CN107314960A - A kind of hematocrite concentration sensor and preparation method thereof, test device - Google Patents

A kind of hematocrite concentration sensor and preparation method thereof, test device Download PDF

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Publication number
CN107314960A
CN107314960A CN201710695544.8A CN201710695544A CN107314960A CN 107314960 A CN107314960 A CN 107314960A CN 201710695544 A CN201710695544 A CN 201710695544A CN 107314960 A CN107314960 A CN 107314960A
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fiber
femtosecond laser
corrosion
mode fiber
sample
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CN107314960B (en
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廖常锐
王义平
李正勇
王英
何俊
朱峰
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Shenzhen University
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Shenzhen University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06Investigating concentration of particle suspensions
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/01Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials specially adapted for biological cells, e.g. blood cells
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06Investigating concentration of particle suspensions
    • G01N15/075Investigating concentration of particle suspensions by optical means

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention is applied to optical fiber technology there is provided a kind of preparation method of hematocrite concentration sensor, including:The single-mode fiber for peeling coat off is placed on fiber clamp and adjusting is horizontally situated single-mode fiber;Femtosecond laser is focused on into the fibre core plane of single-mode fiber and energy is adjusted, according to default mach zhender chamber model, control femtosecond laser carries out by-line scanning machining to single-mode fiber and obtains sample fiber;Sample fiber is placed in etching solution and is corroded to prepare mach zhender chamber, sample fiber after cleaning corrosion is placed in the quality of micro- Microscopic observation corrosion mach zhender chamber and will test transmission spectrum, judge whether the quality and transmission spectrum of corroding mach zhender chamber reach pre-set criteria value, if not up to, then need Optimal Parameters, if reaching, the sample fiber after corrosion is regard as hematocrite concentration sensor.Sensor construction and manufacture craft that the present invention is provided are simple, reliability is high, sensitivity is high.

Description

A kind of hematocrite concentration sensor and preparation method thereof, test device
Technical field
The invention belongs to technical field of optical fiber, more particularly to a kind of hematocrite concentration sensor and preparation method thereof, test Device.
Background technology
Haemocyte detection is in the phenomenon to a certain degree with the health and disease that human body can be reflected in quantity.Normal adults Haemocyte quantity and concentration be fixed within the specific limits, if more or less than range of normal value, can be corresponding Show certain illness.
The spacecrafts such as Divine Land airship are although bulky, but inner space is limited, as cellanalyzer or fluidic cell This kind of maxicell counting instruments such as instrument, due to it is bulky, professional operation is strong the features such as lead to not bring space into.And it is outer Space environment is severe, strong electromagnetic, intense radiation cause usual device can not normal work, it is but how right in the presence of a harsh environment The haemocyte of astronaut is detected, and then monitors the healthy situation of astronaut, is the weight for concerning astronaut's life security Want problem.
The equipment volume of detection haemocyte is huge at present, and detection process is excessively complicated, and efficiency is low, and with certain pollution Property.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of hematocrite concentration sensor and preparation method thereof, test Device, it is intended to which the equipment volume for solving the detection haemocyte of prior art offer is huge, and detection process is excessively complicated, and efficiency is low Problem.
