CN114485981A - Temperature measurement method and temperature measurement device based on diamond first-order Raman spectrum - Google Patents
Temperature measurement method and temperature measurement device based on diamond first-order Raman spectrum Download PDFInfo
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Abstract
The invention discloses a temperature measurement method based on diamond first-order Raman spectroscopy, which comprises the following steps: step 1, collecting first-order Raman spectrum data of the diamond at different temperatures, and recording corresponding temperature values as a data set; step 2, fitting is carried out through a Voigt fitting function based on the data set obtained in the step 1, and a full width at half maximum value, a central position and peak intensity of a corresponding Raman peak are obtained; step 3, constructing a monotonic function curve group related to temperature change through nonlinear fitting; step 4, putting the diamond into a temperature field to be measured, and obtaining a full width at half maximum value, a central position and peak intensity of a corresponding Raman peak based on the fitting function in the step 2; and 5, inputting the data measured in the step 4 into the monotonic function curve group, and analyzing and judging to output a final temperature value. The invention also provides a temperature measuring device based on the method. The method provided by the invention can be used for ensuring the accuracy of the final temperature measurement result on the basis of completing the temperature detection.
Description
Technical Field
The invention relates to the technical field of temperature detection, in particular to a temperature measuring method and a temperature measuring device based on diamond first-order Raman spectroscopy.
Background
The non-contact temperature measurement technology has the characteristics of high upper limit of temperature measurement, no damage to scenes and the like, and is widely applied to the fields of production and life, scientific research, modern national defense and the like. Infrared thermometry is a common non-contact thermometry method, but the method is greatly influenced by the emissivity and reflectivity of the measured surface and the ambient atmosphere, so that the measurement accuracy is greatly reduced. For temperature measurement in severe environments such as radiation, corrosion, high frequency and high voltage, conventional measurement means cannot meet the requirements, and therefore, an effective temperature measurement method is urgently needed to be developed.
Diamond has excellent physicochemical properties such as high hardness, corrosion resistance, high thermal conductivity, etc., making it absolutely advantageous in withstanding extreme conditions. The Raman spectrum is a scattering spectrum, has the characteristics of rapidness, high efficiency and no damage, and is not influenced by the surface emissivity, the reflectivity and the environmental atmosphere of a detected sample. In terms of scattered signal energy, the raman spectrum is divided into two types, namely a Stokes peak and an anti-Stokes peak, wherein scattered photons with energy smaller than that of incident photons are Stokes signals (Stokes), and scattered photons with energy larger than that of incident photons are anti-Stokes signals (anti-Stokes).
Patent document CN112683419B discloses a method for accurately detecting temperature based on surface enhanced raman scattering effect, which includes the following steps: (1) loading the plasmon nanoparticle single-layer film on a support substrate; (2) soaking the single-layer film substrate in a probe molecular solution, and drying to prepare a hard substrate temperature sensor or a flexible substrate temperature sensor; (3) placing the hard substrate temperature sensor or the flexible substrate temperature sensor at a gradient working temperature to acquire a Raman spectrum of the surface of the hard substrate temperature sensor or the flexible substrate temperature sensor, and establishing a standard curve between a characteristic temperature and corresponding characteristic peak intensity; (4) and placing the hard substrate temperature sensor or the flexible substrate temperature sensor in a detection range, collecting the Raman spectrum of the surface of the hard substrate temperature sensor or the flexible substrate temperature sensor, reading the peak intensity of the characteristic peak and comparing the peak intensity with a standard curve of the temperature interval, and realizing the detection of the unknown environment temperature.
The method adopts the fitting of the characteristic Raman peak intensity and the temperature value to obtain a characteristic Raman peak intensity-temperature value curve, but the characteristic Raman peak intensity has very high requirement on the purity of the probe material, namely the identification precision of the probe can be influenced after the probe is replaced.
Patent document CN111896140A discloses an optical fiber temperature sensor and system, including: optical fiber, pulse laser, temperature-sensing portion, diamond portion and detection portion, have a plurality of nitrogen vacancy centers in the diamond portion, density through this metal nanoparticle changes to arouse that the magnetic field intensity that this metal nanoparticle produced changes, and because contain a plurality of nitrogen vacancy centers in this diamond portion, make this diamond portion can produce fluorescence under the effect in magnetic field, when the magnetic field intensity that this metal nanoparticle produced changes, the fluorescence intensity that this diamond portion produced under the effect in magnetic field also changes, detect through the fluorescence intensity change to this diamond portion, and through the corresponding relation of this fluorescence intensity and this temperature that awaits measuring, obtain the temperature that awaits measuring.
