crystal sapphire wafer, and the method comprises the following steps:
(1) pretreatment of
Putting the single crystal sapphire sensing unit 2 in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit 2 in concentrated sulfuric acid for 4 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit 2 for 15 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 4min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water to ammonia water to hydrogen peroxide of 4:1:1, and heating in a water bath at 75 ℃ for 5 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 4min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 75 ℃ for 4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
thirdly, cleaning the mixture for 4min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(4) placing the single crystal sapphire sensing unit 2 in a phosphoric acid solution, cleaning for 45min at 150 ℃ when the concentration of the phosphoric acid solution is 85%, and leaching the single crystal sapphire sensing unit 2 with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
And step 3: pre-bonding: FIG. 2 is a flow chart of bonding of a single crystal sapphire sensing wafer and a zirconia ferrule, wherein a cleaned single crystal sapphire sensing unit 2 is firstly placed on a zirconia rod with a flat end surface but frosted, then a bonding fixture is slowly sleeved, then the flat end surface of an optical fiber ferrule 1 is aligned with the single crystal sapphire sensing unit 2 and placed in the bonding fixture, and finally the bonding fixture is placed in a vacuum drying oven for drying, so that moisture between the single crystal sapphire sensing units 2 and between the single crystal sapphire sensing units and the optical fiber ferrule 1 is removed; the temperature of the vacuum drying oven is raised to 50 ℃ in advance, and the drying time is 60 min.
And 4, step 4: strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with a flaring part of the optical fiber insertion core 1, applying a weight with the mass of 1.8-2.3 kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit 2 and the optical fiber insertion core 1 can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor; the high-temperature bonding temperature is 1200 ℃, the time is 120min, and as shown in fig. 3, the monocrystalline sapphire sheet and the zirconia ferrule can be firmly connected together.
In conclusion, the direct bonding method without the intermediate bonding medium is adopted, the sensing unit and the optical fiber ferrule can be bonded and molded at one time, the method is simple and convenient, and the ferrule can play a role in fixing and protecting the optical fiber; the problem of unmatched thermal expansion coefficients is avoided, the stability of a bonding interface in a high-temperature environment is high, and high-precision alignment packaging of the optical fiber and the sapphire sensing unit can be realized.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. An optical fiber sensor based on sapphire and optical fiber ferrule bonding is characterized in that: the optical fiber sensor comprises an optical fiber ferrule (1) and a single crystal sapphire sensing unit (2), and during preparation, the single crystal sapphire sensing unit (2) and the optical fiber ferrule (1) are connected by diffusion bonding of interface materials through high-temperature bonding; the single crystal sapphire sensing unit (2) is one of a single crystal sapphire sensing unit which forms a Fabry-Perot cavity temperature sensing unit and a plurality of single crystal sapphire sensing units which form a Fabry-Perot cavity pressure sensing unit;
the preparation method comprises the following steps:
A. grinding and polishing treatment: respectively putting the optical fiber insertion cores (1) into an automatic grinding machine for grinding and polishing;
B. cleaning: carrying out standard RCA cleaning on the polished single-crystal sapphire sensing unit (2), meanwhile, sending the polished optical fiber ferrule (1) into an ultrasonic machine for ultrasonic treatment until no obvious foreign matter exists on the end face, wiping the end face with alcohol, and then cleaning in a dilute sulfuric acid solution;
C. pre-bonding: putting a cleaned single crystal sapphire sensing unit (2) on a zirconium oxide rod with a smooth but frosted end surface, slowly sleeving a bonding fixture, aligning the end surface of an optical fiber insertion core (1) with the single crystal sapphire sensing unit (2), putting the optical fiber insertion core into the bonding fixture, and finally putting the optical fiber insertion core into a vacuum drying box for drying to remove moisture between the single crystal sapphire sensing units (2) and between the single crystal sapphire sensing units and the optical fiber insertion core (1);
D. strong bonding: taking out the pre-bonded sample, putting the sample into a muffle furnace, inserting a corundum rod from an upper port of the muffle furnace, aligning one end of the corundum rod with a flaring part of the optical fiber insertion core (1), applying a weight with the mass of 1.8-2.3 kg to the other end of the corundum rod, then carrying out high-temperature bonding to ensure that the single crystal sapphire sensing unit (2) and the optical fiber insertion core (1) can be firmly connected together, cooling to room temperature, and taking out to obtain the optical fiber sensor;
the optical fiber ferrule (1) is one or more of zirconia, alumina, quartz glass and single crystal sapphire; the sizes of the optical fiber inserting core (1) and the single crystal sapphire sensing unit (2) can be selected according to actual requirements;
in the step A, after grinding and polishing treatment, the roughness of the end face of the optical fiber ferrule (1) is controlled to be less than 1 mu m; the surface roughness of the single crystal sapphire sensing unit (2) is less than 0.1 nm.
