CN110231298A - A kind of method and apparatus based on infrared emanation spectrum in double modulation measurement material - Google Patents
A kind of method and apparatus based on infrared emanation spectrum in double modulation measurement material Download PDFInfo
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- CN110231298A CN110231298A CN201910376696.0A CN201910376696A CN110231298A CN 110231298 A CN110231298 A CN 110231298A CN 201910376696 A CN201910376696 A CN 201910376696A CN 110231298 A CN110231298 A CN 110231298A
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 50
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- GCNLQHANGFOQKY-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4] GCNLQHANGFOQKY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
The present invention provides a kind of method and apparatus based on infrared emanation spectrum in double modulation measurement material, the device has: Fourier Transform Infrared Spectrometer, including by sample emission signal decomposition at optical path difference reflection signal and transmission signal realize the Michelson's interferometer of interference modulations, the signal for receiving interferometer binary channels MCT detector, be connected to acquire and record the computer of the circuit board of radiation signal information, the program containing inverse Fourier transform being connected with circuit board with detector；Machinery modulation system, including chopper and lock-in amplifier, same frequency reference signal is input to lock-in amplifier reference signal input interface by the control unit of chopper, detector AC signal output interface is connected with lock-in amplifier signal input interface, and lock-in amplifier signal output interface is connected with detector direct current signal input interface；High vacuum sample room, including specimen holder and set on the sample to be tested of specimen holder.The present invention can guarantee to receive sufficiently strong signal strength.
Description
Technical field
The present invention relates to a kind of middle infrared material heat-radiating properties test method and devices, more particularly to one kind based on double
The method and apparatus of infrared emanation spectrum in modulation measurement material.
Background technique
Heat radiation refers to the phenomenon that material thus issues radiation energy because of pyrogen, is interior of articles microcosmic particle warm-up movement state
It is ejected when change.The intensity of heat radiation is mainly determined by the temperature of object and wavelength.Caloradiance is usually with wave
Long increase first increases to be reduced afterwards；Temperature is higher, and caloradiance is higher, and the peak value of caloradiance is mobile to shortwave direction.
Infrared spectroscopy is mainly to study in molecule with the rotation of vibrational spectrum and molecule between the atom of chemical bond connection
Spectrum.It is well known that infrared in have a fingerprint region, different types of compound has different bands of a spectrum in fingerprint region.Steam and
Carbon dioxide is very serious to the selection absorption of spectrum at 2.5~3.0 μm of middle infrared band and 5.0~8.0 μm, so not removing
The influence of atmosphere to the greatest extent, hardly results in the middle infrared emanation spectrum of high quality.Intermediate infrared radiation signal is very faint at relatively low temperatures,
It is easy to be covered by room temperature background radiation signal and difficulty or ease extraction, causes difficulty for the detection of intermediate infrared radiation signal.
Summary of the invention
In view of the above, technical problem to be solved by the present invention lies in providing one kind can guarantee to receive enough
The method and apparatus based on infrared emanation spectrum in double modulation measurement material of strong signal strength.
For this purpose, the present invention adopts the following technical scheme:
On the one hand, the device provided by the invention based on infrared emanation spectrum in double modulation technology measurement material, comprising:
Fourier Transform Infrared Spectrometer, machinery modulation system and high vacuum sample room；
The Fourier Transform Infrared Spectrometer, including by sample emission signal decomposition at the reflection signal with certain optical path difference
The Michelson's interferometer of interference modulations is realized with transmission signal, receives the binary channels of the signal from Michelson's interferometer
MCT detector, the circuit board and circuit board for being used to acquire and record radiation signal information being connected with binary channels MCT detector
The connected computer containing inverse Fourier transform program；
The machinery modulation system, including chopper and lock-in amplifier；The control unit of chopper is by same frequency reference signal
It is input to the reference signal input interface of lock-in amplifier；The AC signal output interface of binary channels MCT detector is put with locking phase
The signal input interface of big device is connected；The signal output interface of lock-in amplifier and the direct current signal of binary channels MCT detector are defeated
Incoming interface is connected；
The high vacuum sample room, including specimen holder and set on the sample to be tested of the specimen holder.
