CN111693561B - Method and system for measuring ignition point of nano material - Google Patents
Method and system for measuring ignition point of nano material Download PDFInfo
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- CN111693561B CN111693561B CN202010471013.2A CN202010471013A CN111693561B CN 111693561 B CN111693561 B CN 111693561B CN 202010471013 A CN202010471013 A CN 202010471013A CN 111693561 B CN111693561 B CN 111693561B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20075—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring interferences of X-rays, e.g. Borrmann effect
Abstract
The invention relates to a method and a system for measuring the ignition point of a nano material, wherein the measuring method comprises the following steps: 1) Measuring the complex reflectivity ratio rho of P light and S light of the nano material at different temperatures under single wavelength and single angle by using a variable temperature elliptical polarization spectrometer, and further obtaining two elliptical polarization parameters psi and delta; 2) Obtaining a variation spectrum of the ellipsometry parameters psi and delta with the temperature based on the step 1); 3) Determining a phase change point of the nanomaterial based on the mutation point on the change spectrum; 4) And judging whether the phase change point is an ignition point or not according to the change condition of the substances before and after each phase change point, thereby measuring and obtaining the final ignition point of the nano material. Compared with the prior art, the invention has the advantages of no contact, high speed, high reliability and the like.
Description
Technical Field
The invention relates to the technical field of thermal measurement, in particular to a method and a system for measuring the ignition point of a nano material.
Background
Under the influence of quantum size limitation effect, materials with nano-scale size exhibit different optical, magnetic, electrical, thermal and catalytic properties from bulk materials, and are widely focused and researched in different research fields such as physics, chemistry, biology, materials and the like. The ignition point of the nano material is obviously reduced compared with that of the block material, and the nano material is favorable for saving energy and reducing environmental pollution when used as fuel; and the nanometer metal dust is easy to ignite and explode in the air, thereby bringing great potential safety hazard to the life of people. Therefore, the research on the ignition point of the nano material has important significance.
The current reports on the ignition point of the nano material are relatively limited. Theoretically, researchers have built a series of models to estimate the ignition point of nanomaterials. Experimentally, there are two main methods for studying the ignition point of the nanomaterial:
one method is to adopt a thermogravimetric analysis method to judge the ignition point according to the strong heat release effect and the sudden increase of the quality of the material to be measured, and the method needs to contact with a sample in the measurement, so that the appearance and the structure of the sample are damaged, and the test result is influenced;
the other method is to utilize a high-speed camera to monitor the combustion process of the nano material in real time, and the temperature at which combustion occurs first is determined as the ignition point.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a non-contact and non-destructive method and a non-contact and non-destructive system for measuring the ignition point of a nano material, so that the ignition point of the nano material can be quickly obtained with high precision and high sensitivity.
The purpose of the invention can be realized by the following technical scheme:
a method for measuring the ignition point of a nano material comprises the following steps:
1) Measuring the complex reflectivity ratio rho of P light and S light of the nano material at different temperatures under single wavelength and single angle by using a variable temperature elliptical polarization spectrometer:
ρ＝r p /r s ＝tanψe iΔ
wherein r is p Is the complex reflectivity of P light, r s Obtaining two ellipsometry parameters psi and delta for the complex reflectivity of the S light;
2) Obtaining a variation spectrum of the ellipsometry parameters psi and delta along with the temperature based on the step 1);
3) Determining a phase change point of the nanomaterial based on the mutation point on the change spectrum;
4) And judging whether the phase change point is an ignition point according to the change condition of the substances before and after each phase change point, thereby measuring and obtaining the final ignition point of the nano material.
Further, the wavelength in step 1) is a wavelength at which the change of the ellipsometric parameter with temperature is significant and the measurement error is small.
Further, the wavelength is selected within the range of 200-1000 nm.
Further, in the step 1), the temperature interval of different temperatures is 0.5-2 ℃.