In the method, diamond is only used as a temperature carrier, is irrelevant to final temperature detection, and the magnetic field intensity change is easily influenced by the external environment.
Disclosure of Invention
In order to solve the problems, the invention provides a temperature measurement method based on diamond first-order Raman spectroscopy, which constructs a monotonic function curve group for mutual verification based on key parameters of three first-order Raman spectroscopy, and ensures the accuracy of a final temperature measurement result on the basis of finishing temperature measurement.
A temperature measurement method based on diamond first-order Raman spectroscopy comprises the following steps:
step 1, collecting first-order Raman spectrum data of the diamond at different temperatures through a Raman spectrometer, and recording corresponding temperature values to serve as a data set;
step 2, fitting through a Voigt fitting function based on the data set obtained in the step 1, wherein the Gauss width is consistent with the resolution of the Raman spectrometer in the step 1, and obtaining a half-height width value, a central position and peak intensity of a Raman peak corresponding to each temperature value;
and 3, constructing a monotonic function curve group related to temperature change by nonlinear fitting according to the data obtained by fitting in the step 2 and the corresponding temperature value:
constructing a half-height width-temperature standard curve based on the half-height width value and the corresponding temperature value of the Raman peak;
constructing a Raman displacement-temperature standard curve based on the central position of the Raman peak and the corresponding temperature value;
constructing an intensity ratio-temperature standard curve based on the peak intensity of the Raman peak and the corresponding temperature value;
step 4, placing the diamond in a temperature field to be measured, collecting first-order Raman spectrum data under the temperature value through a Raman spectrometer, and analyzing the Voigt fitting function in the step 2 to obtain a full width at half maximum value, a central position and peak intensity of a corresponding Raman peak;
and 5, inputting the data measured in the step 4 into a monotonic function curve group, and analyzing and judging to output a final temperature value.
The temperature value and the temperature are both absolute temperatures, and the unit is Kelvin (K).
According to the method, diamonds in a temperature field to be measured are collected through a Raman spectrometer, and the actual temperature in the temperature field to be measured is obtained through inverse calculation of the diamonds and a fitted temperature monotonic function curve group.
Preferably, the diamond in the step 1 is single crystal diamond, so that the influence of impurities on first-order Raman spectrum data is avoided, and the accuracy of the data is ensured.
Preferably, in the step 1, data acquisition is performed at intervals of 50k at different temperatures, specifically within a certain temperature interval, and the heating time of the diamond is not less than 1min, so that the obtained first-order raman spectrum data is ensured to be the final stable parameter, and the subsequent fitting of a monotonic function curve is facilitated.
Specifically, the emitted laser of the middle Raman spectrometer in the step 1 is 532nm green light, and the range of the collected scattering signal is 1280cm-1-1350cm-1The acquisition time was 10 s.
Specifically, the mid-peak intensity of step 2 includes an anti-stokes peak intensity and a stokes peak intensity.
Preferably, the analysis and judgment in step 5 is based on the difference between the maximum value and the minimum value of the output results of the three temperature standard curves: when the difference is larger than the threshold value, temperature needs to be measured again; and when the difference value is smaller than the threshold value, calculating the average value of the three output results as a final temperature value to be output.
The invention also provides a temperature measuring device based on the temperature measuring method, and the device can rapidly measure the actual temperature of the material or the temperature field in 300k-1200k in a direct contact mode.
A temperature measuring device based on a diamond first-order Raman spectrum temperature measuring method comprises:
the detection module is used for contacting an object to be detected or stretching into a space to be detected to acquire first-order Raman spectrum data;
the spectrum analysis module is used for analyzing the first-order Raman spectrum data acquired by the detection module;
and the temperature analysis module judges the analysis result of the spectrum analysis module and outputs a final temperature value.
Specifically, the detection module comprises a diamond probe, a high-temperature-resistant anti-oxidation material coated on the diamond and a matched Raman spectrometer, and the problem that the diamond is easy to oxidize at high temperature is solved through the high-temperature-resistant anti-oxidation material coated on the diamond.
