CN105928953A - Microwave absorption spectrum measurement device and microwave absorption spectrum measurement method based on thermo-acoustic effect and application thereof - Google Patents

Microwave absorption spectrum measurement device and microwave absorption spectrum measurement method based on thermo-acoustic effect and application thereof Download PDF

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Publication number
CN105928953A
CN105928953A CN201610543196.8A CN201610543196A CN105928953A CN 105928953 A CN105928953 A CN 105928953A CN 201610543196 A CN201610543196 A CN 201610543196A CN 105928953 A CN105928953 A CN 105928953A
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sample
microwave
sample cell
absorption spectrum
microwave absorption
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计钟
邢达
杨思华
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South China Normal University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N22/00Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more

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  • Electromagnetism (AREA)
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  • Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)

Abstract

The invention relates to a microwave absorption spectrum measurement device based on thermo-acoustic effect. The microwave absorption spectrum measurement device comprises a microwave generator, a transmitting antenna, a sample tank, an ultrasonic detector, an amplifier, a data acquisition card and a computer, wherein the microwave generator, the transmitting antenna and the sample tank are arranged in sequence along a microwave input direction of the sample tank; and the sample tank, the ultrasonic detector, the amplifier, an oscilloscope and the computer are further arranged in sequence along an ultrasonic output direction of the sample tank. The invention further relates to a microwave absorption spectrum measurement method based on the thermo-acoustic effect and application of the microwave absorption spectrum measurement device based on the thermo-acoustic effect. The invention provides a method for directly measuring a microwave absorption coefficient and a microwave absorption spectrum, and the influences of microwave scattering and reflection are alleviated; and the thermo-acoustic effect is introduced into the measurement of the microwave absorption spectrum for the first time and substance concentration analysis can also be provided; and the method belongs to the technical field of the measurement of the microwave absorption spectrum.

