CN109781254A - A kind of method of taper micro-nano fiber surface growing ZnO nanorod structure - Google Patents
A kind of method of taper micro-nano fiber surface growing ZnO nanorod structure Download PDFInfo
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- CN109781254A CN109781254A CN201910128407.5A CN201910128407A CN109781254A CN 109781254 A CN109781254 A CN 109781254A CN 201910128407 A CN201910128407 A CN 201910128407A CN 109781254 A CN109781254 A CN 109781254A
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Abstract
A kind of method of taper micro-nano fiber of the invention surface growing ZnO nanorod structure belongs to oil recovery technique field；This method configures ZnO seed solution first, and then with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips on cleaned taper micro-nano fiber, its surface is set to be stained with seed layer, it is repeated 3 times, places into 150 degrees Celsius of annealing 30min in drying box, repeat 4 times emphatically；It is reconfigured growth solution；Then the growing ZnO nanorod in substrate；The optical fiber of growing ZnO nanorod is taken out from growth solution finally, is cleaned by ultrasonic 2min with deionized water, places into 80 degrees Celsius of dry 2h in drying box；The method of taper micro-nano fiber of the present invention surface growing ZnO nanorod structure is for making fiber mix waveguide, prepared fiber mix waveguide is used for oil well Extraction rate detection device, and cooperate oil well Extraction rate detection method, it can be realized the technical purpose of detection oil well Extraction rate.
Description
Technical field
A kind of method of taper micro-nano fiber of the invention surface growing ZnO nanorod structure belongs to oil recovery technique field.
Background technique
PetroChina Company Ltd. and Daqing Oil Field Co., Ltd its application No. is
It points out, adopts in a kind of 2016105892521 patent of invention " beam pumping unit work in combination system formula pumping operation method "
During oil, under the insufficient operating condition of stripper well feed flow, it is often necessary to reduce individual well theoretical displacement.
In fact, two reduction individual wells just have been disclosed in Harbin Suo Fei electrical technology Co., Ltd in the time earlier
The technological means of theoretical displacement is that application No. is 2015107838762 patents of invention " to be moved based on the non-complete cycle of crank respectively
The non-pumping operation method of beam pumping unit " and application No. is 2015108388310 patents of invention " based on the non-complete cycle fortune of crank
Dynamic beam pumping unit dynamic becomes stroke operation method ".
As it can be seen that i.e. oil well is under the slow operating condition of Extraction rate, under the insufficient operating condition of stripper well feed flow in order to more rationally
Ground recovers the oil, and needs to change pumping strategy, this explanation, oil well Extraction rate is very important one for entire oil recovery process
Item technical indicator, it would be desirable to monitoring or detection oil well Extraction rate.However, finding very easy device and side not yet
Method realizes the technical purpose.
Harbin University of Science and Technology application application No. is 2019100516319 patent of invention " one kind be based on ZnO nano
Stick/micro-nano fiber hybrid waveguide ultraviolet detector " a kind of UV detector structure is disclosed, it can be changed using photo-generated carrier
Become the principle of ZnO refractive index, be based on membrane type structure, tests UV intensity using transmitted spectrum Strength Changes, realize sensitive
Spend the production of higher ultraviolet detector.
Summary of the invention
For the technical need of oil well Extraction rate detection, in combination with ultraviolet detection disclosed in Harbin University of Science and Technology
Device, the invention discloses a kind of oil well Extraction rate detection device and method based on ultraviolet detection being capable of, systems simple in structure
On the basis of making low-cost detection device, with simple method, realizes the detection of oil well Extraction rate, rationally acquire and establish for petroleum
Theoretical and experiment basis is determined.
