阅读说明：本技术 原位测试金属燃烧敏感性特征的方法及系统 (Method and system for in-situ testing of metal combustion sensitivity characteristics ) 是由 张�诚 何康 黄进峰 王凤平 汪从珍 李志斌 于 2021-08-23 设计创作，主要内容包括：本申请涉及光谱检测技术领域,提供了一种原位测试金属燃烧敏感性特征的方法及系统,方法包括步骤：加热金属样品至燃烧；实时监测金属样品从加热至燃烧结束过程中的表面温度；采用短波长脉冲激光照射金属样品表面,产生拉曼信号；采集、处理金属样品从加热至燃烧结束过程中的拉曼信号,得到拉曼光谱；其中短波长脉冲激光的脉冲和拉曼信号的采集以时序同步的方式进行；分析金属样品的表面温度和拉曼光谱,获得在起燃瞬间的相变信息,从而得到金属燃烧敏感性特征。本申请提供的方法,可有效去除待测金属在高温状态下产生的黑体辐射信号对拉曼信号的影响,提高拉曼光谱分析的精度,准确获得起燃瞬间的拉曼信号,进而分析得到金属燃烧敏感性特征。(The application relates to the technical field of spectrum detection, and provides a method and a system for in-situ testing metal combustion sensitivity characteristics, wherein the method comprises the following steps: heating the metal sample to burn; monitoring the surface temperature of the metal sample from heating to the end of combustion in real time; irradiating the surface of a metal sample by adopting short-wavelength pulse laser to generate a Raman signal; collecting and processing Raman signals of the metal sample from heating to combustion ending to obtain a Raman spectrum; wherein, the pulse of the short wavelength pulse laser and the collection of the Raman signal are carried out in a time sequence synchronization mode; and analyzing the surface temperature and the Raman spectrum of the metal sample to obtain phase change information at the ignition moment so as to obtain the metal combustion sensitivity characteristic. The method provided by the application can effectively remove the influence of the blackbody radiation signal generated by the metal to be detected in a high-temperature state on the Raman signal, improve the accuracy of Raman spectrum analysis, accurately obtain the Raman signal at the moment of ignition, and further analyze the metal combustion sensitivity characteristic.)

1. A method for in situ testing of metal combustion sensitivity characteristics, comprising the steps of:

heating the metal sample to burn;

monitoring the surface temperature of the metal sample from heating to the end of combustion in real time;

irradiating the surface of the metal sample by adopting short-wavelength pulse laser to generate a Raman signal; collecting and processing the Raman signal of the metal sample from the heating to the combustion ending process to obtain a Raman spectrum; wherein, the pulse of the short-wavelength pulse laser and the collection of the Raman signal are carried out in a time sequence synchronous mode;

and analyzing the surface temperature of the metal sample from the heating to the combustion ending process and the Raman spectrum to obtain the phase change information of the metal sample at the ignition moment so as to obtain the metal combustion sensitivity characteristic.

2. The method of claim 1, wherein the metal sample comprises one or more of titanium, titanium alloy, iron alloy, nickel, and nickel alloy.

3. The method of claim 1, wherein the metal specimen is placed in a closed container; the gas in the closed container is pure oxygen, and the pressure is 0.09MPa-0.17 MPa.

4. The method of claim 1, wherein the heating comprises one or more of laser heating, flame heating, and electrical resistance heating.

5. The method of claim 1, wherein the maximum temperature of the heating is 700 ℃ to 2400 ℃; the heating rate is not lower than 200 ℃/min.

6. The method of claim 1, wherein the short wavelength pulsed laser has a pulse time of 500ns-1500 ns.

7. The method of claim 1, wherein the raman signal is acquired at a frequency of 5 ms/time to 100 ms/time.

8. The method of claim 1, further comprising the step of: and observing and recording the dynamic process of the metal sample from heating to combustion completion by using a camera device.

9. A system for in situ testing of metal combustion sensitivity characteristics, comprising:

the sample table is used for fixing a metal sample;

a high temperature heat source for heating the metal sample to combustion;

the temperature measuring device is used for monitoring the surface temperature of the metal sample in real time;

the short-wavelength pulse laser light source is used for emitting short-wavelength pulse laser and irradiating the surface of the metal sample to generate a Raman signal;

the Raman signal acquisition device is used for acquiring the Raman signal;

the Raman signal processing device is used for processing the acquired Raman signal to obtain a Raman spectrum, and the Raman spectrum and the surface temperature of the metal sample are used for obtaining metal combustion sensitivity characteristics; and

and the digital delay signal generator is used for carrying out time sequence synchronization on the pulse of the short-wavelength pulse laser and the acquisition of the Raman signal.

10. The system of claim 9, further comprising: and the camera device is used for observing and recording the dynamic process from heating to burning ending of the metal sample.

Technical Field

The application relates to the technical field of spectrum detection, in particular to a method and a system for in-situ testing of metal combustion sensitivity characteristics.

Background

The metal combustion often occurs in extreme conditions such as high temperature, high pressure, oxygen enrichment, high-speed impact and high-speed friction, and unlike general oxidation, the ignition moment is often accompanied by typical sudden change characteristics such as sudden temperature increase, size reduction and visible light generation, but at present, the essential mechanism of the metal ignition moment is still unclear, and the ignition mechanism is always the focus of research.

