CN112362593A - Method for measuring change of diamond substrate along with temperature - Google Patents
Method for measuring change of diamond substrate along with temperature Download PDFInfo
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- CN112362593A CN112362593A CN202011296394.1A CN202011296394A CN112362593A CN 112362593 A CN112362593 A CN 112362593A CN 202011296394 A CN202011296394 A CN 202011296394A CN 112362593 A CN112362593 A CN 112362593A
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- 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
- G01N21/21—Polarisation-affecting properties
- G01N21/211—Ellipsometry
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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
- G01N21/21—Polarisation-affecting properties
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- G01N2021/213—Spectrometric ellipsometry
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Abstract
The invention discloses a method for measuring the change of a diamond substrate along with temperature, which comprises the following steps: measurement of spectroscopic ellipsometry curve (. psi.) of diamond substrate at room temperature0，Δ0) (ii) a S1, controlling the temperature of the heating system to heat the diamond substrate, presetting i heating system temperatures, and measuring each TiEllipsometric spectrum (psi) of the underlying diamond substratei，Δi) (ii) a S2, establishing a dispersion optical model to analyze the spectral curve and recording the spectral curve as (n)0，k0) And (n)i，ki) When the graphitization condition is satisfied, the optical constant (n) is recordedi，ki，di) (ii) a S3, drawing optical constants at all temperatures, and analyzing the change trend; and S4, analyzing the change of the diamond hybridization type and the proportion distribution condition by combining a dispersion optical model after the graphitization condition is met. It has the following advantages: the method has the advantages of high measurement precision, wide temperature change range and sensitivity to refractive index and temperature change, and can obtain the change of optical characteristics and the hybridization type of the diamond substrate.
Description
Technical Field
The invention relates to the technical field of optical measurement, in particular to a method for measuring the hybridization type and the optical characteristic of a diamond substrate along with the change of temperature.
Background
Diamond is widely applied to the fields of infrared windows, high-frequency high-power electronic devices and the like due to high thermal conductivity, high mechanical strength and good optical characteristics. Because diamond belongs to V group elements and C has various valence bond forms, some hybrid states are difficult to avoid in the synthesis and processing processes of the single crystal diamond substrate, and great influence is generated on the optical characteristics of the single crystal diamond substrate. The diamond-based device is mostly used under extremely severe conditions, and the diamond can be graphitized and other component changes at high temperature, so that the thermal conductivity and the optical characteristics of the diamond-based device are changed, the performance of the device is reduced, and the service life of the device is prolonged. Therefore, the change in the composition and optical characteristics of the single crystal diamond substrate due to temperature has an important influence on the processing and even the device.
In the processing process of the single crystal diamond substrate, materials are mostly removed in a high-temperature induced graphitization mode due to extremely high hardness, and the change of components at different temperatures is detected, so that the processing efficiency of the single crystal diamond substrate can be effectively improved, and the use quality of a subsequent substrate can be ensured. Since the condition of graphitization at high temperature is complex, certain impurities and residual defects are inevitably introduced, and the impurities and the residual defects can cause the absorption of non-diamond phases, so that the transmissivity of the non-diamond phases is reduced, the accurate detection of the refractive index, the optical characteristics and the thickness of the non-diamond phases is influenced, and the optical characteristics of the substrate can be fed back in time to adjust processing parameters and determine the subsequent coating.
In the existing detection, the detection of diamond mostly refers to the detection of surface morphology and vacancy color center, such as CN108709877A, a diamond detection method and a detection apparatus, which determine whether a diamond sample is a single crystal or not by detecting a magnetic resonance spectrum curve, determine the diamond sample by using the light of a nitrogen-vacancy luminescent point defect, and further determine whether the diamond sample belongs to a single crystal sample by using the splitting condition of the spectrum line under an external magnetic field.