Description

A kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect and method and application thereof
Technical field
The present invention relates to microwave absorption spectrometry technology, specifically, relate to a kind of based on thermoacoustic effect micro- Ripple absorption spectra measurement apparatus, and use the microwave absorption spectrum measuring method based on thermoacoustic effect of this measurement apparatus, And the application of microwave absorption spectrum measurement apparatus of based on thermoacoustic effect.
Background technology
In fields such as food inspection, biological medicine, mineral geology, chemical composition analysis be one essential Operating procedure, particular, it is important that need a set of can monitor in real time and recorded matter in operation by The device of the change of the maroscopic quantity that the factor such as concentration, temperature causes, to be used for studying these factors shadow to it Ring.Microwave spectroscopy, is called for short Wave Spectrum, by radio frequency or microwave electromagnetic field and the Resonant Interaction of material, The research condition of material, structure and physics's subdiscipline of motion.It research object can be atom, Molecule and condensed state thereof, it is also possible to be neutron, proton, electronics, atomic nucleus and plasma etc..Because it is micro- Wave spectrum has high sensitivity and uniqueness, so microwave can be used for Analysis and Identification, plays very in above-mentioned field Big effect.But, owing to present microwave spectrum (such as dielectric spectrometry) uses the microwave of reception object more Scattering or reflected signal, relatively big by external action, source of error is many, and accuracy is the highest, it is therefore desirable to a kind of The microwave spectrum measurement method of new principle.
Microwave thermal acoustic effect, is called for short thermoacoustic effect, is a kind of method of Measuring Object microwave absorption.Work as microwave When being heat by object sorption enhanced, object temperature fast lifting and cause thermal expansion, thus produce wide band Ultrasound wave (i.e. thermoacoustic signal), ultrasonic wave direction organizational boundary propagates and can be received by the ultrasonic transducer of wideband, The ultrasonic signal received just can be used to the microwave absorption intensity of quantitative reflection object.But, because thermoacoustic Signal intensity by many impacts such as sample shape, ambient temperature, humidity, microwave source shakes, Thermoacoustic effect can not the microwave absorption spectrum of direct Measuring Object, it is therefore desirable to a kind of stable, reliable microwave Thermoacoustic devices, realizes microwave absorption spectrometry based on thermoacoustic effect.
Summary of the invention
For technical problem present in prior art, it is an object of the invention to: provide a kind of by thermoacoustic effect High sensitivity, the microwave absorption spectrometry based on thermoacoustic effect of high accuracy for microwave absorption spectrometry Apparatus and method.
Another object of the present invention is: provide a kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect Application, for the parsing of material concentration.
In order to achieve the above object, the present invention adopts the following technical scheme that
A kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect, including microwave generator, launch antenna, Sample cell, ultrasonic detector, amplifier, data collecting card, computer;Microwave along sample cell inputs Direction, microwave generator, transmitting antenna, sample cell set gradually;Along the ultrasonic outbound course of sample cell, Sample cell, ultrasonic detector, amplifier, oscillograph, computer set gradually.Wherein, launch antenna (or Waveguide) effect be radiation microwave;Microwave radiation at microwave generator dominant frequency to be suitable to, if aerial radiation Efficiency is different at different dominant frequency, also needs to measure its frequency response characteristic for correction.Amplifier effect be by The thermoacoustic signal (signal of telecommunication) that ultrasonic detector receives amplifies, and suppresses noise;Operating frequency to be mated super Detector of sound frequency.Data collecting card effect be by amplifier amplify electrical signal collection, frequency-selecting, filtering, Analog digital conversion, is finally transferred to computer;According to that Qwest's law, it is desirable to frequency is maximum more than detector The twice of frequency, preferably more than 10 times.Computer's role is the signal of telecommunication that process amplifier amplifies, and calculates Its peak-to-peak value, draws curve, and image show, and data preserve, and gives signal just control to other devices; Require to calculate speed sufficiently fast.
Preferred as one, a kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect, also include respectively with Waste sample processing means, sample cell that sample cell connects clean device and Sample introduction device.
Preferred as one, sample cell cleans device and Sample introduction device, sample cell, waste sample processing means Being arranged in a straight line, sample flow direction in sample cell is to clean device and Sample introduction device from sample cell Point to waste sample processing means;The microwave propagation direction of input sample cell and the ultrasonic signal exporting sample cell are propagated Direction is consistent, is each perpendicular to sample flow direction in sample cell.Wherein, sample cell cleans device effect It is to clean sample cell;Needs have bath (preferably distilled water), qi of chong channel ascending adversely (preferably pure nitrogen gas), dry, Vacuum extractor.Waste sample processing means effect is to place the sample measured;Owing to some sample is more precious Expensive, it is necessary to there is retracting device.
Preferred as one, sample cell is tubulose, sample in sample cell along the length direction stream of sample cell Dynamic.Wherein, sample cell act as holding sample;Require to keep constant temperature, constant voltage, there is temperature and pressure and survey Amount and adjusting apparatus;Require that microwave and ultrasonic transmitance are big;It is unlikely to deform, is preferably shaped to tubulose;Resistance to Corrosion;High temperature resistant;Easy cleaning, replaceable;Preferably employ vinyon material.Fixed by sample cell Sample shape, size, the constant environmental condition such as temperature, pressure, it would be possible to affect final result because of Element all standardization, have accuracy.