The object of the present invention is achieved like this:
Oil well Extraction rate detection device based on ultraviolet detection, including detection pipeline road and ultraviolet detector,
Detection pipeline road includes conventional pipeline road and signal piping, is led between conventional pipeline road and signal piping
Valve transfer is crossed, the signal piping is made by transparent material, and the volume of signal piping is that beam type oil pumping machine crank is whole
Under all operating statuses at polished rod stroke and polished rod oil transportation path cross section product product, be provided with heating dress on the signal piping
It sets, the heating device is by storage battery power supply, and the battery connects solar panel, and solar panel is for receiving too
Positive energy, converts solar energy into electrical energy and is stored in battery；
The ultraviolet detector select 1530nm as sensing wavelength progress signal demodulation, including solar panel, battery,
ASE wideband light source, input single mode optical fiber, ZnO nanorod-micro-nano fiber hybrid waveguide, output single mode optical fiber and spectrometer；
The solar panel connects battery, and solar panel is converted solar energy into electrical energy for receiving solar energy
It is stored in battery；
The battery connection ASE wideband light source and spectrometer, for providing electric energy to ASE wideband light source and spectrometer；
The ASE wideband light source is used to generate optical signal, wherein a length of 1550nm of cardiac wave, bandwidth 80nm；
The input single mode optical fiber is used to receive the optical signal of ASE wideband light source, and optical signal transmission is micro- to ZnO nanorod-
Nano fiber hybrid waveguide；
The ZnO nanorod-micro-nano fiber hybrid waveguide input terminal and input single mode optical fiber align welding, output end and output
Single mode optical fiber aligns welding, detects for ultraviolet signal；ZnO nanorod-micro-nano fiber hybrid waveguide includes taper micro-nano
Optical fiber and ZnO nanorod structure, the taper micro-nano fiber are formed by a single mode optical fiber through fused biconical taper, and cone waist diameter is 4
The cone area of micron, taper micro-nano fiber is coated ZnO nanorod structure；ZnO nanorod-micro-nano fiber hybrid waveguide is by ultraviolet light spoke
According to when, cone area's evanscent field changes with irradiation intensity, to change ZnO nanorod-micro-nano fiber hybrid waveguide output light letter
Number optical power；
It exports single mode optical fiber and ZnO nanorod-micro-nano fiber hybrid waveguide output optical signal is sent into spectrometer；
The optical signal that the spectrometer exports output single mode optical fiber carries out spectral detection, and is obtained accordingly according to detection structure
Obtain detection data.
Oil well Extraction rate detection method based on ultraviolet detection, comprising the following steps:
Step a, valve is adjusted, is connected to the signal piping in detection pipeline road with oil transportation path at polished rod；
Step b, beam type oil pumping machine crank is run one week according to the period complete cycle of regulation；
Step c, valve is adjusted, the oil drawn up during step b is stored in signal piping；
Step d, start heating device, signal piping is heated, will test pipeline heating to defined temperature, or to detection
Time as defined in pipeline heating；
Step e, the optical signal that the described spectrometer exports output single mode optical fiber carries out spectral detection；
Step f, according to the corresponding relationship of spectrum and ultraviolet radiation, ultraviolet radiation is determined；The spectrum and ultraviolet radiation
Corresponding relationship, can be obtained by scaling method；
Step g, according to the corresponding relationship of ultraviolet radiation and petroleum volume, petroleum volume, i.e. beam type oil pumping machine crank are determined
Oil production rate when being run one week according to the period complete cycle of regulation；The corresponding relationship of the ultraviolet radiation and petroleum volume, energy
Enough obtained by scaling method.
A kind of detection pipeline road, including conventional pipeline road and signal piping, conventional pipeline road and signal piping
Between by valve transfer, the signal piping is made by transparent material, and the volume of signal piping is beam pumping unit
Under crank complete cycle operating status at polished rod stroke and polished rod oil transportation path cross section product product, be provided on the signal piping
Heating device, the heating device connect solar panel by storage battery power supply, the battery, and solar panel is used for
Solar energy is received, converts solar energy into electrical energy and is stored in battery.
A kind of ultraviolet detector selectes 1530nm as sensing wavelength and carries out signal demodulation, including solar panel, storage
Battery, ASE wideband light source, input single mode optical fiber, ZnO nanorod-micro-nano fiber hybrid waveguide, output single mode optical fiber and spectrum
Instrument；
The solar panel connects battery, and solar panel is converted solar energy into electrical energy for receiving solar energy
It is stored in battery；
The battery connection ASE wideband light source and spectrometer, for providing electric energy to ASE wideband light source and spectrometer；
The ASE wideband light source is used to generate optical signal, wherein a length of 1550nm of cardiac wave, bandwidth 80nm；
The input single mode optical fiber is used to receive the optical signal of ASE wideband light source, and optical signal transmission is micro- to ZnO nanorod-
Nano fiber hybrid waveguide；
The ZnO nanorod-micro-nano fiber hybrid waveguide input terminal and input single mode optical fiber align welding, output end and output
Single mode optical fiber aligns welding, detects for ultraviolet signal；ZnO nanorod-micro-nano fiber hybrid waveguide includes taper micro-nano
Optical fiber and ZnO nanorod structure, the taper micro-nano fiber are formed by a single mode optical fiber through fused biconical taper, and cone waist diameter is 4
The cone area of micron, taper micro-nano fiber is coated ZnO nanorod structure；ZnO nanorod-micro-nano fiber hybrid waveguide is by ultraviolet light spoke
According to when, cone area's evanscent field changes with irradiation intensity, to change ZnO nanorod-micro-nano fiber hybrid waveguide output light letter
Number optical power；
It exports single mode optical fiber and ZnO nanorod-micro-nano fiber hybrid waveguide output optical signal is sent into spectrometer；
The optical signal that the spectrometer exports output single mode optical fiber carries out spectral detection, and is obtained accordingly according to detection structure
Obtain detection data.
