CN107365983B - The preparation method of fibre optic temperature sensor and its cadmium sulphide membrane - Google Patents
The preparation method of fibre optic temperature sensor and its cadmium sulphide membrane Download PDFInfo
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- CN107365983B CN107365983B CN201610316151.7A CN201610316151A CN107365983B CN 107365983 B CN107365983 B CN 107365983B CN 201610316151 A CN201610316151 A CN 201610316151A CN 107365983 B CN107365983 B CN 107365983B
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- optical fiber
- cadmium
- cadmium sulphide
- sulphide membrane
- temperature sensor
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
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- 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
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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- General Physics & Mathematics (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The present invention provides a kind of preparation method of fibre optic temperature sensor cadmium sulphide membrane, includes the following steps: after optical fiber is fixed on lock pin, and the exposed end face of the optical fiber is polished;Plated film: thiocarbamide, cadmium sulfate and ammonium hydroxide are dissolved in deionized water according to quality-volume ratio for 5.694g:0.184g:45mL mixing and form reaction solution;Then the exposed end face is inserted into the reaction solution, in temperature is 65 DEG C using chemical water bath, reacts 9min, complete the plated film of a cadmium sulphide membrane;The plating steps are repeated to n times, obtain the exposed end face for being deposited with n+1 layers of cadmium sulphide membrane, n is the natural number greater than 0;It will be made annealing treatment at a temperature of 200 DEG C by the optical fiber for repeating plating steps acquisition.The present invention plates cadmium sulphide membrane using chemical water bath, and this method can make cadmium sulphide film combine closely with fiber end face, and coating film thickness is controllable.
Description
Technical field
The present invention relates to the temperature mediation systems of sensor technical field, especially sensor.
Background technique
Fibre optic temperature sensor has the advantages that other temperature sensors are incomparable, have electromagnetism interference, high temperature resistant,
The features such as high voltage withstanding, resistant to chemical etching and low-loss, therefore it is widely used in high DC electric field, high-intensity magnetic field, strong high frequency field, micro-
In the adverse circumstances such as wave field.The research contents of fibre optic temperature sensor is concentrated mainly on there are three aspect both at home and abroad at present: first is that
The research of temperature sensitive material, more semiconductor materials are applied on fibre optic temperature sensor;Second is that system structure and
The research of modulation technique;Third is that the research of commercialization functionization, i.e., from practical application, to being able to satisfy particular requirement, be applicable in
In the research of the temperature sensor of specific occasion.But in current research achievement, the manufacture craft of fibre optic temperature sensor is multiple
It is miscellaneous, higher cost, therefore describe in the present invention a kind of more accurate, more stable, and the simple fiber optic temperature of manufacture craft passes
Sensor.
A kind of fibre optic temperature sensor probe apparatus of CN201110459236.8, devises a kind of fibre optic temperature sensor
Sonde configuration, it is characterised in that conduction optical fiber one end fibre core and covering fixed with ceramic contact pin, conduction fiber core end face,
Covering end face and ceramic contact pin end face in the same plane, can plate the semiconductive thin films such as silicon, germanium, GaAs on this plane.
A kind of Reflecting double-layer membrane optical fiber temperature sensor probe of CN201020188165.3 devises a kind of reflective
The double-deck fibre optic temperature sensor, which is characterized in that ceramic contact pin is bonded outside optical fiber, using optical fiber and ceramic contact pin end as biography
Sensor probe, and bilayer film is plated in the end face of optical fiber and ceramic contact pin.Ceramic contact pin and close fiber optic bond, and the two end
Face polishing alignment.Optical fiber and the first layer film of ceramic contact pin end face plating use semiconductor Germanium material.Optical fiber and ceramic contact pin end
Second layer film of face plating uses low-index material, preferentially uses earth silicon material.Germanium film and optical fiber and ceramic contact pin
Densification is bonded a kind of reflective temperature sensor.
A kind of reflection-type optical fiber temperature sensor of CN201010154666.4, it discloses a kind of temperature sensors, especially
It is a kind of semiconductor reflection-type optical fiber temperature sensor, it is characterised in that including optical fiber, semiconductor film, ceramic contact pin.By light
Long and slender core is inserted into ceramic contact pin, makes core end surface and ceramic contact pin end face in the same plane, using coating technique by semiconductor
Film layer is plated in the plane, and coating technique is completely embedded semiconductor film and optical fiber, is not influenced half by ambient pressure, vibration etc.
The refractive index of conductor, so that temperature measurement accuracy greatly improves;Ceramic contact pin can fix fiber core, while increase semiconductor film
The area of layer contacts semiconductor film and close fiber optic.A ceramic sleeve is encapsulated outside the ceramic contact pin of plated film.