According to the present invention, based on the interference modulations of the machinery modulation of chopper and Fourier Transform Infrared Spectrometer are mutually tied
The double modulation technology of conjunction, the detection of Lai Jinhang intermediate infrared radiation signal, to obtain the middle infrared emanation spectrum of high quality.
It is also possible in the present invention, the Fourier Transform Infrared Spectrometer further includes in mid and far infrared broadband range
The diamond window of high transmittance.The loss of sample in the transmission can be reduced as a result,.
It is also possible in the present invention, the vacuum degree of the high vacuum sample room reaches 1.3~6.0 × 10-3mbar.As a result,
The absorption interference of steam etc. can be effectively eliminated.
It is also possible in the present invention, the Fourier Transform Infrared Spectrometer is vacuum type.
It is also possible in the present invention, the binary channels MCT detector is liquid nitrogen refrigerating type.It makes an uproar thus, it is possible to reduce background
The interference that sound measures radiation signal.
On the other hand, the present invention also provides a kind of sides based on infrared emanation spectrum in above-mentioned apparatus measurement material
Method, comprising the following steps:
S1, the radiation signal that chopper is fixed on to sample to be tested enter in the optical path of Fourier Transform Infrared Spectrometer；
S2, Fourier Transform Infrared Spectrometer and vacuum specimen chamber are vacuumized respectively；
S3, starting chopper carry out machinery modulation to the radiation signal of sample to be tested；Radiation signal after machinery modulation enters
Fourier Transform Infrared Spectrometer carries out interference modulations to radiation signal by Michelson's interferometer, forms double modulated signal；It is double
Modulated signal is received by binary channels MCT detector, and the signal input interface of lock-in amplifier is input in the form of AC signal；
Machinery modulation is demodulated through lock-in amplifier, from the signal that binary channels MCT detector receives extract obtain to
The direct current signal of the heat radiation of sample, and it is input to the direct current signal input interface of binary channels MCT detector；
The direct current signal that S4, circuit board acquisition are input to binary channels MCT detector obtains corresponding interference pattern, and is entered into
In computer, inverse Fourier transform is carried out using program, obtains infrared emanation spectrum in the double modulation of sample to be tested.
It is also possible in the present invention, in step sl, Fourier Transform Infrared Spectrometer is placed in measurement pattern, by
Signal check function in the program of computer, adjustment optical path keep the radiation signal of sample to be tested maximum.
It is also possible in the present invention, in step s 2, Fourier Transform Infrared Spectrometer and vacuum specimen chamber is taken out respectively
Vacuum is to 1mbar or less.
It is also possible in the present invention, in step s3, Fourier Transform Infrared Spectrometer is placed in step-scan test.
It is also possible in the present invention, the sample to be tested is various blocks and thin-film material with different emissivity.
Detailed description of the invention
Fig. 1 show an of the invention implementation form based on the device of infrared emanation spectrum in double modulation measurement material
Structural schematic diagram；
Fig. 2 schematically shows the functional block diagrams of the circuit board in Fig. 1 shown device；
Fig. 3 is that stainless steel and self-control cavate black matrix are measured using the device of the invention and method in 193K in 5~20 μm of hot spokes
Penetrate the diagram of spectrum；
Appended drawing reference:
1 Fourier Transform Infrared Spectrometer,
1-1 Michelson's interferometer,
1-2 binary channels MCT detector,
1-3 circuit board,
1-4 diamond window,
1-5 computer,
2 machinery modulation systems,
2-1 chopper,
2-2 lock-in amplifier,
3 high vacuum sample rooms,
3-1 sample,
3-2 sample stage.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
Fourier Transform Infrared Spectrometer due to high-resolution and high s/n ratio, and can high efficiency acquire radiation energy
Amount, and become best spectroscopy instruments in infrared band.Therefore inventor herein propose machinery modulation based on chopper and
Under step-scan mode, the double modulation technology that the interference modulations of Fourier Transform Infrared Spectrometer combine, come infrared in carrying out
The detection of radiation signal, to obtain the middle infrared emanation spectrum of high quality.Namely based on vacuum type Fourier transform infrared spectroscopy
The Michelson's interferometer interference modulations of instrument and the double modulation technology of chopper machinery modulation, obtain the middle infrared emanation of material
The method and apparatus of spectrum.