A kind of ZnO nanorod for ultraviolet detector-micro-nano fiber hybrid waveguide, including taper micro-nano fiber and ZnO
Nanorod structure, the taper micro-nano fiber are formed by a single mode optical fiber through fused biconical taper, and cone waist diameter is 4 microns, taper
The cone area of micro-nano fiber is coated ZnO nanorod structure；When ZnO nanorod-micro-nano fiber hybrid waveguide is by ultraviolet light irradiation, area is bored
Evanscent field changes with irradiation intensity, to change ZnO nanorod-micro-nano fiber hybrid waveguide output optical signal light function
Rate.
A kind of method of taper micro-nano fiber surface growing ZnO nanorod structure, comprising the following steps:
Step a, ZnO seed solution: zinc acetate 0.01M is configured, wherein M is mol/L, is configured to 5 parts of identical 40ml zinc acetates
Ethanol solution, and sodium hydroxide configures the 20mL sodium hydroxide ethanol solution of 5 kinds of various concentrations, by the above zinc acetate
Ethanol solution stirs on one side with sodium hydroxid ethanol solution, mixes on one side, and the seed for being prepared into 5 kinds of various concentrations is molten
Liquid, solution concentration are respectively 0.010M, 0.015M, 0.020M, 0.025M and 0.030M, and selected OH ion concentration is
0.015M；It is poured into beaker after mixing, 60 C water baths stir 2h under magnetic stirring apparatus, are up to there is white precipitate
Only, it seals up and places 18h, the sediment of bulky grain is allowed to be deposited to bottom of bottle by gravity；
Step b, with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips to cleaned taper micro-nano light
On fibre, so that its surface is stained with seed layer, be repeated 3 times, place into 150 degrees Celsius of annealing 30min in drying box, repeats 4 times emphatically；
Step c, configure growth solution: zinc nitrate 0.01M is configured to the zinc nitrate aqueous solution of 200m1；Hexamethylenetetramine
0.01M is configured to the hexamethylenetetramine aqueous solution of 200m1；Under magnetic stirring, 2 kinds of solution are uniformly mixed；
Step d, growing ZnO nanorod in substrate: the optical fiber of kind is put into growth solution, is closed to be placed on thermostatic drying chamber
Lower 95 degrees Centigrades, by the length of heating time control ZnO nanorod；
Step e, the optical fiber of growing ZnO nanorod is taken out from growth solution, is cleaned by ultrasonic 2min with deionized water, places into
80 degrees Celsius of dry 2h in drying box.
A kind of ultraviolet detection method, the broadband optical signal of ASE wideband light source output enter ZnO nano through inputting single mode optical fiber
Stick-micro-nano fiber hybrid waveguide, when ZnO nanorod-micro-nano fiber hybrid waveguide is by ultraviolet irradiation, ZnO nanorod structure folding
The rate of penetrating changes, and then ZnO nanorod-micro-nano fiber hybrid waveguide evanscent field changes, and leads to the strong of output optical signal
Degree changes, and output optical signal intensity, with the linear rule variation of ultraviolet irradiation intensity, output optical signal passes through spectrum
Instrument carries out signal acquisition and processing, and it is strong to calculate ultraviolet irradiation according to light signal strength.