Preferably, the high-temperature-resistant anti-oxidation material is aluminum nitride, and compared with other coating materials with the same performance, the material is high in thermal conductivity and firmer in combination with diamond, and the coating is prevented from influencing the measurement of the actual temperature.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts the principle that the first-order Raman spectrum data of the diamond has a certain change rule at different temperatures, which is different from the traditional infrared temperature measurement method, and fits a monotonic function curve related to the temperature change.
(2) The method selects three key parameters in the first-order Raman spectrum data, fits three monotonic function curve groups related to temperature change, and provides accuracy of the final temperature value measurement through mutual verification.
Drawings
FIG. 1 is a schematic flow chart of a temperature measurement method according to the present invention;
FIG. 2 is a first order Raman spectrum of diamond at different temperatures;
FIG. 3 is a graph of full width at half maximum versus temperature standard calculated by step 3 of the thermometry method of the present invention;
FIG. 4 is a Raman shift versus temperature standard curve calculated by step 3 of the thermometry method of the present invention;
FIG. 5 is a graph of intensity ratio versus temperature criteria calculated by step 3 of the thermometry method of the present invention;
fig. 6 is a graph comparing the temperature value measured by the temperature measuring device and the temperature change curve of the hot stage.
Detailed Description
The present example is based on the temperature response characteristic of the single crystal diamond first order raman spectrum to achieve temperature measurement.
Firstly, heating or cooling the diamond by using a temperature changing device, recording a temperature value displayed by equipment, and then collecting a Raman spectrum of the diamond at the current temperature; changing the temperature, and measuring Raman spectra at a plurality of temperatures; then, performing fitting analysis on the acquired Raman spectrum, extracting the central position, the full width at half maximum and the intensity data of a Raman peak, and establishing a functional relation between the extracted data and the temperature; then, placing the diamond in a temperature field to be measured, and collecting a Raman spectrum; and finally, substituting the extracted data into the functional relation, and performing reverse calculation to obtain a temperature value.
The specific steps are shown in figure 1:
step 1, collecting first-order Raman spectrum data of the diamond at different temperatures through a Raman spectrometer, and recording corresponding temperature values as a data set:
placing a single-crystal diamond in a sample chamber of a high-temperature heating table, controlling the heating table to heat or cool the diamond through a temperature control device connected with the heating table, carrying out heat preservation for 1min at temperature points at intervals of 50K within a temperature range of 300K-1200K, and recording temperature values of the temperature points during the heat preservation period;
when the temperature value is stable, the excitation laser (532nm green light) of the Raman spectrometer is focused on the surface of the diamond, and the Raman spectrometer is used for collecting 1280cm-1-1350cm-1The signal is a single peak, and the acquisition time is 10 s.
As shown in fig. 2, the collected first-order raman spectrogram has a stokes peak moving towards a low-frequency direction along with the increase of temperature, and has weaker intensity along with the broadening of the peak shape; the position and the peak shape of the anti-Stokes peak are symmetrically changed relative to the Stokes peak, and the intensity is gradually enhanced; in addition, the background signal is easy to deduct, the obtained physical signal is clean, the signal-to-noise ratio is high, and the measurement precision is improved.
And 2, fitting by a Voigt fitting function based on the data set obtained in the step 1, wherein the Gauss width is consistent with the resolution of the Raman spectrometer in the step 1, and obtaining a half-height width value, a central position and peak intensity of each temperature value corresponding to a Raman peak, wherein the peak intensity comprises anti-Stokes peak intensity and Stokes peak intensity:
the scattering signal is fit analyzed by a control computer connected to the Raman spectrometer, the fitting function is a Voigt function, 0.55cm-1The resolution of the raman spectrometer of (a) is fixed as the Gauss width in the Voigt function, where the basis for fitting the Voigt function is:
y＝y0+(f1(x)*f2(x))
wherein y is0Is the shift of the fitted curve from the ordinate of the actual spectrum, x is the abscissa of the first-order Raman spectrum, xcIs the Raman shift (peak center frequency), A is the peak area, wLIs the Lorentz width, wGIs gaussian in width.