Further, in the step 4), the change of the substance before and after the phase change point is measured by using an X-ray diffractometer.
Further, in the step 4), the X-ray diffraction patterns of the nano material at normal temperature and after the phase change are respectively tested.
Further, the ellipsometry parameter ranges are: 0 ° < ψ <90 °, -180 ° < Δ <0 °.
The invention also provides a system for measuring the ignition point of the nano material, which comprises a variable-temperature elliptical polarization spectrometer, an X-ray diffractometer and an upper computer, wherein a computer program is stored in the upper computer, and the operation executed by the computer program comprises the following steps:
collecting optical measurement results of optical measurement tests of the variable-temperature elliptical polarization spectrometer under single wavelength, single angle and different temperatures;
obtaining the complex reflectivity ratio rho of P light and S light of the nano material at different temperatures based on the optical measurement result:
ρ＝r p /r s ＝tanψe iΔ
wherein r is p Is the complex reflectivity of P light, r s Obtaining two ellipsometry parameters psi and delta for the complex reflectivity of the S light;
obtaining the variation spectrums of the ellipsometric parameters psi and delta along with the temperature;
determining a phase change point of the nanomaterial based on the mutation point on the change spectrum;
and obtaining the change condition of the substances before and after each phase change point, which is measured by an X-ray diffractometer, and judging whether the phase change point is an ignition point or not, thereby measuring and obtaining the final ignition point of the nano material.
The variable-temperature elliptical polarization spectrometer comprises a light source, a fixed polarizer, a rotating polarizer, a temperature control sample stage, a rotating polarization analyzer and a detector, wherein a sample is placed on the temperature control sample stage, light emitted by the light source sequentially passes through the fixed polarizer and the rotating polarizer and then is changed into linear polarization light to be incident on the sample, the linear polarization light is reflected by the sample, then passes through the rotating polarization analyzer and then is incident on the detector to complete signal detection, and the temperature control of the sample is realized through the temperature control sample stage in the measurement process.
Further, the temperature control sample stage comprises a temperature controller, a k-type thermocouple, a sample stage, a thermal resistor, a relay and a direct current power supply, the temperature controller, the k-type thermocouple, the sample stage, the thermal resistor and the relay are sequentially connected to form a loop, the direct current power supply is connected with the relay, the thermal resistor heats the sample stage, the temperature of the sample stage is measured by the k-type thermocouple and fed back to the temperature controller in real time, and the temperature controller controls the on-off of the relay, so that the temperature of the sample stage is controlled.
Further, the computer program performs operations further comprising:
and respectively testing the X-ray diffraction patterns of the nano material at normal temperature and after phase change.
Compared with the prior art, the invention has the following beneficial effects:
1. the temperature-changing ellipsometry measures the optical property of a sample accurately by measuring the change of the front and back polarization states of polarized light passing through the surface of the sample, and is a non-contact and non-destructive method which can realize measurement with high precision and high sensitivity and can realize measurement quickly. The change of the combustion optical property of the material is reflected through the change of the ellipsometric parameter, the property of a sample to be measured does not need to be fully known, the simulation analysis and data fitting of a complex film system are not needed, and the phase change point can be directly obtained from the change curve of the ellipsometric parameter along with the temperature. The invention can quickly and accurately obtain the phase change point based on the variable-temperature ellipsometry, and quickly determine the phase change point as the ignition point according to the change of the substances before and after the phase change point. The measuring method is simple and visual, has smaller measuring error, and can meet the requirement of real-time in-situ measurement and analysis.
2. The invention utilizes the X-ray diffractometer to measure the change of the substances before and after the phase change point, and has high accuracy.
3. The invention adopts optical means, can measure the ignition point of the nano material in a high-precision, rapid, non-contact and non-destructive manner, and has potential application prospect in a plurality of fields such as physics, chemistry, environmental science, material science, nanotechnology and the like.