A kind of production method of ultraviolet detector described in claim 4, comprising the following steps:
Step a, taper micro-nano fiber is prepared
Optical fiber coating is removed into 3cm, then dips alcohol wipe optical fiber with dust-free paper, and optical fiber is fixed on fused fiber splice
On machine；Welding strength of discharge is changed to 5% by customized setting fused fiber splice mode, and discharge time reaches maximum value 4000ms；It is logical
The variation for crossing online observation spectrometer transmitted spectrum determines the parameter of micro-nano fiber；
Step b, ZnO nanorod-micro-nano fiber hybrid waveguide is prepared
The following steps are included:
Step b1, ZnO seed solution: zinc acetate 0.01M is configured, wherein M is mol/L, is configured to 5 parts of identical 40ml zinc acetates
Ethanol solution, and sodium hydroxide configures the 20mL sodium hydroxide ethanol solution of 5 kinds of various concentrations, by the above zinc acetate
Ethanol solution stirs on one side with sodium hydroxid ethanol solution, mixes on one side, and the seed for being prepared into 5 kinds of various concentrations is molten
Liquid, solution concentration are respectively 0.010M, 0.015M, 0.020M, 0.025M and 0.030M, and selected OH ion concentration is
0.015M；It is poured into beaker after mixing, 60 C water baths stir 2h under magnetic stirring apparatus, are up to there is white precipitate
Only, it seals up and places 18h, the sediment of bulky grain is allowed to be deposited to bottom of bottle by gravity；
Step b2, with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips to cleaned taper micro-nano
On optical fiber, so that its surface is stained with seed layer, be repeated 3 times, place into 150 degrees Celsius of annealing 30min in drying box, repeats to focus on 4
It is secondary；
Step b3, configure growth solution: zinc nitrate 0.01M is configured to the zinc nitrate aqueous solution of 200m1；Hexamethylenetetramine
0.01M is configured to the hexamethylenetetramine aqueous solution of 200m1；Under magnetic stirring, 2 kinds of solution are uniformly mixed；
Step b4, growing ZnO nanorod in substrate: the optical fiber of kind is put into growth solution, is closed to be placed on freeze-day with constant temperature
95 degrees Centigrade under case, by the length of heating time control ZnO nanorod；
Step b5, the optical fiber of growing ZnO nanorod is taken out from growth solution, is cleaned by ultrasonic 2min with deionized water, then put
Enter 80 degrees Celsius of dry 2h in drying box；
Step c, it assembles
The ZnO nanorod that step b is obtained-micro-nano fiber hybrid waveguide one end passes through input single mode optical fiber and ASE broadband light
Source is connected, and the other end is connected by exporting single mode optical fiber with spectrometer.
The utility model has the advantages that
The first, the invention discloses a kind of detection pipeline road, including conventional pipeline road and signal piping, conventional petroleum pipelines
By valve transfer between road and signal piping, the signal piping is made by transparent material, and the volume of signal piping is
The product of polished rod stroke and oil transportation path cross section product at polished rod, the detection under beam type oil pumping machine crank complete cycle operating status
Heating device is provided on pipeline；Under this configuration, beam type oil pumping machine crank can not only be stored according to the period of regulation
Complete cycle runs the petroleum of one week when institute's pumping, and can handle petroleum, using radiation theory, realizes to UV signal
Amplification.
The second, present invention improves over Harbin University of Science and Technology application application No. is 2019100516319 patents of invention
" a kind of based on ZnO nanorod/micro-nano fiber hybrid waveguide ultraviolet detector ", increases solar panel and battery,
So that entire ultraviolet detector may be completely independent of power environment and work.
Third, the present invention combine designed detection with pipeline road with improved ultraviolet detector, realize inspection
The technical purpose of oil well Extraction rate is surveyed, and is compared compared with method, not only detection can be completed in scene, and having does not influence just
The beneficial effect often recovered the oil, and have that structure of the detecting device is simple, cost of manufacture is cheap, detection method step is few, and operation is held
Easily.
Detailed description of the invention
Fig. 1 is the oil well Extraction rate structure of the detecting device schematic diagram based on ultraviolet detection.
Fig. 2 is detection pipeline road structural schematic diagram.
Fig. 3 is UV detector structure schematic diagram.
Fig. 4 is ZnO nanorod-micro-nano fiber mixed wave guide structure schematic diagram.
In figure: 1 detection with pipeline road, 1-1 routine pipeline road, 1-2 signal piping, 1-3 valve, 1-4 heating device,
2 ultraviolet detectors, 2-1 solar panel, 2-2 battery, 2-3 ASE wideband light source, 2-4 input single mode optical fiber, 2-5 ZnO
Nanometer rods-micro-nano fiber hybrid waveguide, 2-5-1 taper micro-nano fiber, 2-5-2ZnO nanorod structure, 2-6 output single mode optical fiber,
2-7 spectrometer.
Specific embodiment
The specific embodiment of the invention is described in further detail with reference to the accompanying drawing.
Specific embodiment one
The present embodiment is the embodiment of the oil well Extraction rate detection device based on ultraviolet detection.