Most of characteristic detection along with temperature change is thin film detection, such as CN110376136A, the designed device and method for measuring the optical constant and the morphological parameter of the thin film under high temperature loading can calibrate the ellipsometric parameter deviation introduced by a quartz glass window under different heating temperatures in a wider thermal temperature range, and the optical constant and the morphological parameter of a sample to be measured can be more accurately measured by constructing a reductive measurement gas atmosphere, but if a high-temperature platform used by the device meets the condition of diamond graphitization, the measured gas atmosphere can be changed, so that errors are caused, only the optical constant and the morphological parameter are included, and the component change is not involved; for example, CN106706521A, a method for testing an optical film ultra-wideband optical constant is used to calculate a full-spectrum optical constant of an optical film material in a visible light to infrared band, especially in a wavelength range of 0.3um to 20um, by using a combination of a substrate-a spectrum transmittance of a transparent region of the film and a spectrum reflectance of a non-transparent region as a target spectrum, and using an oscillation submodel as a dispersion model of the optical constant, the ultra-wideband optical constant of the film is calculated by inverting target spectrum data, which only includes the optical constant and morphological parameters, and does not involve component changes.
Disclosure of Invention
The invention provides a method for measuring the change of a diamond substrate along with temperature, which overcomes the defects of the prior art that the characteristic detection along with the change of the temperature is mostly film detection.
The technical scheme adopted by the invention for solving the technical problem is as follows: the measuring method of the change of the diamond substrate with the temperature comprises the following steps:
s1, measuring an ellipsometric spectrum curve (ψ, Δ) of the diamond substrate, which includes: s11, measuring the ellipsometry spectrum curve (psi) of the diamond substrate at room temperature0，Δ0) (ii) a S12, controlling the temperature of the heating system to heat the diamond substrate, and presetting the temperature of i heating systems and the temperature of the ith heating system as TiEach measured in order of temperature from low to highTiEllipsometric spectrum (psi) of the underlying diamond substratei，Δi)；
S2, establishing a dispersion optical model to analyze the spectral curves, and respectively recording the spectral curves as ellipsometric spectral curves (psi)0，Δ0) Corresponding to (n)0，k0) And (psi)i，Δi) Corresponding to (n)i，ki) When the graphitization condition is satisfied, the optical constant (n) is recordedi，ki，di) N is a refractive index, k is an extinction coefficient, and d is a thickness of the diamond substrate;
s3, plotting optical constants (n) at all temperaturesi，ki，di) Analyzing the variation trend;
and S4, analyzing the change and proportion distribution condition of the diamond hybridization type by combining the established dispersion optical model after the graphitization condition is met.
In one embodiment: in S1, the ellipsometry curve of the diamond substrate is measured by a measurement system, which is a broad spectrum ellipsometer whose spectral range covers ultraviolet, visible and near infrared.
In one embodiment: the heating system in S1 satisfies the diamond graphitization condition, and the atmosphere of the heating gas is selected, and the heating gas is oxygen or nitrogen.
In one embodiment: every two adjacent T in the S1iAre equal.
In one embodiment: in S2, a dispersive optical model is selected according to whether the spectral curve is an absorption region, wherein:
if the dispersion optical model is a Cauchy model, the calculation formula is as follows:
in the formula, n is a refractive index, An, Bn and Cn are Cauchy model parameters, and lambda is a wavelength;
if the dispersion optical model is an absorption region, the dispersion optical model is a Lorentz oscillator model, and the calculation formula is as follows:
in the formula, A, En and Br are the amplitude, center position and half-wave width of the model parameter, respectively.
In one embodiment: the graphitization conditions in S4 are set as required depending on the gas atmosphere and temperature.
In one embodiment: in the S4, the optical model can improve the fitting result by adjusting the volume fraction of the diamond hybridization type, namely the graphitized specific volume, and the final graphitized degree is obtained according to the fitting condition.
Compared with the background technology, the technical scheme has the following advantages:
the method has the advantages of high measurement precision, wide temperature change range, sensitivity to refractive index and temperature change, capability of reflecting the change of the refractive index of 0.01, capability of obtaining the change of optical characteristics and the hybridization type of the diamond substrate. And selecting a built dispersion optical model according to whether the spectrum curve is an absorption region, wherein the dispersion optical model is a Cauchy model if the spectrum curve is a non-absorption region, the dispersion optical model is a Cauchy model if the spectrum curve is an absorption region, and the dispersion optical model is a Lorentz oscillator model, so that the measurement precision is high.
Drawings
The invention is further described with reference to the following figures and detailed description.
FIG. 1 is a schematic view of a measurement system according to this embodiment;
FIG. 2 is a schematic view of a heating system according to this embodiment;
fig. 3 is a schematic view of the hybrid structure of the diamond substrate according to the present embodiment.
In the figure: 11-broad spectrum light source, 12-collimating lens, 13-polarizer, 14-compensator, 15-sample stage, 16-collimating lens group, 17-compensator, 18-analyzer, 19-detector.