Drawings
FIG. 1 is a schematic flow chart of a measurement method according to the present invention;
FIG. 2 is a schematic diagram of the operating principle of the variable temperature elliptical polarization spectrometer of the present invention;
FIG. 3 is a graph showing the change of the ellipsometric parameters psi and delta of the nano indium particle thin film with temperature in the example;
fig. 4 is an X-ray diffraction spectrum of the nano indium particle thin film in the embodiment, wherein a) is an X-ray diffraction spectrum at room temperature, and b) is an X-ray diffraction spectrum after an ellipsometry temperature change experiment at 260 ℃;
reference numbers in the figures: 1-light source, 2-fixed polarizer, 3-rotating polarizer, 4-sample, 5-rotating analyzer, 6-detector, 7-temperature controller, 8-k type thermocouple, 9-sample stage, 10-thermal resistor, 11-relay, 12-DC power supply.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
As shown in fig. 1, the present invention provides a method for measuring the ignition point of a nanomaterial, comprising the following steps:
s01, measuring the complex reflectivity ratio rho of P light and S light of the nano material at different temperatures under single wavelength and single angle by using a variable temperature elliptical polarization spectrometer:
ρ＝r p /r s ＝tanψe iΔ
wherein r is p Is the complex reflectivity of P light, r s Two ellipsometric parameters psi and delta are obtained for the complex reflectivity of the S-light.
When the variable-temperature elliptical polarization spectrometer is used for an optical measurement test, the detection wavelength is selected within the range of 200-1000 nm, the requirement of the band on the detection environment is not strict, the requirement of an ultraviolet band on the vacuum measurement environment can be avoided, and the influence of the humidity of an infrared band on the detection is also avoided. The detection temperature interval should be selected to be smaller in the range of 0.5-2 ℃, which can make the detection phenomenon more obvious. The ellipsometry parameter ranges are: 0 ° < ψ <90 °, -180 ° < Δ <0 °.
And S02, obtaining a variation spectrum of the ellipsometric parameters psi and delta with the temperature based on the step S01.
And S03, determining the phase change point of the nano material based on the catastrophe point on the change spectrum.
And S04, measuring the change of the substances before and after the phase change point by adopting an X-ray diffractometer, and judging whether the phase change point is an ignition point according to the change condition of the substances before and after each phase change point, thereby measuring and obtaining the final ignition point of the nano material. In the step, X-ray diffraction patterns of the nano material at normal temperature and after phase change are respectively tested.
The data processing process in the method can be realized by an upper computer.
As shown in fig. 2, the variable-temperature elliptical polarization spectrometer adopted in the method comprises a light source 1, a fixed polarizer 2, a rotating polarizer 3, a temperature-controlled sample stage, a rotating analyzer 5 and a detector 6, wherein the temperature-controlled sample stage comprises a temperature controller 7, a k-type thermocouple 8, a sample stage 9, a thermal resistor 10, a relay 11 and a direct-current power supply 12, the temperature controller 7, the k-type thermocouple 8, the sample stage 9, the thermal resistor 10 and the relay 11 are sequentially connected to form a loop, and the direct-current power supply 12 is connected with the relay 11.
When an optical measurement test is carried out, a sample 4 is placed on a temperature control sample table, light emitted by a light source 1 sequentially passes through a fixed polarizer 2 and a rotating polarizer 3 and then becomes linear polarized light to be incident on the sample 4, the light interacts with a substance, the light is reflected by the sample 4, then passes through a rotating analyzer 5 and then is incident on a detector 6 to complete signal detection. The temperature control of the sample is realized through a temperature control sample table in the measuring process: the thermal resistor 10 heats the sample platform 9, the k-type thermocouple 8 measures the temperature of the sample platform 9 and feeds the temperature to the temperature controller 7 in real time, and the temperature controller 7 controls the on-off of the relay 11, so that the temperature of the sample platform is controlled.