Zhao Yong, veteran's " fibre optic temperature sensor research based on semiconductor absorber principle ", propose one kind herein
The fibre optic temperature sensor of GaAs transmission-type structure, structure is similar to FC connector used in fiber optic communication, arsenic
Gallium piece is bonded between two contact pins, and optical fiber is inserted into two root cutting needles respectively, and contact pin is fixed with casing, is guaranteed incident optical, is gone out
Penetrate optical fiber and gallium arsenide film point-blank, casing serves fixed and thermally conductive.
A kind of knot of reflective temperature sensor of GaAs is proposed in Wang Yutian " photoelectronics and optical fiber sensing technology "
Structure, it is characterized in that inserting optical fibers into contact pin, incident optical and the output optical fiber share an optical fiber, and gallium arsenide chips plate anti-reflection on one side
Film plates reflectance coating on one side, and the one side for being coated with anti-reflection film is Nian Jie with contact pin, then will entirely be popped one's head in package with metal shell.Enter
The light of optical fiber is penetrated through reflecting after GaAs piece in the end face for being coated with reflectance coating, and is returned after transmission GaAs piece through the output optical fiber
It returns.
The shortcomings that prior art:
(1) temperature-sensitive material is done using semiconductor materials such as silicon, germanium, since these materials are all indirect band-gap semiconductors
Material, its absorption coefficient of light is more much smaller than straight gap semiconductor material, does not have excellent absorbing properties.
(2) it from the point of view of prior art, is fixed by way of bonding using GaAs, germanium as temperature sensing material
To fiber end face, plated film, cutting and packaging technology are complicated.
(3) the Temperature Demodulation System higher cost used.
Summary of the invention
In order to overcome prior art problem, the present invention provides a kind of preparation side of fibre optic temperature sensor cadmium sulphide membrane
Method includes the following steps:
After optical fiber is fixed on lock pin, the exposed end face of the optical fiber is polished;
Plated film: it thiocarbamide, cadmium sulfate is mixed to be dissolved in deionized water with ammonium hydroxide forms reaction solution;The thiocarbamide, cadmium sulfate
The mass ratio of the material be 12~110:1;The ammonium hydroxide volume is 40~50mL;Then the reaction is inserted into the exposed end face
In liquid, using chemical water bath temperature be 60~70 DEG C, complete the plated film of a cadmium sulphide membrane;
It repeats plated film: repeating the plating steps to n times, obtain the exposed end face for being deposited with n+1 layers of cadmium sulphide membrane, n
For the natural number greater than 0;
It will be made annealing treatment at a temperature of 180~220 DEG C by the optical fiber for repeating plating steps acquisition.
Further, the thiocarbamide, cadmium sulfate are made into thiourea solution, cadmium sulfate aqueous solution respectively;The ammonium hydroxide first with
The cadmium sulfate aqueous solution mixing, then be dissolved in the deionized water together with the thiourea solution and form reaction solution.
Further, the mass fraction of the ammonium hydroxide is 28%-35%.
Further, the n is 0~5.
It successively include: incidence the present invention also provides this fibre optic temperature sensor is prepared using above-mentioned cadmium sulphide membrane
Optical fiber, cadmium sulphide membrane and the output optical fiber.
Another fibre optic temperature sensor successively includes: incidence, outgoing common optical fiber, cadmium sulphide membrane and reflectance coating.
The utility model has the advantages that
(1) good to visible light wave range absorbing properties using cadmium sulfide as temperature-sensitive material, when photon energy is greater than
When its forbidden bandwidth energy, the absorption coefficient of light can suddenly be risen.
(2) cadmium sulphide membrane is plated using chemical water bath, this method can make cadmium sulphide film combine closely with fiber end face,
And coating film thickness is controllable.
(3) stability, accuracy are higher, and the plated film directly on the end face of conduction optical fiber eliminates traditional fiber temperature biography
Paste semiconductor chip defect easily affected by environment in sensor end face.
(4) at low cost, the plated film and manufacture craft of fibre optic temperature sensor are all very simple, are convenient for large-scale production.
Detailed description of the invention
Fig. 1 (a) (b) (c) is respectively the cadmium sulphide membrane scanning electron microscope (SEM) photograph that the embodiment of the present invention 1~3 obtains.
Fig. 2 is that the embodiment of the present invention 4~8 obtains cadmium sulphide membrane transmissivity spectrum.
Fig. 3 is that the present invention obtains transmission-type cadmium sulfide fibre optic temperature sensor structural schematic diagram.
Fig. 4 is that the present invention obtains reflective cadmium sulfide fibre optic temperature sensor structural schematic diagram.