The oil well Extraction rate detection device based on ultraviolet detection of the present embodiment, as shown in Figure 1, the oil well Extraction rate
Detection device includes detection pipeline road 1 and ultraviolet detector 2,
Detection pipeline road 1 is as shown in Fig. 2, detection pipeline road includes routine pipeline road 1-1 and detection pipe
Road 1-2 is switched between conventional pipeline road 1-1 and signal piping 1-2 by valve 1-3, and the signal piping 1-2 is by transparent material
Material is made, and the volume of signal piping 1-2 is under beam type oil pumping machine crank complete cycle operating status at polished rod stroke and polished rod
The product of oil transportation path cross section product, is provided with heating device 1-4 on the signal piping 1-2, the heating device 1-4 is by storing
Battery 2-2 power supply, the battery 2-2 connection solar panel 2-1, solar panel 2-1, will for receiving solar energy
Solar energy is converted into power storage in battery 2-2；It should be noted that the structure in attached drawing 2 is only schematic diagram, it cannot
It is interpreted as realizing the unique method of detection pipeline road 1, as long as including the necessity such as conventional pipeline road 1-1, signal piping 1-2
Technical characteristic, all in its protection scope；
The ultraviolet detector 2, as shown in Figure 3 and Figure 4, the ultraviolet detector 2 select 1530nm as sensing wavelength and carry out letter
Number demodulation, including solar panel 2-1, battery 2-2, ASE wideband light source 2-3, input single mode optical fiber 2-4, ZnO nano
Stick-micro-nano fiber hybrid waveguide 2-5, output single mode optical fiber 2-6 and spectrometer 2-7；
The solar panel 2-1 connection battery 2-2, solar panel 2-1 turn solar energy for receiving solar energy
Power storage is turned in battery 2-2；
Battery 2-2 connection the ASE wideband light source 2-3 and spectrometer 2-7, for ASE wideband light source 2-3 and spectrometer 2-
7 provide electric energy；
The ASE wideband light source 2-3 is used to generate optical signal, wherein a length of 1550nm of cardiac wave, bandwidth 80nm；
The input single mode optical fiber 2-4 is used to receive the optical signal of ASE wideband light source 2-3, and by optical signal transmission to ZnO nano
Stick-micro-nano fiber hybrid waveguide 2-5；
The ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 input terminal and input single mode optical fiber 2-4 align welding, output end
Welding is aligned with output single mode optical fiber 2-6, is detected for ultraviolet signal；ZnO nanorod-micro-nano fiber hybrid waveguide 2-5
Including taper micro-nano fiber 2-5-1 and ZnO nanorod structure 2-5-2, the taper micro-nano fiber 2-5-1 is by a single mode optical fiber
It is formed through fused biconical taper, cone waist diameter is 4 microns, and the cone area of taper micro-nano fiber 2-5-1 is coated ZnO nanorod structure 2-5-2；
When ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 is by ultraviolet light irradiation, cone area's evanscent field changes with irradiation intensity, thus
Change ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 output optical signal optical power；
It exports single mode optical fiber 2-6 and ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 output optical signal is sent into spectrometer 2-7；
The spectrometer 2-7 carries out spectral detection to the output single mode optical fiber 2-6 optical signal exported, and according to detection structure phase
The acquisition detection data answered.
Specific embodiment two
The present embodiment is the embodiment of the oil well Extraction rate detection method based on ultraviolet detection.
The oil well Extraction rate detection method based on ultraviolet detection of the present embodiment, the base documented by specific embodiment one
It is realized in the oil well Extraction rate detection device of ultraviolet detection, detection method includes the following steps for the oil well Extraction rate:
Step a, valve 1-3 is adjusted, is connected to the signal piping 1-2 in detection pipeline road 1 with oil transportation path at polished rod；
Step b, beam type oil pumping machine crank is run one week according to the period complete cycle of regulation；
Step c, valve 1-3 is adjusted, the oil drawn up during step b is stored in signal piping 1-2；
Step d, start heating device 1-4, signal piping 1-2 is heated, pipeline 1-2 is will test and is heated to defined temperature
Degree, or the defined time is heated to signal piping 1-2；
Step e, the described spectrometer 2-7 carries out spectral detection to the output single mode optical fiber 2-6 optical signal exported；
Step f, according to the corresponding relationship of spectrum and ultraviolet radiation, ultraviolet radiation is determined；The spectrum and ultraviolet radiation
Corresponding relationship, can be obtained by scaling method；
Step g, according to the corresponding relationship of ultraviolet radiation and petroleum volume, petroleum volume, i.e. beam type oil pumping machine crank are determined
Oil production rate when being run one week according to the period complete cycle of regulation；The corresponding relationship of the ultraviolet radiation and petroleum volume, energy
Enough obtained by scaling method.
Specific embodiment three
The present embodiment is the embodiment of detection pipeline road.