The present invention is achieved in that a kind of preparation method of hematocrite concentration sensor, including:
The single-mode fiber for peeling coat off, which is placed on fiber clamp, and adjusts the fiber clamp makes the single-mode fiber It is horizontally situated;
Femtosecond laser is focused on to the fibre core plane of the single-mode fiber, the energy of the femtosecond laser is adjusted, according to pre- If Mach-Zehnder chamber model, control energy adjustment after femtosecond laser to the single-mode fiber carry out by-line scanning machining, Obtain sample fiber;
The sample fiber is placed in preset etching solution and corroded, to etch Mach-Zehnder chamber;
Sample fiber after cleaning corrosion, is placed in micro- Microscopic observation by the sample fiber after corrosion and corrodes Mach-Zehnder The quality of your chamber, the sample fiber after corrosion is accessed between light source and spectrometer, the transmission of the sample fiber after test corrosion Spectrum;
Judge corrode Mach-Zehnder chamber quality or the corrosion after sample fiber transmission spectrum whether reach it is pre- Standard value is put, if not up to, adjusting the machined parameters of the femtosecond laser or the parameter of etching, and new single-mode fiber is taken, The step that the single-mode fiber for peeling coat off is placed on fiber clamp is performed, adjusting the machined parameters of the femtosecond laser includes The energy of the femtosecond laser is adjusted, the parameter of adjustment etching includes adjusting concentration, the etching time of the etching solution;
If reaching, the sample fiber after corrosion is regard as hematocrite concentration sensor.
Further, it is described that the single-mode fiber for peeling coat off is placed on fiber clamp, and adjust the fiber clamp Make the single-mode fiber be horizontally situated including:
The single-mode fiber for peeling coat off is fixed on the adjustable flexion-extension platform of two dimension, the flexion-extension platform is located at three-dimensional mobile On platform;
The movement of the three-dimensional mobile platform is controlled, and adjusts the flexion-extension platform, makes the optical fiber axial direction of the single-mode fiber It is parallel with the hot spot moving direction of the femtosecond laser.
Further, the energy of the regulation femtosecond laser includes:
The attenuator being made up of half-wave plate and Glan prism adjusts the energy of the femtosecond laser, by the femtosecond laser Energy hole in 65nJ to 100nJ, modulated with the suitable refractive index intensity for forming local uniform.
Further, after the energy of the regulation femtosecond laser, in addition to:
The femtosecond laser is focused on to the covering and fibre of the fibre core plane of the single-mode fiber by 100 times of immersion oil object lens Core intersection, and enter at about 3 μm to 5 μm of the fibre core.
Further, the step of configuring the etching solution includes:
Deionized water and alcohol is added to dilute for 40% hydrofluoric acid stoste mass fraction, using alcohol as cushioning liquid, Configure the hydrofluoric acid solution that solution concentration is 5%-8%.
Further, the sample fiber is placed in into progress corrosion in preset hydrofluoric acid solution includes:
The sample fiber is placed in the hydrogen-oxygen acid solution, the temperature of corrosion is set as 40 DEG C to 45 DEG C, using water Bathe mode of heating to be corroded, and add magnetic agitation and disturbed.
Further, etching time control was at 10 to 20 minutes.
Present invention also offers a kind of hematocrite concentration sensor, the hematocrite concentration sensor passes through described above Preparation method is prepared.
Present invention also offers a kind of test device of hematocrite concentration, the test device is by dimethyl silicone polymer system It is standby to obtain, including microchannel, the feed pathway that is connected with the microchannel and liquid outlet channel.
Further, a diameter of 300 μm to 359 μm of the microchannel.
Compared with prior art, beneficial effect is the present invention:The preparation method system provided using the embodiment of the present invention Make the obtained hematocrite concentration sensor based on single-mode fiber, using all -fiber formula structure, electromagnetic interference can be avoided to detection As a result influence.Meanwhile, the sensor construction and manufacture craft are simple, and reliability is high, in use, only need to be by the haemocyte solution Using syringe from the feed pathway of test device injects the Mach-Zehnder chamber of single-mode fiber, the connection of single-mode fiber two ends Light source and spectrometer are high with sensitivity detecting that hematocrite concentration changes by way of the drift situation for detecting interference spectrum The characteristics of.