In order to obtain the middle infrared emanation spectrum of high quality, the steam and carbon dioxide in elimination air are to sample emission
The selection of signal absorbs, and sample emission signal is extracted from the signal that detector detects and guarantees that detector effectively receives
Radiation signal etc. is main problem.For the selection absorption of steam and carbon dioxide to sample emission signal in air, to Fu
In leaf transformation infrared spectrometer and high vacuum sample room vacuumize respectively, so that entire optical path is in higher vacuum, eliminate steam
Deng absorption interference.For the interference effect of room temperature background radiation, using by the machinery modulation of chopper and step-scan mode
Double modulation technology that the interference modulations of lower Fourier Transform Infrared Spectrometer combine extracts sample emission signal.Further
Ground is effectively received sample emission signal for guarantee detector, is subtracted using the Diamond window in mid and far infrared high transmittance
The few loss of sample in the transmission.In addition, also use has highly sensitive and high s/n ratio binary channels MCT to visit in middle infrared band
Device is surveyed to ensure that faint sample emission signal can be received.
Specifically, the device of the invention based on infrared emanation spectrum in double modulation technology measurement material, comprising: Fu Li
Leaf transformation infrared spectrometer, machinery modulation system and high vacuum sample room.
The Fourier Transform Infrared Spectrometer is vacuum type Fourier Transform Infrared Spectrometer.The vacuum type Fourier transformation
Infrared spectrometer, including sample emission signal decomposition is realized interference at reflection signal and transmission signal with certain optical path difference
Michelson's interferometer, signal of the reception from Michelson's interferometer and the centering infrared radiation signal of modulation have highly sensitive
The binary channels MCT detector of degree, the circuit for being used to acquire and record radiation signal information being connected with binary channels MCT detector
Plate, the computer containing inverse Fourier transform program being connected with circuit board.
Binary channels MCT detector is liquid nitrogen refrigerating, to reduce the interference that background noise measures radiation signal.In addition,
The vacuum type Fourier Transform Infrared Spectrometer further include for reduce decaying of the radiation signal in transmission process and use
The diamond window of mid and far infrared broadband range high transmittance.It specifically, can on the shell of Fourier Transform Infrared Spectrometer
It is used as radiation signal entrance equipped with opening, diamond window is set in the opening.
Above-mentioned machinery modulation system, including chopper and lock-in amplifier.The control unit of chopper refers to same frequency
Signal is input to the reference signal input interface of lock-in amplifier；The AC signal output interface and lock of binary channels MCT detector
The signal input interface of phase amplifier is connected；The signal output interface of lock-in amplifier and the direct current of binary channels MCT detector are believed
Number input interface is connected.
Above-mentioned high vacuum sample room, including sample to be tested and specimen holder；Vacuum degree 1.3~6.0 × 10-3mbar。
Above-mentioned sample to be tested is block and thin-film material with different emissivity.
On the other hand, it using the method for above-mentioned apparatus measurement material thermal radiation optical spectrum, mainly comprises the steps that
S1, chopper is fixed on to sample emission signal enters in the optical path of Fourier Transform Infrared Spectrometer.In the step
In rapid, Fourier Transform Infrared Spectrometer can be placed in general measure mode, detector selects LN-MCT mid, by computer
Signal check function in software, adjustment optical path keep sample signal maximum.
S2, Fourier Transform Infrared Spectrometer and vacuum specimen chamber are vacuumized respectively.For example, can be red by Fourier transformation
External spectrum instrument and vacuum specimen chamber be evacuated to 1mbar respectively hereinafter, eliminate 99% or more atmosphere in vapor and titanium dioxide
Carbon absorbs the selection of material radiation signal.