When degree of fitting R2When the maximum value is reached, obtaining the half-height width value of the Raman peak corresponding to each temperature point, the central position of the Raman peak and the peak intensity, wherein the peak intensity comprises the anti-Stokes peak intensity and the Stokes peak intensity.
And 3, constructing a monotonic function curve group related to temperature change by nonlinear fitting according to the data obtained by fitting in the step 2 and the corresponding temperature value:
as shown in fig. 3, based on the full width at half maximum value of the raman peak and the corresponding temperature value, a full width at half maximum-temperature standard curve is constructed:
taking a scatter diagram of the temperature value (X) of each temperature point and the obtained full width at half maximum (Y) of the Raman peak corresponding to each temperature point, and carrying out nonlinear fitting by using a phonon decay model to establish a full width at half maximum-temperature standard curve:
wherein Γ is full width at half maximum; t is the absolute temperature; omega is the phonon frequency (unit cm-1) of triple degenerated LTO phonons at the center of the diamond Brillouin zone, and the omega is reflected in a Raman spectrum and is Raman shift;
n (ω, T) ═ 1/[ exp (hc ω/kT) -1] is the temperature-dependent bose-einstein phonon distribution function;
a and B are adjustable parameters which respectively correspond to the relative contribution of the three-phonon process and the four-phonon process to the full width at half maximum during phonon decay; h, c and k are Planck constant, light speed and Boltzmann constant respectively.
As shown in fig. 4, a raman shift-temperature standard curve is constructed based on the central position of the raman peak and the corresponding temperature value:
taking a scatter diagram of the temperature value (X) of each temperature point and the central position (Y) of the Raman peak corresponding to each obtained temperature point, performing nonlinear fitting, and establishing a Raman displacement-temperature standard curve:
wherein Ω is the raman shift; omega0Raman shift at 0K; t is the absolute temperature; omega is the phonon frequency (unit cm-1) of triple degenerated LTO phonons at the center of the diamond Brillouin zone, and the omega is reflected in a Raman spectrum and is Raman shift;
n (ω, T) ═ 1/[ exp (hc ω/kT) -1] is the temperature-dependent bose-einstein phonon distribution function;
c and D are adjustable parameters which respectively correspond to the relative contribution of the three-phonon process and the four-phonon process to the full width at half maximum during phonon decay; h, c and k are Planck constant, light speed and Boltzmann constant respectively.
As shown in fig. 5, based on the peak intensity of the raman peak and the corresponding temperature value, an intensity ratio-temperature standard curve is constructed:
calculating the ratio of the anti-Stokes peak intensity to the Stokes peak intensity, then making a scatter diagram of the temperature value (X) of each temperature point and the calculated intensity ratio (Y) of each temperature point, performing nonlinear fitting, and establishing an intensity ratio-temperature standard curve;
wherein ω islIs the incident laser frequency, γ is the correction factor;
step 4, placing the diamond in a temperature field to be measured, collecting first-order Raman spectrum data under the temperature value through a Raman spectrometer, and analyzing the Voigt fitting function in the step 2 to obtain a full width at half maximum value, a central position and peak intensity of a corresponding Raman peak;
and 5, inputting the data measured in the step 4 into a monotonic function curve group, and analyzing and judging to output a final temperature value.
A temperature measuring device based on a diamond first-order Raman spectrum temperature measuring method comprises:
the detection module is used for contacting an object to be detected or stretching into a space to be detected to acquire first-order Raman spectrum data;
the spectrum analysis module is used for analyzing the first-order Raman spectrum data acquired by the detection module;
and the temperature analysis module judges the analysis result of the spectrum analysis module and outputs a final temperature value.
The detection module comprises a diamond probe, aluminum nitride coated on the diamond and a matched Raman spectrometer.
The judging method of the device comprises the following steps: the spectral analysis module outputs three temperature monotonic function curve values t1，t2And t3And analyzing by a temperature analysis module:
when | t1-t2|≤t0，|t1-t3|≤t0And | t3-t2|≤t0If the two are true, the output is finally
Otherwise, when one of the inequalities is not true, the operator is informed to re-detect.
Wherein t is0For the predetermined threshold, 5k is usually selected.
As shown in FIG. 6, in the temperature interval 300k-1200k, the output results of the three monotonic functions are overlapped together, and the finally fitted temperature change curve is basically overlapped with the temperature change curve of the hot stage, which shows that the temperature detection accuracy of the device is high.