Brief description of the drawings
Fig. 1 is the structural representation of hematocrite concentration sensor provided in an embodiment of the present invention;
Fig. 2 is the flow chart of the preparation method of hematocrite concentration sensor provided in an embodiment of the present invention;
Fig. 3 is the structural representation of the preparation system of hematocrite concentration sensor provided in an embodiment of the present invention;
Fig. 4 is the scanning track schematic diagram of femtosecond laser provided in an embodiment of the present invention;
Fig. 5 is the model pictorial diagram of the Mach-Zehnder chamber of femtosecond laser processing and fabricating provided in an embodiment of the present invention;
Fig. 6 is the pictorial diagram of the Mach-Zehnder chamber provided in an embodiment of the present invention after hydrofluoric acid solution corrodes;
Fig. 7 is the aerial interference spectrogram of the single-mode fiber provided in an embodiment of the present invention for possessing Mach-Zehnder chamber;
Fig. 8 is the structural representation of the test device of hematocrite concentration provided in an embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
The embodiments of the invention provide a kind of femtosecond laser wet etching technique prepare hematocrite concentration sensor and its Preparation method, by single-mode fiber internal production Mach-Zehnder MZ chambers, by detecting that the MZ intracavitary haemocytes solution is reflected The detection to hematocrite concentration is realized in the change of rate.
Fig. 1 shows hematocrite concentration sensor provided in an embodiment of the present invention, to possess the single mode of Mach-Zehnder chamber Optical fiber.Light is transmitted in the fibre core of single-mode fiber 101, is divided into two beams by MZ chambers 102, and light beam is passed still along fibre core Defeated, light beam is transmitted by MZ chambers 102 in addition, and last two-beam is converged in the fibre core of single-mode fiber 101 again.Due to two beams The refractive index for the medium that light passes through is different, produces optical path difference, so as to form MZ interference.Environmental liquids pass through microchannel 103 Change the refractive index of chamber medium into MZ chambers 102, so as to detect this change on transmitted spectrum.
Fig. 2 shows a kind of preparation method of hematocrite concentration sensor provided in an embodiment of the present invention, including:
S201, the single-mode fiber for peeling coat off is placed on fiber clamp, and is adjusted the fiber clamp and made the list Mode fiber is horizontally situated;
S202, femtosecond laser is focused on the fibre core plane of the single-mode fiber, is adjusted the energy of the femtosecond laser, is pressed According to default Mach-Zehnder chamber model, the femtosecond laser after control energy adjustment carries out by-line scanning to the single-mode fiber Processing, obtains sample fiber;
S203, the sample fiber is placed in preset etching solution and corroded, to etch Mach-Zehnder chamber;
S204, the sample fiber after cleaning corrosion, by the sample fiber after corrosion be placed in micro- Microscopic observation corrode Mach- The quality of Zeng Deer chambers, the sample fiber after corrosion is accessed between light source and spectrometer, the sample fiber after test corrosion Transmission spectrum;
S205, judge corrode Mach-Zehnder chamber quality or the corrosion after sample fiber transmission spectrum whether Pre-set criteria value is reached, if not up to, adjusting the machined parameters of the femtosecond laser or the parameter of etching, and take new single mode Optical fiber, performs the step that the single-mode fiber for peeling coat off is placed on fiber clamp, adjusts the processing ginseng of the femtosecond laser Number includes adjusting the energy of the femtosecond laser, and the parameter of adjustment etching includes adjusting concentration, the etching time of the etching solution. In this step, if the quality for the Mach-Zehnder chamber that judgement corrosion is obtained or the transmission spectrum of sample fiber are not up to preset Standard value, then this time the single-mode fiber of processing is undesirable, and the machined parameters of femtosecond laser or the parameter of etching need to be entered Row adjustment, and takes new single-mode fiber, re-starts processing, the single-mode fiber discarding of original processing failure without.
S206, if reaching, regard the sample fiber after corrosion as hematocrite concentration sensor.