S3, starting chopper carry out machinery modulation to the radiation signal of sample；Radiation signal after machinery modulation enters
Fourier Transform Infrared Spectrometer carries out interference modulations to radiation signal by Michelson's interferometer, forms double modulated signal；It is double
Modulated signal is received by binary channels MCT detector, and the signal input interface of lock-in amplifier is input in the form of AC signal；
Machinery modulation is demodulated through lock-in amplifier, extracts and is obtained from sample heat radiation from the signal that detector receives
Direct current signal, and it is input to the direct current signal input interface of binary channels MCT detector.It in this step, can be by Fourier transformation
Infrared spectrometer is placed in step-scan test, and detector selects DC-IN；
The direct current signal that S4, circuit board acquisition are input to MCT detector obtains corresponding interference pattern, and is entered into meter
In calculation machine, inverse Fourier transform is carried out using software, obtains infrared emanation spectrum in the double modulation of sample.
Preferably, the Fourier Transform Infrared Spectrometer can be Bruker Vertex 70V type FTIR spectrum instrument；Institute
The chopper stated can be 540 type mechanical chopper of Standford SR；The lock-in amplifier can be Standford
SR830 DSP type lock-in amplifier；The detector can be the binary channels MCT detector of Bruker；The sample is room
The lower solid material with different emissivity of temperature.The present invention is not limited to above-mentioned model devices, can also be using with identical function
Device replaced.As long as such as Fourier transform spectrometer, is used with step-scan (step-scan) scan pattern
Vacuum type Fourier transform spectrometer,；Chopper can also be used the blade dimensions of other models slightly larger than paraboloid gold mirror ruler
Very little chopper replaces.
The present invention mainly radiates double modulation technology, that is, chopper machinery modulation and interferometer interference modulations applied to material
The measurement of spectrum.To enable chopper blade smoothly to carry out machinery modulation to radiation signal, chopper is placed on high vacuum sample
On bracket in product room, enable radiation signal periodically by chopper blade.Bracket is mainly used for fixed chopper, so that
Chopper is stablized.And bracket can be set to delustering functions, such as can coat pitch-dark etc..Further, to enable chopper
It works in high vacuum environment, vacuum adapter can be crossed by the control line of chopper and chopper by be set to high vacuum sample room
Control unit is connected, to realize that the data under vacuum environment are transmitted.
Great advantage of the invention is:
1, entire optical path is in vacuum state, eliminates the interference of steam and carbon dioxide in atmospheric environment；
2, the application of double modulation technology can effectively extract sample emission signal from the signal that detector measures；
3, in the wide wave-length coverage of mid and far infrared the diamond window of high transmittance and highly sensitive binary channels MCT detector knot
Conjunction can effectively receive faint intermediate infrared radiation signal；
4, device measuring speed is fast, easy to operate.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Fig. 1 show an of the invention implementation form based on the device of infrared emanation spectrum in double modulation measurement material
Structural schematic diagram.As shown in Figure 1, the device of infrared emanation spectrum includes: in the double modulation measurement material of this implementation form
It includes: vacuum type Fourier Transform Infrared Spectrometer 1, machinery modulation system 2, high vacuum sample room 3.
The vacuum type Fourier Transform Infrared Spectrometer 1, including the Michelson's interferometer 1-1 for interference modulations.It steps
Ke Erxun interferometer 1-1 is usually mainly made of beam splitter, index glass and horizontal glass.Wherein in the process of intermediate infrared radiation spectral measurement
In, using KBr beam splitter.Wherein in step-scan scan pattern test process, index glass is moved by way of step-scan
Dynamic, when carrying out data acquisition, index glass remains static.Each section of interferometer is fixed on Fourier Transform Infrared Spectrometer
In internal stent.
The vacuum type Fourier Transform Infrared Spectrometer 1 further includes that centering infrared radiation signal has highly sensitive bilateral
Road MCT detector 1-2.Binary channels MCT detector is located at the terminal of optical path, is converted into for receiving signal, and by radiation signal
Electric signal.That is, interferometer is located between chopper and binary channels MCT detector, to the spoke of chopped device machinery modulation
It penetrates signal and carries out interference modulations, and receive double modulated signal by binary channels MCT detector.