Detailed Description
Referring to fig. 1 to 3, a method for measuring a change in temperature of a diamond substrate includes:
s1, measuring the ellipsometry spectrum curve (ψ, Δ) of the single crystal diamond substrate, specifically: the ellipsometry curve of the diamond substrate is measured by a measurement system, which is a broad spectrum ellipsometer whose spectral range covers ultraviolet, visible and near infrared. The S1 includes:
s11, measuring the ellipsometry spectrum curve (psi) of the single crystal diamond substrate at room temperature0，Δ0) Room temperature, such as 25 degrees celsius; and
s12, controlling the temperature of the heating system to heat the diamond substrate, and presetting the temperature of i heating systems and the temperature of the ith heating system as TiMeasuring each T in a sequence of temperature from low to highiEllipsometric spectrum (psi) of the underlying diamond substratei，Δi) The method specifically comprises the following steps: presetting the temperature of the heating system, wherein the preset temperature T1When the temperature is stabilized T1Then, T is measured1Ellipsometric spectrum curve (psi) of lower single crystal diamond substrate1，Δ1) (ii) a Continuing to heat until the temperature T2After the temperature has stabilized, T is measured2Ellipsometric spectrum curve (psi) of lower single crystal diamond substrate2，Δ2) … … until all heating system temperatures within the temperature range have been detected. In this embodiment: every two adjacent T in the S1iAre equal to each other, so that the adjustment is performed according to the control variable method.
S2, establishing a dispersion optical model to analyze the spectral curves, and respectively recording the spectral curves as ellipsometric spectral curves (psi)0，Δ0) Corresponding to (n)0，k0) And (psi)i，Δi) Corresponding to (n)i，ki) When the graphitization condition is satisfied, the optical constant (n) is recordedi，ki，di) Wherein: n is a refractive index, k is an extinction coefficient, and d is the thickness of the diamond substrate; the method specifically comprises the following steps: establishing corresponding dispersion models to analyze the spectral curves, and respectively recording the spectral curves as (n)0，k0)，(n1，k1)，(n2，k2) …, when graphitization conditions are met, it is recorded as (n)1，k1，d1)，(n2，k2，d2) … … are provided. Wherein: n is0、k0And d0The optical constants were obtained at room temperature.
S3, plotting optical constants (n) at all temperaturesi，ki，di) Analyzing the variation trend to obtain optical characteristics;
and S4, analyzing the change and proportion distribution condition of the diamond hybridization type by combining the established dispersion optical model after the graphitization condition is met.
The broad spectrum ellipsometer, as shown in fig. 1, includes a broad spectrum light source 11, a collimating lens 12, a polarizer 13, a compensator 14, a multilayer film sample 15 to be measured, a collimating lens group 16, a compensator 17, an analyzer 18, and a detector 19, wherein light emitted from the broad spectrum light source 11 is irradiated on the multilayer film sample 15 to be measured through the collimating lens 12, the polarizer 13, and the compensator 14, and reflected by the collimating lens group 16, the compensator 17, the analyzer 18, and the detector 19. The broad spectrum ellipsometer has a spectral range covering ultraviolet, visible and near infrared.
The graphitization condition in this embodiment is related to the gas atmosphere and temperature, and can be set according to the requirement, and the heating system is shown in fig. 2, and the heating gas atmosphere is selected to provide a gas atmosphere of vacuum or pure oxygen, etc. in the heated diamond substrate of S12 under the diamond graphitization condition.
In S2, a dispersive optical model is selected according to whether the spectral curve is an absorption region, wherein:
if the dispersion optical model is a Cauchy model, the calculation formula is as follows:
in the formula, n is a refractive index, An, Bn and Cn are Cauchy model parameters, and lambda is a wavelength;
if the dispersion optical model is an absorption region, the dispersion optical model is a Lorentz oscillator model, and the calculation formula is as follows:
in the formula, A, En and Br are the amplitude, center position and half-wave width of the model parameter, respectively.
In this embodiment, the optical model in S4 may improve the fitting result by adjusting the volume fraction of the diamond hybridization type, i.e., the graphitization specific volume, and obtain the final graphitization degree according to the fitting condition. Specifically, the established model fits the measured curve by adjusting the graphitization ratio in the model, and the final graphitization degree is judged according to the fitting effect and the MSE value.