Below, specifically illustrated by providing the embodiment of the present invention preparation method of hematocrite concentration sensor:
Step 1, the single-mode fiber for peeling coat off is placed on fiber clamp, and adjusts the fiber clamp makes the list Mode fiber is horizontally situated;
As shown in figure 3, the single-mode fiber for peeling coat off is fixed on the adjustable flexion-extension platform of two dimension, the flexion-extension platform is located at In three-dimensional mobile platform.By adjusting two-dimentional adjustable pitching platform and three-dimensional mobile platform, make the fibre core axial direction of single-mode fiber It is parallel with the hot spot moving direction of femtosecond laser.The attenuator of half-wave plate and Glan prism composition is adjusted, by the energy of femtosecond laser Amount control enables femtosecond laser to form local more uniform suitable refractive index intensity modulation in 65-100nJ.By calculating Machine control three-dimensional mobile platform movement, makes femtosecond laser focus at the fibre core and cladding interface of the fibre core plane of single-mode fiber, Then moving Y-axis makes the focal spot of femtosecond laser enter about 3-5 μm of the fibre core of single-mode fiber.
Step 2, the femtosecond laser after control energy adjustment is scanned processing to the single-mode fiber, obtains optical fiber sample Product.
During femtosecond laser scans track as shown in figure 4, specifically operating, femtosecond laser transfixion, moving three dimension movement Platform, the movement of femtosecond laser is described by static object of reference of three-dimensional mobile platform below.Setting possesses high-precision Three-dimensional mobile platform is 5-10 μm/s in the translational speed of X, Y, Z axis.Shutter is opened, three-dimensional mobile platform is controlled toward X-direction Mobile, now femtosecond laser starts scanning, when femtosecond laser stops along X-axis after positive (or reverse) about 60-100 μm of scanning Only, continue to move 2-3 μm along Z axis negative sense (forward direction), move and stop after 60-100 μm then along X-axis negative sense (forward direction), along Y-axis Mobile 1-1.5 μm to negative direction (direction of vertical fibre core and remote fibre core), then femtosecond laser is positive (or reverse) along X-axis Stop after about 60-100 μm of scanning, it is mobile 2-3 μm along Z axis positive (negative sense), move 60- then along X-axis negative sense (forward direction) Stop after 100 μm, move 1-1.5 μm along Y-axis negative direction, above step is a cycle, so repeat three after multiple cycles Completion of processing of the MZ chambers of dimension by way of by-line is scanned.Multiple microchannel connection MZ chambers and light are processed finally along Y-direction Fine cladding surface, finally obtains the sample fiber with MZ chambers.Fig. 5 represents the MZ chambers after femtosecond laser parallel micromachining.Can be with by Fig. 5 Find out, it is processed after field color it is deeper because processing difference material be refracted rate modification, refractive index is than undressed region Greatly, therefore micro- Microscopic observation color is deeper.
Step 3, it is configured to the hydrofluoric acid solution of corrosion.
Mass fraction is mixed with alcohol and deionized water respectively by volume for 40% hydrofluoric acid solution, volume is configured Fraction is 5%-8% hydrofluoric acid solution.Plus the purpose of alcohol is the effect of buffering.The container material quality of hydrofluoric acid contact is poly- four PVF.Sample fiber is cut off at the 2-3mm apart from MZ cavity configurations, is then inserted perpendicularly into and fills the hydrofluoric acid that configuration is completed In the container of solution.It is 40-45 DEG C that magnetic stirring apparatus, which adds design temperature after water, has hydrofluoric acid solution after will be remained after temperature stabilization Container be put into wherein, set etching time as 10-20 minutes, finally cleaned successively with ethanol and deionized water, be put into baking oven Drying, by the sample fiber corroded and single-mode fiber welding.
Step 4, the MZ chamber quality sample fiber corroded being placed in after micro- Microscopic observation corrosion.
