CN103743710A - Portable laser probe component analyzer based on optical fiber laser - Google Patents

Portable laser probe component analyzer based on optical fiber laser Download PDF

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Publication number
CN103743710A
CN103743710A CN201310740318.9A CN201310740318A CN103743710A CN 103743710 A CN103743710 A CN 103743710A CN 201310740318 A CN201310740318 A CN 201310740318A CN 103743710 A CN103743710 A CN 103743710A
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laser
miniature
portable
displacement platform
spectrometer
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CN201310740318.9A
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CN103743710B (en
Inventor
曾晓雁
曾庆栋
李祥友
郭连波
段军
贺超
沈萌
李阔湖
郝中骐
陆永枫
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Abstract

The invention discloses a portable LIBS (Laser Induced Breakdown Spectroscopy) analyzer based on an optical fiber laser. The analyzer comprises a laser detection head and a main machine system, wherein the detection head comprises a laser output end, a diaphragm, a reflector, a dichroscope, a lens, a first micro displacement table, a second micro displacement table and a light collector; the main machine system comprises a spectrograph, a microcontroller, a portable PC (Personal Computer) and an optical fiber laser main machine. The analyzer disclosed by the invention uses the optical fiber laser as a laser light source and provides a novel spectrum collecting manner, the detection sensitivity is improved and the detection limit is reduced. When the analyzer is additionally provided with a polarizer, the analyzer further can inhibit interference of a continuous background in a plasma spectrum, so that the detection sensitivity is further improved. The analyzer provided by the invention is small in size, light in weight, convenient to carry, simple to operate and fast to analyze, can be used for real-time detection in a field environment or an industrial field, and is free from a vacuum environment and pretreatment on a sample. The size and electrical conductivity of the analyzed sample are not limited, so that the analytical efficiency is high.

Description

Portable laser probe analytical instrument based on fiber laser
Technical field
The invention belongs to laser accurate detection technique field, be specially a kind of portable laser probe analytical instrument (being called for short portable LIBS laser probe instrument) based on fiber laser, be mainly used in the qualitative and quantitative analysis of material element composition.
Background technology
Laser-induced Breakdown Spectroscopy (Laser Induced Breakdown Spectroscopy, be called for short LIBS) be a kind of novel elemental analysis technology, it is pulse laser beam to be focused on to sample surfaces ablation form plasma and launch spectrum, analyzes composition and the content thereof of its element by gathering plasma spectrometry.Compared with traditional analytical instrument, LIBS technology has significant technical advantage, for example, without sample preparation, analyzes rapidly, can detect that multiple element, detection limit are low, low cost and other advantages simultaneously, can be used for detecting solid, liquids and gases material etc.
But, the existing LIBS system part that also comes with some shortcomings:
First, traditional LIBS system adopts Nd:YAG solid state laser on optical table, to build complicated light path system mostly, and equipment volume is huge, and the environmental requirement that equipment is placed is high, optical tables as special in needs etc. (for example, South China Science & Engineering University, Li Runhua etc., photoelectric double-pulse laser induced breakdown spectrograph and spectroscopic analysis methods, [P], China, 200910041442,20100106; Tsing-Hua University, horse Xiao Hong etc., the Laser-induced Breakdown Spectroscopy pick-up unit that detection time and position are controlled, [P], China, 201010569401,20110720).Some laser instrument needs constant temperature, dry environment etc., and therefore huge instrument cannot be moved to field extreme environment or industry spot carries out determination and analysis; Meanwhile, because the fluctuation of Nd:YAG energy of lasers is generally larger, cause measuring result error larger, affected detection accuracy and the stability of LIBS system.
Secondly; some current LIBS system is in order to strengthen plasma light spectral intensity; often adopt some ancillary methods; for example fill protection gas, be evacuated, electric spark or microwave heating etc., the adding of these servicing units; often need to do a special sample chamber; the size of sample chamber is very limited the size of target sample, particularly cannot complete the constituent analysis of large dimension specimen, also cannot carry out Real-Time Monitoring in industry spot.