The microscopic mechanism of interaction between light and a substance is the interaction between light and free electrons, bound electrons, excitons, atoms, ions, molecules, impurities, defects, and the like in the material, and is closely related to the state, band structure, and various excited states of microscopic particles. When a beam of polarized light of a known polarization state is incident on the surface of the sample, the light interacts with the substance, causing a change in the polarization state of the light reflected by the sample, which is related to the internal structure of the sample. According to the change of the polarization state, the structural information of the sample can be obtained through the measured ellipsometric parameters. The combustible material can generate chemical phase change after being burnt to generate a new material which is completely different from the original material in properties, and a mutation point appears on an ellipsometry parameter change curve along with the temperature through temperature change ellipsometry. By using the principle, the phase change point of the nano material can be determined by observing the mutation point on the curve of the ellipsometric parameter changing along with the temperature. And measuring the change of the material before and after the phase change point by an X-ray diffractometer, and finally determining the phase change point as the ignition point.
In X-ray diffraction, X-rays are projected as incident electromagnetic waves into a crystal, and the X-rays incident into the crystal are coherently scattered by atoms therein. Because atoms are periodically arranged in the crystal, the coherent scattered waves have a fixed phase relationship, which causes waves in certain scattering directions to mutually reinforce and mutually cancel in certain directions, so that diffraction phenomenon occurs. The atomic arrangement inside each crystal is specific, and the corresponding diffraction pattern is also specific, so that phase analysis can be performed.
Examples
This example describes embodiments of the present invention by measuring the ignition point of a nano-indium particle thin film.
Preparing an indium particle film with the particle size of about 43.2nm and the thickness of 44nm on a silicon substrate by adopting an electron beam evaporation method.
The indium particle thin film is measured by using a variable temperature ellipsometer, wherein the selected detection wavelength is 500nm, the detection angle is 70 degrees, the detection temperature range is 210-270 ℃, the temperature interval is 1 ℃, and ellipsometry parameters at different temperatures are obtained, as shown in fig. 3.
As can be seen from fig. 3, the changes of the two ellipsometric parameters ψ, Δ around 251 ℃ are slowly continuous, while a sharp mutation occurs at the same time around 251 ℃, indicating that a phase transition occurs at 251 ℃.
As can be seen from the X-ray diffraction spectrum of fig. 4, the nano indium particle thin film crystallized well at normal temperature and was preferentially oriented in the (101) direction. After the measurement of ellipsometric temperature at 260 ℃, the indium grown in the (101) direction is completely changed into the indium oxide preferentially grown in the (222) direction, which shows that the phase change occurring near 251 ℃ is a chemical phase change generated by a violent oxidation reaction. The burning of the indium particle film enables indium to be rapidly and completely changed into indium oxide, which causes severe mutation of an ellipsometric parameter, so that the burning point of the obtained nano indium particle film is 251 ℃.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A method for measuring the ignition point of a nano material is characterized in that the method is applied to a scene that combustible substances generate chemical phase change after being combusted, and comprises the following steps:
1) Measuring the complex reflectivity ratio of P light and S light of the nano material at different temperatures under single wavelength and single angle by using a variable-temperature elliptical polarization spectrometerρ：
ρ=r p /r s =tanψe iΔ
Wherein the content of the first and second substances,r p in order to obtain the complex reflectivity of the P-ray,r s is the complex reflectivity of S light, and then two ellipsometry parameters are obtainedψAnd Δ;
2) Obtaining ellipsometry parameters based on step 1)ψ、ΔA spectrum of changes with temperature;
3) Determining a phase change point of the nano material based on the mutation point on the change spectrum;
4) And judging whether the phase change point is an ignition point according to the change condition of the substances before and after each phase change point, thereby measuring and obtaining the final ignition point of the nano material.
2. The method for measuring the ignition point of the nanomaterial according to claim 1, wherein the wavelength in the step 1) is a wavelength at which the change of the ellipsometric parameters with the temperature is significant and the measurement error is small.