Claims (9)
1. A temperature measurement method based on diamond first-order Raman spectroscopy is characterized by comprising the following steps:
step 1, collecting first-order Raman spectrum data of the diamond at different temperatures through a Raman spectrometer, and recording corresponding temperature values to serve as a data set;
step 2, fitting through a Voigt fitting function based on the data set obtained in the step 1, wherein the Gauss width is consistent with the resolution of the Raman spectrometer in the step 1, and obtaining a half-height width value, a central position and peak intensity of a Raman peak corresponding to each temperature value;
and 3, constructing a monotonic function curve group related to temperature change by nonlinear fitting according to the data obtained by fitting in the step 2 and the corresponding temperature value:
constructing a half-height width-temperature standard curve based on the half-height width value and the corresponding temperature value of the Raman peak;
constructing a Raman displacement-temperature standard curve based on the central position of the Raman peak and the corresponding temperature value;
constructing an intensity ratio-temperature standard curve based on the peak intensity of the Raman peak and the corresponding temperature value;
step 4, placing the diamond in a temperature field to be measured, collecting first-order Raman spectrum data under the temperature value through a Raman spectrometer, and analyzing the Voigt fitting function in the step 2 to obtain a full width at half maximum value, a central position and peak intensity of a corresponding Raman peak;
and 5, inputting the data measured in the step 4 into a monotonic function curve group, and analyzing and judging to output a final temperature value.
2. The method according to claim 1, wherein the diamond in step 1 is a single crystal diamond.
3. The method according to claim 1, wherein the data acquisition is performed every 50k in the temperature interval of 300k-1200k in step 1 at different temperatures, and the duration of the diamond heating is not less than 1 min.
4. The method for measuring temperature according to claim 1, wherein the Raman spectrometer of step 1 emits 532nm green light and collects scattered signals in a range of 1280cm-1-1350cm-1The acquisition time was 10 s.
5. The thermometric method of claim 1, wherein the peak intensities in step 2 comprise an anti-stokes peak intensity and a stokes peak intensity.
6. The method according to claim 1, wherein the analysis and judgment in step 5 is based on the difference between the maximum value and the minimum value of the three output results of the temperature standard curve: when the difference is larger than the threshold value, temperature needs to be measured again; and when the difference value is smaller than the threshold value, calculating the average value of the three output results as a final temperature value to be output.
7. A temperature measuring device for implementing the diamond first-order Raman spectrum-based temperature measuring method according to any one of claims 1 to 6, comprising:
the detection module is used for contacting an object to be detected or stretching into a space to be detected to acquire first-order Raman spectrum data;
the spectrum analysis module is used for analyzing the first-order Raman spectrum data acquired by the detection module;
and the temperature analysis module judges the analysis result of the spectrum analysis module and outputs a final temperature value.
8. The thermometric apparatus according to claim 7, wherein the detection module comprises a diamond probe, a high temperature resistant and oxidation resistant material coated on the diamond, and a matched Raman spectrometer.
9. The temperature measuring device of claim 8, wherein the refractory and antioxidant material is aluminum nitride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114441505A (en) * | 2022-03-17 | 2022-05-06 | 中国工程物理研究院机械制造工艺研究所 | Water vapor in-situ calibration device and method for Raman probe and application |
| CN115343269A (en) * | 2022-07-11 | 2022-11-15 | 清华大学 | Material thermal conductivity regulation and control method and system based on phonon defect engineering |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441505A (en) * | 2022-03-17 | 2022-05-06 | 中国工程物理研究院机械制造工艺研究所 | Water vapor in-situ calibration device and method for Raman probe and application |
| CN114441505B (en) * | 2022-03-17 | 2023-08-18 | 中国工程物理研究院机械制造工艺研究所 | Water vapor in-situ calibration device for Raman probe, calibration method and application |
| CN115343269A (en) * | 2022-07-11 | 2022-11-15 | 清华大学 | Material thermal conductivity regulation and control method and system based on phonon defect engineering |
| CN115343269B (en) * | 2022-07-11 | 2023-10-03 | 清华大学 | Phonon defect engineering-based material thermal conductivity property regulation and control method and system |
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