Summary of the invention
For the needs that overcome some defects of existing LIBS technology existence and detect in real time in order to adapt to field work and industry spot, the invention provides a kind of portable LIBS analyser based on fiber laser, this portable LIBS analyser volume is little, lightweight, easy to carry, simple to operate, analyze rapidly, can be used for field environment or industry spot detects in real time, do not need vacuum environment, without sample is carried out to pre-service; Size and electric conductivity to institute's analytic sample are unrestricted, and analysis efficiency is high.
A kind of portable laser probe analytical instrument provided by the invention, it is characterized in that, it comprises laser acquisition head and host computer system two parts, wherein, detecting head comprises Laser output head, diaphragm, catoptron, dichroic mirror, lens, the first miniature displacement platform, the second miniature displacement platform and light collector; Host computer system comprises spectrometer, microcontroller, portable PC and fiber laser main frame;
The first miniature displacement platform, the second miniature displacement platform are installed in the housing of laser acquisition head, and lens are arranged on the first miniature displacement platform, and light collector is arranged on the second miniature displacement platform; Laser output head, diaphragm and catoptron are all positioned in same light path, and the optical axis of catoptron and Laser output head in angle of 45 degrees; Dichroic mirror is arranged on the reflected light path of catoptron, and principal plane is parallel with the principal plane of catoptron; The light-emitting window of light collector, two-phase look mirror, lens and detecting head successively in another light path, and with the light path parallel at Laser output head, diaphragm and catoptron place; Light collector is connected by optical fiber with spectrometer;
Described the first miniature displacement platform is all connected with microcontroller electric signal with the second miniature displacement platform, and microcontroller is connected with portable PC dynamoelectric signal, makes can realize on portable PC the motion of controlling the first miniature displacement platform and the second miniature displacement platform; Portable PC respectively with spectrometer and fiber laser control card electrical signal, for controlling the work of spectrometer and laser instrument, and make the data of spectrometer synchronous acquisition be sent to portable PC.
Another kind of portable laser probe analytical instrument provided by the invention, it is characterized in that, it comprises laser acquisition head and host computer system two parts, wherein, laser acquisition head comprises Laser output head, diaphragm, lens, light collector and the first to the 3rd miniature displacement platform, host computer system comprise spectrometer, microcontroller, portable PC and and fiber laser main frame;
The first miniature displacement platform and the 3rd miniature displacement platform are arranged in the housing of laser acquisition head, and lens are arranged on the first miniature displacement platform; The light-emitting window of Laser output head, diaphragm, lens and detecting head is positioned in same light path, Laser output head is arranged on the 3rd miniature displacement platform, light collector is arranged on the second miniature displacement platform, and is paraxonic collection, and light collector is connected with spectrometer by optical fiber;
The miniature displacement platform of described the first miniature displacement platform to the three is all connected with microcontroller electric signal, and microcontroller is connected with portable PC dynamoelectric signal, makes can realize control the first motion to the 3rd miniature displacement platform on portable PC; Portable PC respectively with spectrometer and fiber laser control card electrical signal, for control spectrometer and work with laser instrument simultaneously, and make the data of spectrometer synchronous acquisition be sent to portable PC.
As the improvement of above-mentioned two technical schemes, this portable laser probe analytical instrument can also arrange polarizer and Miniature turntable.
The present invention adopts fiber laser as LASER Light Source, and a kind of new spectra collection mode is provided, and has improved detection sensitivity and has reduced detection limit.Because novel fiber laser has that cost is low, miniaturization, the advantage such as conversion efficiency is high, power is high, good beam quality, loss are low, rapid heat dissipation, laser threshold are low, high stability, can be competent at severe working environment, dust, concussion, impact, humidity, temperature are had to very high tolerance, do not need thermoelectric cooling and water-cooled, only need be simply air-cooled, be particularly suitable for being portable LIBS.Meanwhile, the present invention passes through structural design cleverly, makes structure of the present invention convenient and practical, small and exquisite convenient, reliable and stable.