The detection pipeline road of the present embodiment, as shown in Fig. 2, detection pipeline road includes conventional pipeline road 1-
1 and signal piping 1-2, is switched between conventional pipeline road 1-1 and signal piping 1-2 by valve 1-3, the signal piping 1-
2 are made by transparent material, and the volume of signal piping 1-2 is polished rod stroke under beam type oil pumping machine crank complete cycle operating status
With the product of oil transportation path cross section product at polished rod, heating device 1-4 is provided on the signal piping 1-2, the heating fills
It sets 1-4 to be powered by battery 2-2, the battery 2-2 connection solar panel 2-1, solar panel 2-1 are for receiving
Solar energy is converted solar energy into electrical energy and is stored in battery 2-2.
It should be noted that the structure in attached drawing 2 is only schematic diagram, should not be understood as realizing detection pipeline road 1
Unique method, as long as including the essential features such as conventional pipeline road 1-1, signal piping 1-2, all in its protection scope
It is interior.
Specific embodiment four
The present embodiment is the embodiment of ultraviolet detector.
The ultraviolet detector of the present embodiment, as shown in Figure 3 and Figure 4, the ultraviolet detector select 1530nm as sensing wave
It is long to carry out signal demodulation, including solar panel 2-1, battery 2-2, ASE wideband light source 2-3, input single mode optical fiber 2-4,
ZnO nanorod-micro-nano fiber hybrid waveguide 2-5, output single mode optical fiber 2-6 and spectrometer 2-7；
The solar panel 2-1 connection battery 2-2, solar panel 2-1 turn solar energy for receiving solar energy
Power storage is turned in battery 2-2；
Battery 2-2 connection the ASE wideband light source 2-3 and spectrometer 2-7, for ASE wideband light source 2-3 and spectrometer 2-
7 provide electric energy；
The ASE wideband light source 2-3 is used to generate optical signal, wherein a length of 1550nm of cardiac wave, bandwidth 80nm；
The input single mode optical fiber 2-4 is used to receive the optical signal of ASE wideband light source 2-3, and by optical signal transmission to ZnO nano
Stick-micro-nano fiber hybrid waveguide 2-5；
The ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 input terminal and input single mode optical fiber 2-4 align welding, output end
Welding is aligned with output single mode optical fiber 2-6, is detected for ultraviolet signal；ZnO nanorod-micro-nano fiber hybrid waveguide 2-5
Including taper micro-nano fiber 2-5-1 and ZnO nanorod structure 2-5-2, the taper micro-nano fiber 2-5-1 is by a single mode optical fiber
It is formed through fused biconical taper, cone waist diameter is 4 microns, and the cone area of taper micro-nano fiber 2-5-1 is coated ZnO nanorod structure 2-5-2；
When ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 is by ultraviolet light irradiation, cone area's evanscent field changes with irradiation intensity, thus
Change ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 output optical signal optical power；
It exports single mode optical fiber 2-6 and ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 output optical signal is sent into spectrometer 2-7；
The spectrometer 2-7 carries out spectral detection to the output single mode optical fiber 2-6 optical signal exported, and according to detection structure phase
The acquisition detection data answered.
Specific embodiment five
The present embodiment is ZnO nanorod-micro-nano fiber hybrid waveguide embodiment for ultraviolet detector.
ZnO nanorod for the ultraviolet detector-micro-nano fiber hybrid waveguide of the present embodiment, as shown in figure 4, the mixing
Waveguide includes taper micro-nano fiber 2-5-1 and ZnO nanorod structure 2-5-2, and the taper micro-nano fiber 2-5-1 is by a single mode
Optical fiber is formed through fused biconical taper, and cone waist diameter is 4 microns, and the cone area of taper micro-nano fiber 2-5-1 is coated ZnO nanorod structure 2-
5-2；When ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 is by ultraviolet light irradiation, cone area's evanscent field changes with irradiation intensity,
To change ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 output optical signal optical power.
Specific embodiment six
The present embodiment is the embodiment of taper micro-nano fiber surface growing ZnO nanorod structural approach.