2. The optical fiber sensor based on sapphire and optical fiber ferrule bonding of claim 1, wherein: in step a, the specific process of grinding and polishing is as follows:
firstly, using 9 mu m grinding paper to carry out rough grinding, reducing the radian of the end face of the optical fiber ferrule (1) or the single crystal sapphire sensing unit (2) for 4-6 min, then taking down the optical fiber ferrule (1) or the single crystal sapphire sensing unit (2), washing away residues of the end face of the optical fiber ferrule (1) or the single crystal sapphire sensing unit (2) in the grinding process by water flow, and wiping the residues by dust-free paper;
secondly, finely grinding the optical fiber ferrule (1) or the end face of the single crystal sapphire sensing unit (2) by using 3 mu m grinding paper for 4-6 min, and cleaning the end face by using dust-free paper;
and thirdly, polishing by using ADS polishing paper for 14-16 min, wherein the holes of the optical fiber ferrule (1) after grinding and polishing are blocked by abrasive materials, and tungsten wires and optical fibers are required to be used for sequentially processing through holes.
3. The optical fiber sensor based on sapphire and optical fiber ferrule bonding of claim 1, wherein: in step B, the standard RCA cleaning specifically includes the steps of:
(1) pretreatment of
Putting a single crystal sapphire sensing unit (2) in a beaker, and cleaning for 3-5 times by adding ultrasonic into deionized water until no obvious foreign matter exists on the surface;
soaking the single crystal sapphire sensing unit (2) in concentrated sulfuric acid for 3.5-4.5 min;
thirdly, slowly pouring hydrogen peroxide into the sulfuric acid along the wall of the beaker, wherein the mass ratio of hydrogen peroxide: mixing concentrated sulfuric acid at a ratio of 1:1, and soaking the single crystal sapphire sensing unit (2) for 14-16 min;
pouring out the concentrated sulfuric acid and hydrogen peroxide mixed solution in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit (2) with deionized water for 3-5 times;
washing with hydrofluoric acid buffer solution for 3-5 min, and rinsing with deionized water for 3-5 times;
(2) alkali washing
Adding a proper amount of deionized water into a beaker, sequentially adding ammonia water and hydrogen peroxide according to the proportion of deionized water to ammonia water to hydrogen peroxide of 4:1:1, and heating in a water bath at 74-76 ℃ for 4-5 min;
pouring the ammonia water and hydrogen peroxide mixed solution in the beaker to a fixed alkali recovery barrel, and leaching the single crystal sapphire sensing unit (2) with deionized water for 3-5 times;
thirdly, cleaning the mixture for 3-5 min by using a hydrofluoric acid buffer solution, and leaching the mixture for 3-5 times by using deionized water;
(3) acid pickling
Adding a proper amount of deionized water into a beaker, sequentially adding hydrochloric acid and hydrogen peroxide according to the proportion of deionized water to hydrochloric acid to hydrogen peroxide of 4:1:1, and heating in a water bath at 74-76 ℃ for 3-4 min;
pouring out the mixed solution of hydrochloric acid and hydrogen peroxide in the beaker to a fixed acid recovery barrel, and leaching the single crystal sapphire sensing unit (2) with deionized water for 3-5 times;
(4) placing the single crystal sapphire sensing unit (2) in a phosphoric acid solution, cleaning for 44-46 min at 148-152 ℃, and leaching the single crystal sapphire sensing unit (2) with deionized water for 3-5 times;
(5) putting into dilute sulfuric acid solution, and depositing hydroxyl ions.
4. The optical fiber sensor based on sapphire and optical fiber ferrule bonding of claim 1, wherein: and C, raising the temperature of the vacuum drying oven to 50 ℃ in advance, wherein the drying time is 55-65 min.
5. The optical fiber sensor based on sapphire and optical fiber ferrule bonding of claim 1, wherein: in the step D, the temperature of the high-temperature bonding is 1150-1250 ℃, and the time is 115-130 min.
6. The optical fiber sensor based on sapphire and optical fiber ferrule bonding of claim 3, wherein: the concentration of the phosphoric acid solution is 85%.
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