When the present invention sets up polarizer, can also suppress the interference of the continuous background in plasma spectrometry, further improve detection sensitivity and reduce detection limit.
In a word, portable laser probe machine provided by the invention analysis is rapid, detection limit is low, highly sensitive, can be in the wild or rugged surroundings and industry spot Real-Time Monitoring, well make up the shortcoming and defect of existing LIBS scheme.
Accompanying drawing explanation
Fig. 1 is the structural representation of the first embodiment of the present invention;
In figure, symbol represents respectively: A is the detecting head part of portable LIBS analyser, B is the host computer system of portable LIBS analyser, 1 is the Laser output head of fiber laser, 2 is diaphragm, 3 is catoptron, 4 is housing, 5 is lens, 6 is detecting head light-emitting window, 7 is plasma plume, 8 is sample, 9, 13 and 26 is miniature displacement platform, 10 is dichroic mirror, 11 and 14 is handle, 12 is light collector, 15 is control signal wire, 16 is optical fiber, 17 is optical fiber, 18 is sleeve pipe, 19 is spectrometer, 20 is fiber laser control card, 21 is microcontroller, 22 is portable PC, 23 is fiber laser main frame, 24 is polarizer, 25 is Miniature turntable.
Fig. 2 is the course of work schematic diagram of Portable laser probe analyzer;
Fig. 3 is the structural representation of the second embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further.At this, it should be noted that, for the explanation of these embodiments, be used for helping to understand the present invention, but do not form limitation of the invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
As shown in Figure 1, the portable LIBS analyser of one that the embodiment of the present invention provides, comprises a laser acquisition A and host computer system B two parts, wherein, detecting head A comprises: Laser output head 1, diaphragm 2, catoptron 3, dichroic mirror 10, lens 5, first, second miniature displacement platform 9,13, polarizer 24, Miniature turntable 25, and light collector 12 etc.Host computer system B comprises spectrometer 19, fiber laser control card 20, and microcontroller 21, and portable PC 22, host computer system B can carry or outer luminous intensity distribution fibre laser main frame 23 etc.
In detecting head A, Laser output head 1, diaphragm 2 and catoptron 3 are arranged on same straight line, and catoptron 3 and laser beam are in angle of 45 degrees; Dichroic mirror 10 be arranged on catoptron 3 under, and principal plane is parallel with the principal plane of catoptron 3; Light collector 12, polarizer 24, two-phase look mirror 10, lens 5 and detecting head light-emitting window 6 successively on another straight line, and with the straight line parallel at Laser output head 1, diaphragm 2 and catoptron 3 places; Light collector 12 is connected by optical fiber 16 with spectrometer 19, and Laser output head 1 is connected with fiber laser main frame 23 by optical fiber.
The first miniature displacement platform 9, the second miniature displacement platform 13 and Miniature turntable 25 are installed in the housing 4 of detecting head A, wherein, lens 5 are arranged on miniature displacement platform 9, and polarizer 24 is arranged on Miniature turntable 25, and light collector 12 is arranged on miniature displacement platform 13.Miniature turntable 25, miniature displacement platform 9 are all connected with microcontroller 21 by control signal wire with 13.
In host computer system B, microcontroller 21 is connected by data line with portable PC 22, for communicating by letter between PC 22 and microcontroller 21, thereby on PC, controls the motion of Miniature turntable 25, miniature displacement platform 9 and 13.Between spectrometer 19 and portable PC 22, by data line, be connected, for communicating by letter between spectrometer 19 and PC 22, the data that spectrometer 19 is gathered are sent on PC 22 and show.
Fiber laser main frame 23 disposes fiber laser control card 20, and portable PC 22 is connected with fiber laser control card 20 electric signal, and portable PC 22 can be controlled fiber laser main frame 23 and spectrometer 19 synchronous workings.
Miniature displacement platform used in the present invention is the micro two-dimensional displacement platform that volume is little, can be to x axle and the motion of y axle both direction, and preferred orientation precision can reach 10 μ m, and straigheness can reach the two-dimension displacement platform of 10 μ m.