Preferred as one, microwave generator, transmitting antenna, sample cell are respectively positioned on micro-wave screening indoor.Its In, the effect of micro-wave screening room is shield microwaves, prevents it from disturbing external instrument and operator.
Preferred as one, microwave generator single pulse energy metric density in irradiation range is at 0.1-10 J/cm2, repetition rate is 10Hz-1000Hz scope, and operating frequency is in the range of 100MHz-100GHz Continuously adjustabe, operational frequency bandwidth is at below 10MHz.Wherein, microwave generator effect is to provide high power Microwave;For the continuous high power microwave generator of high power pulse microwave generator or modulation, it is preferably High power pulse microwave generator;Irradiation range is more than sample cell size;Single pulse energy in irradiation range Metric density is at 0.01-100J/cm2In the range of, preferably 0.1-10J/cm2;Repetition rate is the biggest, preferably For 10Hz-1000Hz in the range of;Operating frequency is continuously adjustabe, operational frequency bandwidth in the most on a large scale The least, preferably continuously adjustabe in the range of 100MHz-100GHz, operational frequency bandwidth is at 10MHz Below;The power stability of microwave generator requires higher, and preferred microwave amplitude dither is within 1%.
Preferred as one, ultrasonic detector is flat field type or focus type, and ultrasonic dominant frequency scope is at 1MHz-10 MHz, uses single array element or multiple array element.Wherein, ultrasonic detector effect is to receive thermoacoustic signal, will It is converted to the signal of telecommunication;Require the highest sensitivity;Can be flat field type can also be focus type, preferably For point focused-type;Ultrasonic dominant frequency scope is at 100KHz-100MHz, preferably in 1MHz-10MHz; Can be that single array element can also have multiple array element, the most multiple array elements be to improve sensitivity and accuracy.
Preferred as one, it is provided with ultrasonic coupling module between sample cell and ultrasonic detector, this ultrasonic coupling Module front end is little, and rear end is big;The front end of ultrasonic coupling module is close to sample cell, in size and sample cell The size of ultrasonic signal collecting zone is corresponding;The rear end of ultrasonic coupling module is close to ultrasonic detector, size Corresponding to the size of the ultrasonic signal receiving area of ultrasonic detector.
A kind of microwave absorption spectrum measuring method based on thermoacoustic effect, uses a kind of microwave based on thermoacoustic effect Absorption spectra measurement apparatus, by the sample in microwave exposure sample cell, sample absorbs microwave energy and causes moment Temperature rise, produces thermoacoustic effect, and the thermoacoustic signal sent reflects the information of sample microwave absorption difference, changes Microwave frequency is repeatedly measured, and obtains the thermoacoustic signal amplitude under multiple frequency, will in computer software These amplitudes are linked to be curve, obtain the relative microwave absorption line of sample, through standard sample correction, obtain Definitely microwave absorption spectral line.
A kind of application of microwave absorption spectrum measurement apparatus based on thermoacoustic effect, dense for the material providing sample Degree resolves.
The operation principle of the present invention is: microwave generator sends microwave, in emitted antenna irradiation to sample cell Testing sample on, testing sample absorb microwave energy cause transient temperature rise, now the pulsewidth of microwave is narrow, The energy absorbed can not occur thermal diffusion in microwave pulse duration, now can regard adiabatic expansion as, produces Heat acoustic effect, i.e. heat energy are converted into mechanical energy and radiate with ultrasound modalities.This thermoacoustic signal reflects The information of sample microwave absorption difference, ultrasonic detector receives the thermoacoustic signal of fixed position, thermoacoustic is believed Number being converted into the signal of telecommunication is transmitted in computer, changes microwave frequency, and repeat the above steps is i.e. available many These amplitudes are linked to be curve in computer software by the thermoacoustic signal amplitude under individual frequency, through normalization, Curve maximum is set to nondimensional 1, and other numerical value is divided by this maximum, and all of value of such curve is all Become the decimal between (0,1), be the relative microwave absorption line of this sample.Through standard sample correction, Absolute microwave absorption spectral line can be obtained.Standard sample described herein, for the sample of known absorbing coefficient, Such as: the absolute absorption coefficient assuming pure water (standard sample) is 150cm-1, relative value is 0.5, then phase It is 75cm to the sample absorptance that value is 0.25-1
This device may be provided for material concentration and resolves, and generally refers to mass fraction here, passes through molecular weight Can be scaled is substance withdrawl syndrome (molar concentration).According to above-mentioned principle, different samples have different absorption Coefficient, when substance classes determines in a kind of mixture, by encoding above-mentioned microwave spectrum, utilizes equation Group carries out material and solves, such as: the absorptance setting A material is c as a, content, the absorption system of B substance Number is b, and content is d, and compounding substances absorptance is e, then by Simultaneous Equations a × c+b × d=e and c+d=1, The occurrence of c and d can be solved, measure the microwave absorption coefficient of mixture under different frequency, can resolve Go out the ratio (concentration) of above-mentioned different material.
Generally speaking, present invention have the advantage that
1. the present invention is a kind of direct measurement microwave absorption coefficient and the method for microwave absorption spectrum, reduces microwave and dissipates The impact penetrated and reflect, introduces microwave absorption spectrometry first by thermoacoustic effect.
2. this device may be provided for material concentration parsing.
3. this device secures sample shape, size by sample cell, the constant environmental condition such as temperature, pressure, Factor all standardization of final result will be affected, there is accuracy.
4. this device can detect solid, liquid, gaseous sample, has wide applicability;Because liquid and Gas fluidity is preferable, is especially suitable for detection.
5. microwave exposure is being limited in micro-wave screening indoor;During detection, an irradiation is to around testing sample, will not let out External environment condition or external instrument, to space outerpace, will not be interfered by dew.