Situation about being likely to occur in practical operation has:Incomplete burn into chamber is in irregular shape, excessive corrosion causes fibre core It is corroded completely.Such as there are the machined parameters that case above needs return to step 2 to change femtosecond laser, machined parameters include swashing Light energy, sweep speed etc., or return to step 3 change the concentration and etching time of hydrofluoric acid solution, until corroding such as Fig. 5 Shown structure.Corrosion area material is completely removed as seen from Figure 6, and MZ chambers pass through microchannel UNICOM, fibre core with the external world Also part retains.Sample fiber two ends after corrosion are connect into light source and spectrometer respectively, the interference spectrogram of MZ chambers is detected.If It can't detect interference spectrum or spectral contrast be less than 5dB, then need return to step 2 or step 3 to change corresponding parameter, weight Multiple experiment.Fig. 7 shows the interference spectrogram of a length of 98 μm of chamber, and interference contrast reaches 17dB.
Step 5, the test device of hematocrite concentration is made.
The solvent of PDMS (dimethyl silicone polymer) glue and curing agent are pressed 10:1 weight ratio is thoroughly mixed, then It is placed in the bubble for vacuumizing and being extracted out in instrument in glue.A diameter of 300-350 μm of iron wire is placed in model, then will be exhausted Glue after vacuum is poured into model, will be integrally positioned in sweat box and is toasted, and temperature setting is 80-90 DEG C, and the time is set as 1-1.5 hour.PDMS glue is fully cured after baking completely, extracts out after iron wire, microchannel is formed.Using card punch in microchannel Two holes are made a call in top, are inserted into metal catheter formation feed pathway and liquid outlet channel.The test device completed such as Fig. 8 institutes Show.
Step 6, the sample fiber etched is placed in the microchannel of test device, tests the concentration of haemocyte.
As shown in figure 8, the sample fiber etched is placed in the microchannel 807 of test device 800, microchannel 807 Two ends sealed with uv-curable glue.One termination Supercontinuum source 802 of sample fiber, another termination spectrometer 806 will be injected Device 801 is connected with the feed pathway 803 of test device by plastic flexible pipe, and liquid outlet channel 804 connects with waste collecting device 805 Connect.Haemocyte solution is extracted with syringe 801, injection rate is set, haemocyte solution passes through feed pathway 803 and microchannel 807 enter in the MZ chambers of sample fiber, after record data after spectrum-stable.Then ethanol injection test device progress structure is changed clear Wash, then change the haemocyte solution injection of another concentration, the spectrogram of the haemocyte of various concentrations is tested successively.Various concentrations Haemocyte density it is different so as to showing otherness in terms of refractive index.When the haemocyte solution of various concentrations injects MZ The refractive index of the medium of MZ chambers is changed after chamber, so as to cause the refringence between two interfere arms to change, is reflected in It is exactly spectrally that wave length shift occurs for interference spectrum.By detecting that this wave length shift indirectly measures the change of hematocrite concentration Change, and the hematocrite concentration sensor provided in an embodiment of the present invention for possessing MZ chambers is with very high refractive index sensitivity and very Low refractive index detection limit, can detect 10-5Variations in refractive index, detect hematocrite concentration in terms of show excellent biography Feel characteristic.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.

Claims (10)

1. a kind of preparation method of hematocrite concentration sensor, it is characterised in that including:
The single-mode fiber for peeling coat off is placed on fiber clamp, and adjusting the fiber clamp is located at the single-mode fiber Horizontal level;
Femtosecond laser is focused on to the fibre core plane of the single-mode fiber, the energy of the femtosecond laser is adjusted, according to default Femtosecond laser after Mach-Zehnder chamber model, control energy adjustment carries out by-line scanning machining to the single-mode fiber, obtains Sample fiber;
The sample fiber is placed in preset etching solution and corroded, to etch Mach-Zehnder chamber;
Sample fiber after cleaning corrosion, is placed in micro- Microscopic observation by the sample fiber after corrosion and corrodes Mach-Zehnder chamber Quality, the sample fiber after corrosion is accessed between light source and spectrometer, the transmission spectrum of the sample fiber after test corrosion;
Judge to corrode Mach-Zehnder chamber quality or the corrosion after the transmission spectrum of sample fiber whether reach preset mark Quasi- value, if not up to, adjusting the machined parameters of the femtosecond laser or the parameter of etching, and takes new single-mode fiber, performs The step that the single-mode fiber for peeling coat off is placed on fiber clamp, adjusting the machined parameters of the femtosecond laser includes adjustment The energy of the femtosecond laser, the parameter of adjustment etching includes adjusting concentration, the etching time of the etching solution;
If reaching, the sample fiber after corrosion is regard as hematocrite concentration sensor.