Miniature turntable used in the present invention is the electric rotary table that volume is little, and rotation angle range is 0 to 360 degree, and preferably repetitive positioning accuracy can reach the miniature electric universal stage below 0.1 degree.
Can by microcontroller 21, control miniature displacement platform 9 by the software on PC, to regulate the locus of lens 5, realize high-precision focusing, precision can reach 10 μ m, that avoids that manual focusing brings wastes time and energy and the situation such as error is large, generally the 2-4mm place outside probe light-emitting window 6 by focal adjustments, the strongest to guarantee that laser spot and sample surfaces have a defocusing amount, laser is got to the plasma spectrometry producing on sample.When defocusing amount need to convert, can carry out accurate adjustment by miniature displacement platform 9.
Can by microcontroller 21, control Miniature turntable 25 by the software on PC, to regulate the angle of polarizer 24, reach the continuous background suppressing in plasma spectrometry and the object that improves detection limit.Structure shown in Fig. 1 can not arrange polarizer 24 and Miniature turntable 25.
Can by microcontroller 21, control miniature displacement platform 13 by the software on PC, to adjust the locus of light collector 12, make it just in time aim at the plasma plume that wish gathers, control accuracy reaches 10 μ m.
Light collector 12 is used for collecting plasma spectrometry, then by optical fiber 16, is transferred to spectrometer 19.
The adjusting of lens 5, polarizer 24 and light collector 12 can regulate by software control, also can manual adjustments.
Said diaphragm 2 is that internal diameter is adjustable, and its diameter is generally adjusted to 1-10mm.
The plane mirror for specific wavelength that catoptron 3 is surface coating, reflectivity reaches more than 98%.
Dichroic mirror 10 is that surface is coated with the medium total reflection film of one deck corresponding to operation wavelength, and to the only reflection of specific wavelength, and reflectivity reaches more than 98%, be transmission, and percent of pass reaches more than 98% to the light of other wavelength.
Detecting head light-emitting window 6 is detecting head and sample contact portion, adopt resistant to elevated temperatures alloy material to make, the diameter of its top round mouth is 2-5mm, for laser, from this mouth, emits, meanwhile, the plasma spectrometry that laser excitation goes out is also to enter light collector 12 from this round mouth.
Said laser instrument is the fiber laser that the wavelength of small size is 1064nm, preferably power is 20w, and single pulse energy is about 0.5mJ, and pulse repetition rate is that 10-400kHz is adjustable, pulsewidth is the adjustable Miniature optical fiber laser instrument of 10-200ns, can meet different detection demands.
Optical path adjusting method:
Laser instrument red-emitting pilot light, be irradiated to the relevant position on sample, by the motion of the miniature displacement platform 9 and 13 of upper computer software control, by adjusting the position of lens 5, make pilot light focus on the relevant position of sample surfaces, by the position of automatic adjustment light collector 12, make spectrometer collect this pilot light, illustrate that light path system adjusts.
Spectra collection method:
Differently with traditional LIBS system be, not to remove the continuous background in plasma spectrometry by the method for time delays, but suppress the continuous background in plasma spectrometry by polarizer, also reduced detection limit simultaneously and strengthened detection sensitivity.So the spectra collection method of this portable LIBS analyser is, integral time and average time that times of collection and spectrometer once gather are set on software, laser instrument is set software and spectrometer is worked simultaneously, between each collection of spectrometer 19 and each laser pulse, delay time is not set, for example, in an integral time of spectrometer (20ms), what collect is the result of multiple pulse accumulation effects.
As shown in Figure 2, specific works process of the present invention is as follows:
1. initialization
During initialization, complete the connection of miniature displacement platform, fiber laser, spectrometer and the setting of correlation parameter default value, then the laser instrument pilot light that glows, be irradiated to the relevant position on sample, utilize the miniature displacement platform of PC control, adjust the position of lens and light collector, make pilot light focus on sample surfaces, make spectrometer collect this pilot light simultaneously, illustrate that light path system adjusts.