6. this apparatus system is easy and simple to handle, and result shows soon, and integrated degree is high, and working stability runs continuously Time is long, cheap.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect.
Fig. 2 is the detailed maps of sample cell adjacent part in Fig. 1.
Fig. 3 is that the relative microwave of the lower four kinds of saline solution of the variable concentrations utilizing the device in embodiment to draw absorbs Coefficient.
Fig. 4 is the relative microwave absorption spectra of the pure water utilizing the device in embodiment to draw.
Wherein, 1-1 is microwave generator;1-2 is for launching antenna;1-3 is sample cell;1-4 is supersonic sounding Device;1-5 is amplifier;1-6 is oscillograph;1-7 is computer;1-8 is that sample cell cleans device and sample Gatherer;1-9 is waste sample processing means.
2-1 is sample flow channel;2-2 is sample flow direction;2-3 is ultrasonic signal collecting zone;2-4 For ultrasonic coupling module;2-5 is the ultrasonic signal direction of propagation;2-6 is microwave propagation direction.
Detailed description of the invention
Come that the present invention will be further described in detail below.
A kind of microwave absorption spectrum measurement apparatus based on thermoacoustic effect, is shown in Fig. 1, including microwave generator, transmitting Antenna, sample cell, ultrasonic detector, amplifier, data collecting card, computer;Micro-along sample cell Ripple input direction, microwave generator, transmitting antenna, sample cell set gradually;Ultrasonic defeated along sample cell Outgoing direction, sample cell, ultrasonic detector, amplifier, oscillograph, computer set gradually.
In Fig. 1, microwave generator, for modulation continuous high power microwave generator, irradiation range be about with 3.2cm is the border circular areas of diameter;Single pulse energy is that 17.5-175J is adjustable, and operating frequency is 100MHz-2 Continuously adjustabe in GHz range, repetition rate is that 1-500Hz is adjustable, and microwave amplitude dither is within 0.5%. Launch antenna, be suitable to the microwave radiation at microwave generator dominant frequency.Sample cell is tubulose, and sample is at sample cell The interior length direction along sample cell flows.Ultrasonic detector, type is the point focused-type of single array element, dominant frequency Being 10MHz, relative bandwidth is about 60%.Amplifier, type is differential amplification type, and amplification is about 30dB, carries a width of 100KHz-80MHz, amplification and frequency to meet requirement.Data collecting card, also Can use oscillograph or analog-digital converter that function is identical, the present embodiment uses oscillograph, and bandwidth of operation is 300 Below MHz, sample rate is 3GHz to the maximum, and sample rate meets collection requirement.Computer, its central authorities process Device cpu model is 2.53GHz Intel Core 2 Duo T9400 dual core processor, meets and calculates rate request. Sample cell cleans device and Sample introduction device, and sample cell cleans device and can wash by water and inflate with compression pump, Sample introduction device also has compression pump can to wash by water and inflate, work time different from sample cell cleaning device, sample The devices such as product gatherer, also with constant temperature, is dried, vacuum extractor.Waste sample processing means, with waste sample Hold the extraction waste sample device of pond and negative-pressure type.Wherein microwave generator, transmitting antenna, sample cell are respectively positioned on Micro-wave screening is indoor.
Shown in Fig. 2, sample flow channel is positioned at sample cell, for sample flow, can change time contaminated, Material is polyethylene.Sample flow direction is the length direction along sample cell, from sample cell clean device with Sample introduction device points to waste sample processing means, and sample does not flows during detection.Ultrasonic signal is received Collection region, this region is the focal zone of ultrasonic detector, and during test, this region is fixed every time, and that chooses is former It it is then the focal zone of ultrasonic detector.Ultrasonic coupling module, make front end little (approximate ultrasonic signal receive Collection area size) shape of rear end big (approximating ultrasonic detector size), front end is pasted with sample cell Closing, fitting with ultrasonic detector in rear end, effect is coupling ultrasonic signal.The ultrasonic signal direction of propagation, with sample Product flow direction is vertical.Microwave propagation direction, vertical with sample flow direction.
A kind of microwave absorption spectrum measuring method based on thermoacoustic effect, uses a kind of microwave based on thermoacoustic effect Absorption spectra measurement apparatus, comprises the following steps:
1. open sample cell and clean device and the sample cell cleaning device cleaning sample cell in Sample introduction device, After repeatedly washing by water, inflate, drying (or directly changing sample cell sample flow channel), inject and treat test sample Product.
2. opening microwave generator, microwave launched by emitted antenna, produces thermoacoustic signal through sample, ultrasonic Detector, amplifier, data collecting card, computer receive successively.Depend on the circumstances and can repeatedly put down All;Change microwave frequency, repeat the above steps.
3. utilize computer software that above-mentioned thermoacoustic signal amplitude is linked to be curve, through normalization, be this sample The microwave absorption spectral line of product, stores data stand-by (depending on the circumstances).
4. after being measured, opening waste sample processing means, depend on the circumstances whether recovery sample;Open sample Pond is cleaned device and is cleaned sample cell, replaceable sample cell when cleaning unsuccessful.
5. close each device.
Fig. 3 is to utilize device in embodiment, and the relative microwave of the lower four kinds of saline solution of variable concentrations of drafting absorbs Coefficient (measured drawing under 1.2GHz operating frequency).It can be seen that along with the growth of concentration of salt solution, its phase Microwave absorption coefficient is linearly increased substantially, coincidence theory, make such a empirical value form, can To measure the relative microwave absorptance of the saline solution of a unknown concentration, thus obtain its concentration.
Fig. 4 is to utilize device in embodiment, the relative microwave absorption spectra (prognostic chart) of the pure water of drafting.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned reality Execute the restriction of example, the change made under other any spirit without departing from the present invention and principle, modification, Substitute, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.