2. preparation method as claimed in claim 1, it is characterised in that described that the single-mode fiber for peeling coat off is placed in optical fiber On fixture, and adjust the fiber clamp make the single-mode fiber be horizontally situated including:
The single-mode fiber for peeling coat off is fixed on the adjustable flexion-extension platform of two dimension, the flexion-extension platform is located at three-dimensional mobile platform On;
The movement of the three-dimensional mobile platform is controlled, and adjusts the flexion-extension platform, makes optical fiber axial direction and the institute of the single-mode fiber The hot spot moving direction for stating femtosecond laser is parallel.
3. preparation method as claimed in claim 1, it is characterised in that the energy of the regulation femtosecond laser includes:
The attenuator being made up of half-wave plate and Glan prism adjusts the energy of the femtosecond laser, by the energy of the femtosecond laser Amount control is modulated in 65nJ to 100nJ with the suitable refractive index intensity for forming local uniform.
4. preparation method as claimed in claim 1, it is characterised in that after the energy of the regulation femtosecond laser, also Including:
The covering that the femtosecond laser is focused on to the fibre core plane of the single-mode fiber by 100 times of immersion oil object lens is handed over fibre core At boundary, and enter at about 3 μm to 5 μm of the fibre core.
5. preparation method as claimed in claim 1, it is characterised in that the step of configuring the etching solution includes:
Add deionized water and alcohol to dilute for 40% hydrofluoric acid stoste mass fraction, regard alcohol as cushioning liquid, configuration Solution concentration is 5%-8% hydrofluoric acid solution.
6. preparation method as claimed in claim 5, it is characterised in that the sample fiber is placed in preset hydrofluoric acid solution Middle progress corrosion includes:
The sample fiber is placed in the hydrogen-oxygen acid solution, the temperature of corrosion is set as 40 DEG C to 45 DEG C, using water-bath plus Hot mode is corroded, and is added magnetic agitation and disturbed.
7. preparation method as claimed in claim 1, it is characterised in that etching time was controlled at 10 to 20 minutes.
8. a kind of hematocrite concentration sensor, it is characterised in that the hematocrite concentration sensor passes through claim 1 to 7 times Preparation method described in meaning one is prepared.
9. a kind of test device of hematocrite concentration, it is characterised in that the test device is prepared into by dimethyl silicone polymer Arrive, including microchannel, the feed pathway that is connected with the microchannel and liquid outlet channel.
10. test device as claimed in claim 9, it is characterised in that a diameter of 300 μm to 359 μm of the microchannel.
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CN107855644A (en) * 2017-12-07 2018-03-30 广东正业科技股份有限公司 A kind of laser processing device and system
CN108680532A (en) * 2018-07-17 2018-10-19 深圳大学 Biosensor and preparation method thereof based on optical fiber mach-Zeng Deer interferometers
CN108680532B (en) * 2018-07-17 2023-06-09 深圳大学 Biosensor based on optical fiber Mach-Zehnder interferometer and manufacturing method thereof
CN110646377A (en) * 2019-09-27 2020-01-03 京东方科技集团股份有限公司 Blood detection system and detection method thereof
CN110646377B (en) * 2019-09-27 2022-07-05 京东方科技集团股份有限公司 Blood detection system and detection method thereof
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