2. spectra collection
The laser beam that Laser output head 1 is launched, after diaphragm 2 shapings, incides catoptron 3, and with catoptron 3 in angle of 45 degrees; After catoptron 3 reflections, again after 10 reflections of two-phase look mirror, incide on lens 5, through lens 5, focus on, then the surface that is irradiated to sample 8 produces plasma plume, the light that plasma resonance goes out enters detecting head A from light-emitting window 6, after lens 5, become directional light, again transmitted through after dichroic mirror 10, by light collector 12, gathered, then by optical fiber 16, be transferred to 19 li of spectrometers, spectrometer 19 is converted to electric signal by the light signal collecting, and then by USB interface, is transferred to portable PC 22.
3. data analysis
PC receiving spectrum signal, it is carried out to pre-service (comprise denoising, go background, overlap peak separate and self-absorption compensation etc.), spectral information in the spectroscopic data obtaining and database is analyzed, determines the contained element kind of sample and content thereof and be shown to user.
The present invention also can adopt the second embodiment as shown in Figure 3, different from the first embodiment: the second embodiment adopts paraxonic to gather the mode of plasma spectrometry.Laser output head 1 is arranged on the 3rd miniature displacement platform 26, lens 5 are arranged on the first miniature displacement platform 9, Laser output head 1, diaphragm 2, lens 5 and light-emitting window 6 are point-blank, light collector 12 is arranged on miniature displacement platform 13,, polarizer 24 is arranged on Miniature turntable 25, and is just in time positioned at the dead ahead of light collector 12, for paraxonic acquisition mode, from the side of plasma plume, gather spectrum of laser plasma.Adopt paraxonic acquisition mode, miniature displacement platform 13 and Miniature turntable 25 can be arranged on outside housing 4, if space allows, also can be arranged in housing 4.
For easy to operate, two handles 11,14 can be installed on housing 4.Can also adopt sleeve pipe 18 by optical fiber 16,17, and the various circuits such as control signal wire 15 overlap inside.
Equally, structure shown in Fig. 3 also can not arrange polarizer 24 and Miniature turntable 25.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.So, every not departing from the equivalence completing under spirit disclosed in this invention or revising, all fall into the scope of protection of the invention.

Claims (5)

1. a portable laser probe analytical instrument, it is characterized in that, it comprises laser acquisition head and host computer system two parts, and wherein, detecting head comprises Laser output head, diaphragm, catoptron, dichroic mirror, lens, the first miniature displacement platform, the second miniature displacement platform and light collector; Host computer system comprises spectrometer, microcontroller, portable PC and fiber laser main frame;
The first miniature displacement platform, the second miniature displacement platform are installed in the housing of laser acquisition head, and lens are arranged on the first miniature displacement platform, and light collector is arranged on the second miniature displacement platform; Laser output head, diaphragm and catoptron are all positioned in same light path, and the optical axis of catoptron and Laser output head in angle of 45 degrees; Dichroic mirror is arranged on the reflected light path of catoptron, and principal plane is parallel with the principal plane of catoptron; The light-emitting window of light collector, two-phase look mirror, lens and detecting head successively in another light path, and with the light path parallel at Laser output head, diaphragm and catoptron place; Light collector is connected by optical fiber with spectrometer;
Described the first miniature displacement platform is all connected with microcontroller electric signal with the second miniature displacement platform, and microcontroller is connected with portable PC dynamoelectric signal, makes can realize on portable PC the motion of controlling the first miniature displacement platform and the second miniature displacement platform; Portable PC respectively with spectrometer and fiber laser control card electrical signal, for controlling the work of spectrometer and laser instrument, and make the data of spectrometer synchronous acquisition be sent to portable PC.
2. portable laser probe analytical instrument according to claim 1, it is characterized in that, it also comprises polarizer and Miniature turntable, Miniature turntable is also arranged in the housing of laser acquisition head, polarizer is arranged on Miniature turntable, and is just in time positioned at the dead ahead of light collector, and polarizer is between light collector and two-phase look mirror, Miniature turntable is connected with microcontroller electric signal, makes can realize on portable PC the motion of controlling Miniature turntable.