Claims (10)

1. a microwave absorption spectrum measurement apparatus based on thermoacoustic effect, it is characterised in that: include microwave generator, Launch antenna, sample cell, ultrasonic detector, amplifier, data collecting card, computer;Along sample cell Microwave input direction, microwave generator, launch antenna, sample cell and set gradually;Surpassing along sample cell Sound outbound course, sample cell, ultrasonic detector, amplifier, oscillograph, computer set gradually.
2., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 1, its feature exists In: also include that the waste sample processing means connected with sample cell respectively, sample cell clean device and fill with Sample introduction Put.
3., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 2, its feature exists In: described sample cell cleans device and is arranged in a straight line with Sample introduction device, sample cell, waste sample processing means, Sample flow direction in sample cell is to clean device from sample cell to point to waste sample process with Sample introduction device Device;The microwave propagation direction of input sample cell is consistent, all with the ultrasonic signal direction of propagation of output sample cell It is perpendicular to sample flow direction in sample cell.
4., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 3, its feature exists In: described sample cell is tubulose, sample in sample cell along sample cell length direction flow.
5., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 1, its feature exists In: described microwave generator, transmitting antenna, sample cell are respectively positioned on micro-wave screening indoor.
6., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 1, its feature exists In: described microwave generator single pulse energy metric density in irradiation range is at 0.1-10J/cm2, repetition rate For 10Hz-1000Hz scope, operating frequency is continuously adjustabe in the range of 100MHz-100GHz, work Frequency bandwidth is at below 10MHz.
7., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 1, its feature exists In: described ultrasonic detector is flat field type or focus type, and ultrasonic dominant frequency scope, at 1MHz-10MHz, uses Single array element or multiple array element.
8., according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus described in claim 4, its feature exists In: being provided with ultrasonic coupling module between described sample cell and ultrasonic detector, this ultrasonic coupling module front end is little, Rear end is big;The front end of ultrasonic coupling module is close to sample cell, and size is collected with the ultrasonic signal in sample cell The size in region is corresponding;The rear end of ultrasonic coupling module is close to ultrasonic detector, size and ultrasonic detector The size of ultrasonic signal receiving area corresponding.
9. a microwave absorption spectrum measuring method based on thermoacoustic effect, uses according to any one of claim 1-8 A kind of based on thermoacoustic effect microwave absorption spectrum measurement apparatus, it is characterised in that: by microwave exposure sample Sample in pond, sample absorbs microwave energy and causes transient temperature rise, produces thermoacoustic effect, and the thermoacoustic sent is believed Number reflect the information of sample microwave absorption difference, change microwave frequency and repeatedly measure, obtain multiple frequency These amplitudes are linked to be curve in computer software by the thermoacoustic signal amplitude under rate, obtain the relative of sample Microwave absorption spectral line, through standard sample correction, obtains absolute microwave absorption spectral line.
10. according to a kind of based on thermoacoustic effect the microwave absorption spectrum measurement apparatus according to any one of claim 1-8 Application, it is characterised in that: for providing the material concentration of sample to resolve.
CN201610543196.8A 2016-07-08 2016-07-08 Microwave absorption spectrum measurement device and microwave absorption spectrum measurement method based on thermo-acoustic effect and application thereof Pending CN105928953A (en)

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