The method for measuring the hybrid type and the optical characteristic of the diamond substrate changing along with the temperature according to the embodiment includes the steps of firstly, measuring a spectrum curve under an initial condition by using an ellipsometer through establishing a temperature change system to be measured, then, heating the single crystal diamond substrate, measuring the ellipsometry spectrum curves under different temperatures, and finally, obtaining the components and the optical characteristic change of the substrate under different temperatures through fitting analysis, wherein the measurement precision is high, the temperature change range is wide, the refraction rate and the temperature change are sensitive, the change of the refraction rate can be reflected to the change of 0.01, and the change of the optical characteristic can be obtained and the hybrid type of the diamond substrate can be obtained. And selecting a built dispersion optical model according to whether the spectrum curve is an absorption region, wherein the dispersion optical model is a Cauchy model if the spectrum curve is a non-absorption region, the dispersion optical model is a Cauchy model if the spectrum curve is an absorption region, and the dispersion optical model is a Lorentz oscillator model, so that the measurement precision is high.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (7)
1. The measuring method of the diamond substrate changing with the temperature is characterized in that: the method comprises the following steps:
s1, measuring an ellipsometric spectrum curve (ψ, Δ) of the diamond substrate, which includes: s11, measuringEllipsometry spectrum curve (. psi.) of diamond substrate at room temperature0，Δ0) (ii) a S12, controlling the temperature of the heating system to heat the diamond substrate, and presetting the temperature of i heating systems and the temperature of the ith heating system as TiMeasuring each T in a sequence of temperature from low to highiEllipsometric spectrum (psi) of the underlying diamond substratei，Δi)；
S2, establishing a dispersion optical model to analyze the spectral curves, and respectively recording the spectral curves as ellipsometric spectral curves (psi)0，Δ0) Corresponding to (n)0，k0) And (psi)i，Δi) Corresponding to (n)i，ki) When the graphitization condition is satisfied, the optical constant (n) is recordedi，ki，di) N is a refractive index, k is an extinction coefficient, and d is a thickness of the diamond substrate;
s3, plotting optical constants (n) at all temperaturesi，ki，di) Analyzing the variation trend;
and S4, analyzing the change and proportion distribution condition of the diamond hybridization type by combining the established dispersion optical model after the graphitization condition is met.
2. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: in S1, the ellipsometry curve of the diamond substrate is measured by a measurement system, which is a broad spectrum ellipsometer whose spectral range covers ultraviolet, visible and near infrared.
3. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: the heating system in S1 satisfies the diamond graphitization condition, and the atmosphere of the heating gas is selected, and the heating gas is oxygen or nitrogen.
4. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: every two adjacent T in the S1iAre equal.
5. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: in S2, a dispersive optical model is selected according to whether the spectral curve is an absorption region, wherein:
if the dispersion optical model is a Cauchy model, the calculation formula is as follows:
in the formula, n is a refractive index, An, Bn and Cn are Cauchy model parameters, and lambda is a wavelength;
if the dispersion optical model is an absorption region, the dispersion optical model is a Lorentz oscillator model, and the calculation formula is as follows:
in the formula, A, En and Br are the amplitude, center position and half-wave width of the model parameter, respectively.
6. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: the graphitization conditions in S4 are set as required depending on the gas atmosphere and temperature.
7. The method for measuring a change with temperature of a diamond substrate according to claim 1, wherein: in the S4, the optical model can improve the fitting result by adjusting the volume fraction of the diamond hybridization type, namely the graphitized specific volume, and the final graphitized degree is obtained according to the fitting condition.
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2020
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| US20040265477A1 (en) * | 2001-09-06 | 2004-12-30 | Nataliya Nabatova-Gabain | Method for analyzing thin-film layer structure using spectroscopic ellipsometer |
| JP2008309843A (en) * | 2007-06-12 | 2008-12-25 | Toyota Central R&D Labs Inc | Optical element, method of manufacturing optical element, multilayered reflection film, optical waveguide device, diffraction grating, and optical recording medium |
| CN102954765A (en) * | 2011-08-12 | 2013-03-06 | 大塚电子株式会社 | Optical characteristic measuring apparatus and optical characteristic measuring method |
| CN109752321A (en) * | 2019-01-29 | 2019-05-14 | 华侨大学 | A kind of polishing silicon carbide substrates metamorphic layer thickness and the ellipse inclined detection method of optical constant |
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