The method of the taper micro-nano fiber surface growing ZnO nanorod structure of the present embodiment, the taper micro-nano fiber table
Face growing ZnO nanorod structure is structure documented by specific embodiment five, method includes the following steps:
Step a, ZnO seed solution: zinc acetate 0.01M is configured, wherein M is mol/L, is configured to 5 parts of identical 40ml zinc acetates
Ethanol solution, and sodium hydroxide configures the 20mL sodium hydroxide ethanol solution of 5 kinds of various concentrations, by the above zinc acetate
Ethanol solution stirs on one side with sodium hydroxid ethanol solution, mixes on one side, and the seed for being prepared into 5 kinds of various concentrations is molten
Liquid, solution concentration are respectively 0.010M, 0.015M, 0.020M, 0.025M and 0.030M, and selected OH ion concentration is
0.015M；It is poured into beaker after mixing, 60 C water baths stir 2h under magnetic stirring apparatus, are up to there is white precipitate
Only, it seals up and places 18h, the sediment of bulky grain is allowed to be deposited to bottom of bottle by gravity；
Step b, with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips to cleaned taper micro-nano light
On fibre, so that its surface is stained with seed layer, be repeated 3 times, place into 150 degrees Celsius of annealing 30min in drying box, repeats 4 times emphatically；
Step c, configure growth solution: zinc nitrate 0.01M is configured to the zinc nitrate aqueous solution of 200m1；Hexamethylenetetramine
0.01M is configured to the hexamethylenetetramine aqueous solution of 200m1；Under magnetic stirring, 2 kinds of solution are uniformly mixed；
Step d, growing ZnO nanorod in substrate: the optical fiber of kind is put into growth solution, is closed to be placed on thermostatic drying chamber
Lower 95 degrees Centigrades, by the length of heating time control ZnO nanorod；
Step e, the optical fiber of growing ZnO nanorod is taken out from growth solution, is cleaned by ultrasonic 2min with deionized water, places into
80 degrees Celsius of dry 2h in drying box.
Specific embodiment seven
The present embodiment is the embodiment of ultraviolet detection method.
The ultraviolet detection method of the present embodiment is realized on the ultraviolet detector documented by specific embodiment four, in the purple
In outer detection method, the broadband optical signal of ASE wideband light source 2-3 output is inputted single mode optical fiber 2-4, and to enter ZnO nanorod-micro-
Nano fiber hybrid waveguide 2-5, when ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 is by ultraviolet irradiation, ZnO nanorod structure
2-5-2 refractive index changes, and then ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 evanscent field changes, and causes to export
The intensity of optical signal changes, and output optical signal intensity is with the linear rule variation of ultraviolet irradiation intensity, output light letter
Number signal acquisition and processing are carried out by spectrometer 2-7, it is strong to calculate ultraviolet irradiation according to light signal strength.
Specific embodiment eight
The present embodiment is the embodiment of ultraviolet detector production method.
The production method of the ultraviolet detector of the present embodiment makes ultraviolet detector documented by specific embodiment four, should
Production method the following steps are included:
Step a, taper micro-nano fiber 2-5-1 is prepared
Optical fiber coating is removed into 3cm, then dips alcohol wipe optical fiber with dust-free paper, and optical fiber is fixed on fused fiber splice
On machine；Welding strength of discharge is changed to 5% by customized setting fused fiber splice mode, and discharge time reaches maximum value 4000ms；It is logical
The variation for crossing online observation spectrometer transmitted spectrum determines the parameter of micro-nano fiber；
Step b, ZnO nanorod-micro-nano fiber hybrid waveguide 2-5 is prepared
The following steps are included:
Step b1, ZnO seed solution: zinc acetate 0.01M is configured, wherein M is mol/L, is configured to 5 parts of identical 40ml zinc acetates
Ethanol solution, and sodium hydroxide configures the 20mL sodium hydroxide ethanol solution of 5 kinds of various concentrations, by the above zinc acetate
Ethanol solution stirs on one side with sodium hydroxid ethanol solution, mixes on one side, and the seed for being prepared into 5 kinds of various concentrations is molten
Liquid, solution concentration are respectively 0.010M, 0.015M, 0.020M, 0.025M and 0.030M, and selected OH ion concentration is
0.015M；It is poured into beaker after mixing, 60 C water baths stir 2h under magnetic stirring apparatus, are up to there is white precipitate
Only, it seals up and places 18h, the sediment of bulky grain is allowed to be deposited to bottom of bottle by gravity；
Step b2, with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips to cleaned taper micro-nano
On optical fiber, so that its surface is stained with seed layer, be repeated 3 times, place into 150 degrees Celsius of annealing 30min in drying box, repeats to focus on 4
It is secondary；
Step b3, configure growth solution: zinc nitrate 0.01M is configured to the zinc nitrate aqueous solution of 200m1；Hexamethylenetetramine
0.01M is configured to the hexamethylenetetramine aqueous solution of 200m1；Under magnetic stirring, 2 kinds of solution are uniformly mixed；
Step b4, growing ZnO nanorod in substrate: the optical fiber of kind is put into growth solution, is closed to be placed on freeze-day with constant temperature
95 degrees Centigrade under case, by the length of heating time control ZnO nanorod；
Step b5, the optical fiber of growing ZnO nanorod is taken out from growth solution, is cleaned by ultrasonic 2min with deionized water, then put
Enter 80 degrees Celsius of dry 2h in drying box；
Step c, it assembles
The one end the ZnO nanorod that step b is obtained-micro-nano fiber hybrid waveguide 2-5 passes through input single mode optical fiber 2-4 and ASE
Wideband light source 2-3 is connected, and the other end is connected by exporting single mode optical fiber 2-6 with spectrometer 2-7.