Preferably, between interferometer and chopper, and between interferometer and binary channels MCT detector it is additionally provided with light
Pass guiding element, such as face mirror is thrown, to carry out light path converting.As shown in Figure 1, the directional light from chopper throws face mirror by one
Generally vertical direction conveying is converted to, and interferometer is delivered to favouring vertical direction by another throwing face mirror.And from dry
The radiation signal of the vertical direction of interferometer is delivered to binary channels MCT detector by two throwing face mirrors.
The vacuum type Fourier Transform Infrared Spectrometer 1 further includes the circuit board for acquiring and recording radiation signal information
1-3.Circuit board 1-3 is mainly made of the different integrated circuit board of function, can be divided into control instrument sample circuit, control instrument
Motion circuitry, measuring signal conversion output circuit, instrument optimum state automatic control circuit and instrument failure self-checking circuit.Control instrument
Motion circuitry is connected to control the movement of the index glass of interferometer in test process with interferometer；Control instrument sample circuit and detection
Device is connected, and samples to the direct current signal for being input to detector after lock-in amplifier demodulates, and acquisition signal is inputed to
Measuring signal converts output circuit, is finally conveyed to computer and is handled.Each modular circuit is carried out by computer in circuit board
Control, and monitor its operating status.Circuit board 1-3 passes through the signal transmission line and bilateral in Fourier Transform Infrared Spectrometer
Road MCT detector is connected, and the ethernet port of circuit board is connected by data line with computer.
The vacuum type Fourier Transform Infrared Spectrometer 1 further includes the diamond window 1-4 of mid and far infrared high transmittance.Gold
The parallel light entrance of Fourier Transform Infrared Spectrometer is arranged in hard rock window 1-4.
The vacuum type Fourier Transform Infrared Spectrometer 1 further includes the computer 1-5 containing inverse Fourier transform software.Meter
Calculation machine 1-5 can carry out inverse Fourier transform to the collected interference pattern of foregoing circuit plate using program, and for showing Fourier
Transform infrared spectroscopy operating condition.
The machinery modulation system 2 includes chopper 2-1 and lock-in amplifier 2-2.Chopper 2-1 is to sample emission signal
Carry out machinery modulation.The control unit of chopper 2-1 believes the reference that the reference signal of same frequency is input to lock-in amplifier 2-2
Number input interface；The AC signal output interface of binary channels MCT detector 1-2 and the signal input interface of lock-in amplifier 2-2
It is connected；The signal output interface of lock-in amplifier 2-2 is connected with the direct current signal input interface of binary channels MCT detector 1-2.It cuts
Wave device 2-1 is arranged in radiation signal and enters in the optical path of Fourier Transform Infrared Spectrometer directional light entrance.Further, may be used
The height for adjusting chopper 2-1, enables radiation signal to pass through the exterior portion of chopper blade.
Above-mentioned high vacuum sample room 3 includes sample to be tested 3-1 and specimen holder 3-2.Sample to be tested 3-1 is set to specimen holder 3-2
On.Specimen holder can be rectangle oxygen-free copper block structure, and being provided with such as diameter is 25.4mm, and depth is the groove of 5mm,
It can be used for placing sample to be tested 3-1.
Specifically, sample to be tested 3-1 is fixed on sample stage 3-2, chopper 2-1 and interferometer 1-1 are modulated, warp
Radiation signal after double modulation is received by binary channels MCT detector 1-2.Binary channels MCT detector received signal can indicate
Are as follows:
VPSD=Vsig sin(ωt+θsig)+Vback (1)
It is wherein Vsigsin(ωt+θsig) it is intermediate infrared radiation signal of the sample through double modulation, VbackIt is background radiation letter
Number；
The signal that above-mentioned signal passes through the AC signal output end feed-in lock-in amplifier 2-2 of binary channels MCT detector 1-2
Input terminal, while the control unit of chopper is by same frequency reference signal Vrefsin(ωt+θref) feed-in lock-in amplifier 2-2
Reference signal input terminal, through signal processed in lock-in amplifier are as follows:
VPSD=1/2VsigVref cos(θsig-θref) (2)
Above-mentioned signal be direct current signal, the signal input port feed-in binary channels MCT detector through lock-in amplifier it is straight
Flow signal input part.The direct current signal on binary channels MCT detector is acquired by circuit board again, and in the form of interference pattern
It is input to computer 1-2, inverse Fourier transform is carried out by the software in computer and obtains infrared emanation light in sample double modulation
Spectrum；
In view of above-mentioned thinking, in the present embodiment, lock-in amplifier 2-2 is that Standford SR830 DSP type locking phase is put
Big device；Chopper 2-1 is 540 type mechanical chopper of Standford SR；Fourier Transform Infrared Spectrometer 1-1 is Bruker
Vertex 70V type FTIR spectrum instrument；Detector 1-3 is the implementation that Bruker binary channels MCT detector proposes new method.