3. another kind of portable laser probe analytical instrument, it is characterized in that, it comprises laser acquisition head and host computer system two parts, wherein, laser acquisition head comprises Laser output head, diaphragm, lens, light collector and the first to the 3rd miniature displacement platform, host computer system comprise spectrometer, microcontroller, portable PC and and fiber laser main frame;
The first miniature displacement platform and the 3rd miniature displacement platform are arranged in the housing of laser acquisition head, and lens are arranged on the first miniature displacement platform; The light-emitting window of Laser output head, diaphragm, lens and detecting head is positioned in same light path, Laser output head is arranged on the 3rd miniature displacement platform, light collector is arranged on the second miniature displacement platform, and is paraxonic collection, and light collector is connected with spectrometer by optical fiber;
The miniature displacement platform of described the first miniature displacement platform to the three is all connected with microcontroller electric signal, and microcontroller is connected with portable PC dynamoelectric signal, makes can realize control the first motion to the 3rd miniature displacement platform on portable PC; Portable PC respectively with spectrometer and fiber laser control card electrical signal, for control spectrometer and work with laser instrument simultaneously, and make the data of spectrometer synchronous acquisition be sent to portable PC.
4. portable laser probe analytical instrument according to claim 3, it is characterized in that, it also comprises polarizer and Miniature turntable, polarizer is arranged on Miniature turntable, and be just in time positioned at the dead ahead of light collector, Miniature turntable is connected with microcontroller electric signal, makes can realize on portable PC the motion of controlling Miniature turntable.
5. according to arbitrary described portable laser probe analytical instrument in claim 1 to 4, it is characterized in that, two handles are installed on described housing.
CN201310740318.9A 2013-12-28 2013-12-28 Based on the portable laser probe analytical instrument of fiber laser Active CN103743710B (en)

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CN105527274A (en) * 2016-01-29 2016-04-27 华中科技大学 Efficient multipath laser probe analysis system and method
CN106896099A (en) * 2017-03-27 2017-06-27 河钢股份有限公司 A kind of device and method of laser detection solid material composition
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CN109444111A (en) * 2018-12-10 2019-03-08 西安交通大学 A kind of optical fiber LIBS detection system and method for optional double pulse modes
CN109557057A (en) * 2018-11-19 2019-04-02 西安交通大学 A kind of optical fiber LIBS detection device and method in Nuclear power plant main pipeline
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CN104007090A (en) * 2014-05-27 2014-08-27 四川大学 Portable elementary composition analysis device based on laser-induced breakdown spectroscopy technology
CN104007090B (en) * 2014-05-27 2016-06-08 四川大学 Portable element composition analysis device based on LIBS
CN105527274A (en) * 2016-01-29 2016-04-27 华中科技大学 Efficient multipath laser probe analysis system and method
CN105527274B (en) * 2016-01-29 2018-01-02 华中科技大学 A kind of efficient multi-path laser probe analysis System and method for
CN106896099A (en) * 2017-03-27 2017-06-27 河钢股份有限公司 A kind of device and method of laser detection solid material composition
CN106896099B (en) * 2017-03-27 2023-08-22 河钢股份有限公司 Device and method for detecting solid material components by laser
CN108362682A (en) * 2018-01-24 2018-08-03 西安交通大学 A kind of multimode fibre LIBS detection device based on compound constant enhanced spectrum
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CN109557057A (en) * 2018-11-19 2019-04-02 西安交通大学 A kind of optical fiber LIBS detection device and method in Nuclear power plant main pipeline
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CN109444111A (en) * 2018-12-10 2019-03-08 西安交通大学 A kind of optical fiber LIBS detection system and method for optional double pulse modes
CN109872442A (en) * 2019-02-15 2019-06-11 常州万泰天平仪器有限公司 A kind of Detecting of coin method, system and its coin weight detector
CN109872442B (en) * 2019-02-15 2021-02-02 常州万泰天平仪器有限公司 Coin detection method and system and coin weight detector

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Inventor after: Zeng Xiaoyan

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