Specific embodiment
In the following, will be described in detail in conjunction with attached drawing to the embodiment of the present invention.
The present invention provides a kind of cadmium sulphide membrane preparation method of fibre optic temperature sensor, using CBD (chemical water bath)
Cadmium sulphide membrane is prepared, this method equipment is simple, can be realized batch plated film, the film quality of growth is good, and can realize
Single, multiple or consecutive deposition, therefore be controllable for the thickness of growing film.Prepare the chemical reaction machine of cadmium sulphide membrane
Reason is: being decomposed in the alkaline solution containing cadmium salt based on thiocarbamide, deposits cadmium sulphide membrane.High-temperature cabinet after deposition at 200 DEG C moves back
Fire keeps film more evenly finer and close more smooth.
Specific steps include:
Step S1: fixed optical fiber
Fix optical fiber with fiber stub, in lock pin inject high temperature resistant, soluble glue, solidified glue, make optical fiber with
Lock pin, which is tightly fastened, not to be loosened.
Step S2: grinding optical fiber
After solidification using optic fiber polishing machine polishing, the exposed end face of polishing optical fiber, make the exposed end face of optical fiber and lock pin
End face is in the same plane.Check whether are exposed end face and insertion core end face after exposed end surface grinding on optical fiber end face detector
Smooth, cadmium sulphide membrane is in conjunction with optical fiber densification when the surface of only smooth alignment just can guarantee plated film.
Step S3: in the exposed end face coating of optical fiber
Cadmium sulphide membrane is plated in the end face that the exposed end face of optical fiber is aligned with lock pin using front chemical water bath, plated film is implemented
Method is as follows:
(1) thiocarbamide of certain mass is taken to be dissolved in deionized water, number solution A;
(2) cadmium sulfate of certain mass is taken to be dissolved in deionized water, number solution B;
(3) it measures 40~50mL, the ammonium hydroxide that mass fraction is 28%-35%, is added in solution B and stirs, number solution C;
(4) it measures certain volume deionized water and pours into reactor, solution A and solution C are then poured into reactor and mix shape
At reaction solution, exposed end face one end of optical fiber is immersed in reaction solution.Reactor is put into water-bath, reaction temperature is set
It is 60~70 DEG C, reaction time 9min, so far, one time plated film is completed;
It (5), can be in the multiple plated film in end face, the available different film of different coating times by repeating the above steps
Thickness;
(6) in 180~220 DEG C of high temperature close annealing 1h after reacting, make to obtain it is finer and close, more evenly.
According to above-mentioned preparation method, the present invention has carried out 8 embodiments respectively, and response parameter is as shown in table 1:
The response parameter of 1 Examples 1 to 8 of table
(connecting table)
Examples 1 to 8 realizes the deposition of cadmium sulphide membrane.Wherein, embodiment 1, embodiment 2, embodiment 3 obtain sulphur
The scanning electron microscope (SEM) photograph of cadmium film is referred to respectively shown in Fig. 1 (a) (b) (c), and as shown in Figure 1, the cadmium sulfide that embodiment 1 obtains is thin
Membrane molecule particle is smaller, more evenly, finer and close.
In addition, in conjunction with the embodiments 4~8 it is found that deposited cadmium sulphide membrane respectively on the basis of reaction condition is identical
4 layers, 1 layer, 2 layers, 3 layers and 5 layers, then pass through the transmissivity spectral line of the cadmium sulphide membrane of test different-thickness.Referring to Fig. 1 institute
Show, it is known that at plated film 4 times, the transmissivity line absorption side of (cadmium sulphide membrane there are four layers) is best.
In the following, preparing two different fibre optic temperature sensors using above-mentioned cadmium sulphide membrane.
(2) transmission-type cadmium sulfide fibre optic temperature sensor
As shown in Fig. 2, transmission-type cadmium sulfide fibre optic temperature sensor is mainly by incident optical 1, the output optical fiber 3 and sulphur
2 three parts of cadmium film form, on its end face for being set to the incident optical 3 of cadmium sulphide membrane 2.Light passes through incident optical 1
Into cadmium sulphide membrane 2, after cadmium sulphide membrane 2, unabsorbed light enters the output optical fiber 3, incident optical 1 and cadmium sulfide
Transmission film 2, the output optical fiber 3 pass through fixed device and keep point-blank.