Illustrate the specific operation process of above-mentioned apparatus below.
Data acquisition: chopper is mounted in the optical path between sample and spectrometer and signal can be enable from chopper leaf
Piece passes through, by the reference signal input terminal of the reference signal output end connection lock-in amplifier of chopper.Binary channels MCT is detected
The signal input part of the AC signal output end connection lock-in amplifier of device, and the signal output end feed-in of lock-in amplifier is double
Channel MCT detector direct current signal input terminal.Before test, Fourier Transform Infrared Spectrometer is placed in general measure mould
Formula, detector select LN-MCT mid option, and the signal for showing that binary channels MCT detector detects by the signal check page is strong
Degree, adjustment optical path make signal strength detection reach maximum.In conjunction with the modulating frequency of chopper, lock-in amplifier sample integration is set
Time is 30ms, to improve the signal-to-noise ratio for obtaining lock-in amplifier and extracting signal.In Fourier Transform Infrared Spectrometer stepping
Scan pattern sets the stepping waiting time as 50ms, and detector selects DC-IN.Parameter setting finishes, and starts infrared in double modulation
The measurement of thermal radiation optical spectrum.
Data processing: infrared emanation spectrum in double modulation proposed by the present invention completes interference pattern by computer software
Inverse Fourier transform obtain.
It is above-mentioned two aspect in contain key inventive point (1) of the invention in conjunction with chopper machinery modulation and demodulation with
The interference modulations and demodulation of interferometer, to extract the radiation letter of high s/n ratio from the signal that binary channels MCT detector detects
Number；(2) to whole device vacuumize process, interference of the steam to radiation signal is eliminated；(3) highly sensitive, high s/n ratio double
Channel MCT detector significantly enhances the detectivity of faint intermediate infrared radiation signal；(4) use is in the wide wavelength model of mid and far infrared
The diamond window for enclosing high transmittance ensure that the signal strength that detector can receive.
As application example, as shown in figure 3, side of the present invention with infrared emanation spectrum in double modulation measurement material
Method, measure 193K low-launch-rate middle infrared emanation spectrum at 5~20 μm of stainless steel and self-control cavate black matrix.From figure
As can be seen that the difference between stainless steel hot radiation spectrum and the thermal radiation optical spectrum for making cavate black matrix by oneself is clearly.And hot spoke
It penetrates spectrum integrally to present as the increase of wavelength first increases the trend reduced afterwards, be consistent with theory.Prove that package unit can be smoothly
For measure with it is various difference emissivity materials middle infrared emanation spectrum.
The present invention by using Michelson's interferometer carry out interference modulations vacuum type Fourier Transform Infrared Spectrometer,
Chopper, the lock-in amplifier for demodulation and the high vacuum sample of machinery modulation are carried out to radiation signal using chopper wheel
Room constructs the method and apparatus based on infrared emanation spectrum in double modulation technology measurement material.
The present invention can effectively extract sample emission signal, the Gao Zhen of whole device from the signal that detector receives
Sky can eliminate the absorption of 99% or more steam and carbon dioxide to radiation signal respectively, and diamond window can ensure that radiation signal height
Energy transmission guarantees that detector can receive sufficiently strong signal strength, infrared emanation light in the sample to obtain high-quality
Spectrum.
The industrial applicability present invention has device simple, easy to operate, the high advantage of stability, is suitable for various emissivity blocks
The detection of body and thin-film material thermal radiation property.