It should be noted that in the embodiment above, as long as reconcilable technical solution can carry out permutation and combination, this
Field technical staff can be according to the exhaustive all possibility of mathematical knowledge of permutation and combination, and therefore, the present invention is no longer to permutation and combination
Technical solution afterwards is illustrated one by one, but it is understood that presently disclosed for the technical solution after permutation and combination.
It should be noted that above embodiments is only a kind of specific embodiment of the invention.It is clear that the invention is not restricted to
Above embodiments, can also be there are many deforming, in short, those skilled in the art can be direct from present disclosure
All deformations for exporting or associating, are considered as protection scope of the present invention.
Claims (3)
1. a kind of method of taper micro-nano fiber surface growing ZnO nanorod structure, which comprises the following steps:
Step a, ZnO seed solution: zinc acetate 0.01M is configured, wherein M is mol/L, is configured to 5 parts of identical 40ml zinc acetates
Ethanol solution, and sodium hydroxide configures the 20mL sodium hydroxide ethanol solution of 5 kinds of various concentrations, by the above zinc acetate
Ethanol solution stirs on one side with sodium hydroxid ethanol solution, mixes on one side, and the seed for being prepared into 5 kinds of various concentrations is molten
Liquid, solution concentration are respectively 0.010M, 0.015M, 0.020M, 0.025M and 0.030M, and selected OH ion concentration is
0.015M；It is poured into beaker after mixing, 60 C water baths stir 2h under magnetic stirring apparatus, are up to there is white precipitate
Only, it seals up and places 18h, the sediment of bulky grain is allowed to be deposited to bottom of bottle by gravity；
Step b, with rubber head dropper, by seed solution, clear solution is sucked out from beaker at the middle and upper levels, drips to cleaned taper micro-nano light
On fibre, so that its surface is stained with seed layer, be repeated 3 times, place into 150 degrees Celsius of annealing 30min in drying box, repeats 4 times emphatically；
Step c, configure growth solution: zinc nitrate 0.01M is configured to the zinc nitrate aqueous solution of 200m1；Hexamethylenetetramine
0.01M is configured to the hexamethylenetetramine aqueous solution of 200m1；Under magnetic stirring, 2 kinds of solution are uniformly mixed；
Step d, growing ZnO nanorod in substrate: the optical fiber of kind is put into growth solution, is closed to be placed on thermostatic drying chamber
Lower 95 degrees Centigrades, by the length of heating time control ZnO nanorod；
Step e, the optical fiber of growing ZnO nanorod is taken out from growth solution, is cleaned by ultrasonic 2min with deionized water, places into
80 degrees Celsius of dry 2h in drying box.
2. a kind of method of taper micro-nano fiber surface according to claim 1 growing ZnO nanorod structure, feature exist
In for making the fiber mix waveguide in oil well Extraction rate detection device.
3. a kind of method of taper micro-nano fiber surface according to claim 2 growing ZnO nanorod structure, feature exist
In the oil well Extraction rate detection device includes detection pipeline road (1) and ultraviolet detector (2).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7473906B2 (en) * | 2005-04-28 | 2009-01-06 | Claudio Oliveira Egalon | Reversible, low cost, distributed optical fiber sensor with high spatial resolution |
| CN109668628A (en) * | 2019-01-21 | 2019-04-23 | 哈尔滨理工大学 | It is a kind of based on ZnO nanorod/micro-nano fiber hybrid waveguide ultraviolet detector |
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2019
- 2019-02-21 CN CN201910128407.5A patent/CN109781254A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7473906B2 (en) * | 2005-04-28 | 2009-01-06 | Claudio Oliveira Egalon | Reversible, low cost, distributed optical fiber sensor with high spatial resolution |
| CN109668628A (en) * | 2019-01-21 | 2019-04-23 | 哈尔滨理工大学 | It is a kind of based on ZnO nanorod/micro-nano fiber hybrid waveguide ultraviolet detector |
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| S AZAD 等: "Side-detecting optical fiber coated with Zn(OH)2 nanorods for ultraviolet sensing applications", 《LASER PHYSICS》 * |
| 徐耀辉等: "紫外光谱技术在油藏注水开发动态监测中的应用—以南堡凹陷柳北地区沙三3油藏为例", 《石油天然气学报》 * |
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