(3) reflective cadmium sulfide fibre optic temperature sensor
As shown in figure 3, reflective cadmium sulfide fibre optic temperature sensor successively includes: incident, outgoing common optical fiber 1, vulcanization
Cadmium film 2 and reflectance coating 3.Incident, outgoing common optical fiber 1 is that incident optical and the output optical fiber share an optical fiber;Vulcanization
It is set in incident, the outgoing common optical fiber 1 cadmium film 2, the exposed end face of optical fiber plate cadmium sulphide membrane 2 and then
One layer of reflectance coating 3 is plated, light enters cadmium sulphide membrane 2, then reflect through reflectance coating 3 by incident, outgoing common optical fiber 1, again
Incident, outgoing common optical fiber 1 is returned to through cadmium sulphide membrane 2.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (6)
1. a kind of preparation method of fibre optic temperature sensor cadmium sulphide membrane, which comprises the steps of:
After optical fiber is fixed on lock pin, the exposed end face of the optical fiber is polished;
Plated film: it thiocarbamide, cadmium sulfate is mixed to be dissolved in deionized water with ammonium hydroxide forms reaction solution;The object of the thiocarbamide, cadmium sulfate
The amount ratio of matter is 12~110:1;The ammonium hydroxide volume is 40~50mL;Then the reaction solution is inserted into the exposed end face
In, using chemical water bath temperature be 60~70 DEG C, complete the plated film of a cadmium sulphide membrane;
It repeats plated film: repeating the plating steps to n times, obtain the exposed end face for being deposited with n+1 layers of cadmium sulphide membrane, n is big
In 0 natural number;
It will be made annealing treatment at a temperature of 180~220 DEG C by the optical fiber for repeating plating steps acquisition.
2. the preparation method of fibre optic temperature sensor cadmium sulphide membrane according to claim 1, which is characterized in that the sulphur
Urea, cadmium sulfate are made into thiourea solution, cadmium sulfate aqueous solution respectively;The ammonium hydroxide is first mixed with the cadmium sulfate aqueous solution, then
It is dissolved in the deionized water together with the thiourea solution and forms reaction solution.
3. the preparation method of fibre optic temperature sensor cadmium sulphide membrane according to claim 1, which is characterized in that the ammonium hydroxide
Mass fraction be 28%-35%.
4. the preparation method of fibre optic temperature sensor cadmium sulphide membrane according to claim 1, which is characterized in that the n is 1
~5.
5. a kind of fibre optic temperature sensor, which is characterized in that successively include: incident optical, preparation method as described in claim 1
The cadmium sulphide membrane and the output optical fiber of acquisition.
6. a kind of fibre optic temperature sensor, which is characterized in that successively include: incidence, outgoing common optical fiber, such as claim 1 institute
State the cadmium sulphide membrane and reflectance coating of preparation method acquisition.
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CN114540781A (en) * | 2022-02-23 | 2022-05-27 | 宁波大学 | Chalcogenide optical fiber end face coating method |
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WO1994012859A1 (en) * | 1992-11-25 | 1994-06-09 | Minnesota Mining And Manufacturing Company | Temperature sensor for medical application |
US5547283A (en) * | 1994-11-01 | 1996-08-20 | Kronberg; James W. | Optical temperature sensor using thermochromic semiconductors |
CN1945246A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | Thin film type optical fiber temperature sensor and its temperature sensing method |
CN102235919A (en) * | 2010-04-23 | 2011-11-09 | 上海华魏光纤传感技术有限公司 | Semiconductor reflection type optical fiber temperature sensor |
CN102299211A (en) * | 2011-09-21 | 2011-12-28 | 上海大学 | Two-step method for manufacturing cadmium sulphide film |
CN105203226A (en) * | 2015-09-09 | 2015-12-30 | 姚胜利 | Optical fiber temperature sensor |
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US20060274813A9 (en) * | 2002-06-06 | 2006-12-07 | Wei Chen | Nanoparticle thermometry and pressure sensors |
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Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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WO1994012859A1 (en) * | 1992-11-25 | 1994-06-09 | Minnesota Mining And Manufacturing Company | Temperature sensor for medical application |
US5547283A (en) * | 1994-11-01 | 1996-08-20 | Kronberg; James W. | Optical temperature sensor using thermochromic semiconductors |
CN1945246A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | Thin film type optical fiber temperature sensor and its temperature sensing method |
CN100526821C (en) * | 2006-10-20 | 2009-08-12 | 中山大学 | Thin film type optical fiber temperature sensor and its temperature sensing method |
CN102235919A (en) * | 2010-04-23 | 2011-11-09 | 上海华魏光纤传感技术有限公司 | Semiconductor reflection type optical fiber temperature sensor |
CN102299211A (en) * | 2011-09-21 | 2011-12-28 | 上海大学 | Two-step method for manufacturing cadmium sulphide film |
CN105203226A (en) * | 2015-09-09 | 2015-12-30 | 姚胜利 | Optical fiber temperature sensor |
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