Under the objective for not departing from essential characteristic of the invention, the present invention can be presented as diversified forms, therefore in the present invention
Implementation form be to be illustrative rather than definitive thereof, limited since the scope of the present invention is defined by the claims rather than by specification,
And all changes fallen in the full scope of equivalents of the range that claim defines or the range that it is defined be understood to include
In detail in the claims.
Claims (10)
1. a kind of device based on infrared emanation spectrum in double modulation technology measurement material characterized by comprising
Fourier Transform Infrared Spectrometer (1), machinery modulation system (2) and high vacuum sample room (3)；
The Fourier Transform Infrared Spectrometer (1), including by sample emission signal decomposition at the reflection with certain optical path difference
Signal and transmission signal realize the Michelson's interferometer (1-1) of interference modulations, receive the signal from Michelson's interferometer
Binary channels MCT detector (1-2), be connected with binary channels MCT detector for acquiring and recording the electricity of radiation signal information
Road plate (1-3), the computer (1-5) containing inverse Fourier transform program being connected with circuit board；
The machinery modulation system (2), including chopper (2-1) and lock-in amplifier (2-2)；The control list of chopper (2-1)
Same frequency reference signal is input to the reference signal input interface of lock-in amplifier (2-2) by member；Binary channels MCT detector (1-
2) AC signal output interface is connected with the signal input interface of lock-in amplifier (2-2)；The signal of lock-in amplifier (2-2)
Output interface is connected with the direct current signal input interface of binary channels MCT detector (1-2)；
The high vacuum sample room (3), including specimen holder (3-2) and set on the sample to be tested (3-1) of the specimen holder (3-2).
2. the apparatus according to claim 1, which is characterized in that the Fourier Transform Infrared Spectrometer (1) further include
The diamond window (1-4) of mid and far infrared broadband range high transmittance.
3. device according to claim 1 or 2, which is characterized in that the vacuum degree of the high vacuum sample room (3) reaches
1.3~6.010-3 mbar。
4. device according to any one of claim 1 to 3, which is characterized in that the Fourier Transform Infrared Spectrometer
It (1) is vacuum type.
5. device according to any one of claim 1 to 4, which is characterized in that the binary channels MCT detector is liquid nitrogen
Refrigeration mode.
6. a kind of method based on infrared emanation spectrum in the measurement material of device described in any one of claims 1 to 5,
Feature, comprising the following steps:
S1, the radiation signal that chopper is fixed on to sample to be tested enter in the optical path of Fourier Transform Infrared Spectrometer；
S2, Fourier Transform Infrared Spectrometer and vacuum specimen chamber are vacuumized respectively；
S3, starting chopper carry out machinery modulation to the radiation signal of sample to be tested；Radiation signal after machinery modulation enters
Fourier Transform Infrared Spectrometer carries out interference modulations to radiation signal by Michelson's interferometer, forms double modulated signal；It is double
Modulated signal is received by binary channels MCT detector, and the signal input interface of lock-in amplifier is input in the form of AC signal；
Machinery modulation is demodulated through lock-in amplifier, from the signal that binary channels MCT detector receives extract obtain to
The direct current signal of the heat radiation of sample, and it is input to the direct current signal input interface of binary channels MCT detector；
The direct current signal that S4, circuit board acquisition are input to binary channels MCT detector obtains corresponding interference pattern, and is entered into
In computer, inverse Fourier transform is carried out using program, obtains infrared emanation spectrum in the double modulation of sample to be tested.
7. according to the method described in claim 6, it is characterized in that, in step sl, Fourier Transform Infrared Spectrometer is set
In measurement pattern, by the signal check function in the program of computer, adjusting optical path keeps the radiation signal of sample to be tested maximum.
8. method according to claim 6 or 7, which is characterized in that in step s 2, by Fourier Transform Infrared Spectrometer
It is evacuated to 1 mbar or less respectively with vacuum specimen chamber.
9. the method according to any one of claim 6 to 8, which is characterized in that in step s3, Fourier transformation is red
External spectrum instrument is placed in step-scan test.
10. method according to any one of claims 6 to 9, which is characterized in that the sample to be tested is various with not
With the block and thin-film material of emissivity.
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