3. The method for measuring the ignition point of the nanomaterial according to claim 1, wherein in the step 1), the temperature interval of different temperatures is 0.5 to 2 ℃.
4. The method for measuring the ignition point of the nanomaterial according to claim 1, wherein in the step 4), an X-ray diffractometer is used to measure the change of the substance before and after the phase change point.
5. The method for measuring the ignition point of the nano material according to claim 1, wherein in the step 4), the X-ray diffraction patterns of the nano material at normal temperature and after the phase transition are respectively tested.
6. The method of claim 1, wherein the ellipsometric parameter ranges are: 0 ° < ψ <90 °, -180 ° < Δ <0 °.
7. The system is characterized in that the system is applied to scenes that combustible substances generate chemical phase change after being combusted, and comprises a temperature-changing elliptical polarization spectrometer, an X-ray diffractometer and an upper computer, wherein a computer program is stored in the upper computer, and the operation executed by the computer program comprises the following steps:
collecting optical measurement results of optical measurement tests of the variable-temperature elliptical polarization spectrometer under single wavelength, single angle and different temperatures;
obtaining the complex reflectivity ratio of P light and S light of the nano material at different temperatures based on the optical measurement resultρ：
ρ=r p /r s =tanψe iΔ
Wherein the content of the first and second substances,r p in order to obtain the complex reflectivity of the P-ray,r s is the complex reflectivity of S light, and then two ellipsometry parameters are obtainedψAnd Δ;
obtaining ellipsometric parametersψ、ΔA spectrum of changes with temperature;
determining a phase change point of the nanomaterial based on the mutation point on the change spectrum;
and obtaining the change condition of the substances before and after each phase change point, which is measured by an X-ray diffractometer, and judging whether the phase change point is an ignition point or not, thereby measuring and obtaining the final ignition point of the nano material.
8. The nanomaterial ignition point measuring system of claim 7, wherein the temperature-variable elliptical polarization spectrometer comprises a light source, a fixed polarizer, a rotating polarizer, a temperature-controlled sample stage, a rotating analyzer and a detector, wherein a sample is placed on the temperature-controlled sample stage, light emitted by the light source passes through the fixed polarizer and the rotating polarizer in sequence, is changed into linearly polarized light and is incident on the sample, the light is reflected by the sample, passes through the rotating analyzer and then is incident on the detector to complete signal detection, and the temperature control of the sample is realized through the temperature-controlled sample stage in the measuring process.
9. The nanomaterial ignition point measuring system of claim 8, wherein the temperature-controlled sample stage comprises a temperature controller, a k-type thermocouple, a sample stage, a thermal resistor, a relay and a direct current power supply, the temperature controller, the k-type thermocouple, the sample stage, the thermal resistor and the relay are sequentially connected to form a loop, the direct current power supply is connected with the relay, the thermal resistor heats the sample stage, the k-type thermocouple measures the temperature of the sample stage and feeds the temperature back to the temperature controller in real time, and the temperature controller controls the on-off of the relay, so that the temperature of the sample stage is controlled.
10. The nanomaterial ignition point measurement system of claim 7, wherein the computer program performs operations further comprising:
and respectively testing the X-ray diffraction patterns of the nano material at normal temperature and after phase change.
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| CN103175785A (en) * | 2013-03-12 | 2013-06-26 | 复旦大学 | Ellipsometer-based measurement method of melting point of nanometer material |
| CN103234914A (en) * | 2013-04-18 | 2013-08-07 | 复旦大学 | Ferroelectric material Curie point measuring method based on ellipsometer |
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| US6052188A (en) * | 1998-07-08 | 2000-04-18 | Verity Instruments, Inc. | Spectroscopic ellipsometer |
| CN103175785A (en) * | 2013-03-12 | 2013-06-26 | 复旦大学 | Ellipsometer-based measurement method of melting point of nanometer material |
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