The current methods for studying metal combustion processes mainly utilize photoionization efficiency spectra, infrared spectra, raman spectra, and the like. Although the combustion process can be observed in situ and the mutation process of ionization energy can be reflected by utilizing the light ionization efficiency spectrum and the infrared spectrum, the structural change of substances cannot be reflected due to lower resolution; the raman spectrum is a fingerprint spectrum which can reflect the change of a material structure, but the raman spectrum under a high-temperature condition has poor analysis precision, cannot accurately obtain a raman signal at the moment of ignition, and further cannot analyze and obtain the metal combustion sensitivity characteristic.

Therefore, how to improve the accuracy of raman spectroscopy under high temperature conditions, accurately obtain a raman signal at the moment of ignition, and further analyze and obtain metal combustion sensitivity characteristics is an urgent problem to be solved.

Disclosure of Invention

The application aims to provide a method for testing metal combustion sensitivity characteristics in situ, so that the accuracy of Raman spectrum analysis under a high-temperature condition is effectively improved, a Raman signal at the moment of ignition is accurately obtained, and then the metal combustion sensitivity characteristics are obtained through analysis.

In a first aspect, the present application provides a method for in-situ testing of metal combustion sensitivity characteristics, comprising the steps of: heating the metal sample to burn; monitoring the surface temperature of the metal sample from heating to the end of combustion in real time; irradiating the surface of a metal sample by adopting short-wavelength pulse laser to generate a Raman signal; collecting and processing Raman signals of the metal sample from heating to combustion ending to obtain a Raman spectrum; wherein, the collection of the pulse of the short-wavelength pulse laser and the Raman signal is carried out in a time sequence synchronization mode; and analyzing the surface temperature and the Raman spectrum of the metal sample in the process from heating to combustion ending to obtain the phase change information of the metal sample at the ignition moment, thereby obtaining the metal combustion sensitivity characteristic.

In some embodiments, the metal sample comprises one or more of titanium, a titanium alloy, iron, an iron alloy, nickel, and a nickel alloy.

In some embodiments, the metal sample is placed in a closed container; the gas in the closed container is pure oxygen, and the pressure is 0.09MPa-0.17 MPa.

In some embodiments, the manner of heating includes one or more of laser heating, flame heating, and electrical resistance heating.

In some embodiments, the maximum temperature of heating is from 700 ℃ to 2400 ℃; the heating rate is not lower than 200 ℃/min.

In some embodiments, the short wavelength pulsed laser has a pulse time of 500ns-1500 ns.

In some embodiments, the acquisition frequency of the raman signal is between 5 ms/time and 100 ms/time.

In some embodiments, further comprising the step of: and observing and recording the dynamic process of the metal sample from heating to combustion completion by using a camera device.

A second aspect of the present application provides a system for in situ testing of metal combustion sensitivity characteristics, comprising: the sample table is used for fixing a metal sample; a high temperature heat source for heating the metal sample to combustion; the temperature measuring device is used for monitoring the surface temperature of the metal sample in real time; the short-wavelength pulse laser light source is used for emitting short-wavelength pulse laser and irradiating the surface of the metal sample to generate a Raman signal; the Raman signal acquisition device is used for acquiring Raman signals; the Raman signal processing device is used for processing the collected Raman signals to obtain a Raman spectrum, and the Raman spectrum and the surface temperature of the metal sample are used for obtaining the metal combustion sensitivity characteristic; and the digital delay signal generator is used for carrying out time sequence synchronization on the pulse of the short-wavelength pulse laser and the acquisition of the Raman signal.

In some embodiments, the device further comprises a camera device for observing and recording the dynamic process of the metal sample from heating to combustion ending.

According to the method for in-situ testing the metal combustion sensitivity characteristics, the digital delay signal generator is adopted for time sequence synchronization, namely, the short-wavelength pulse laser light source and the Raman signal acquisition device are respectively indicated to be started under different response times, and a computer is selected for receiving spectral data from the detector and analyzing the spectral data so as to obtain phase change information of a sample to be tested. Furthermore, the control module also comprises a time sequence controller which is connected with and adjusts the pulse laser and the detector so as to synchronize the pulse time sequence of the pulse laser with the shutter time sequence of the detector. The shutter time of the spectral line acquisition is limited to the nanosecond magnitude of the pulse laser width, so that the influence of a black body radiation signal generated by the metal sample to be detected in a high-temperature state on a Raman signal is effectively eliminated, the Raman spectrum analysis precision under the high-temperature condition is improved, the obtained Raman spectrum line information of the metal sample is more accurate and reliable, and the phase change characteristic of the metal sample in the process of temperature rise, ignition, violent combustion and combustion ending is obtained in real time. The temperature measuring device is adopted to monitor the temperature change of the metal sample in the heating-ignition-violent combustion process in real time, and the temperature curve of the whole process is obtained. Acquiring the ignition temperature of the metal sample combustion by capturing the temperature before the sudden change of the temperature curve; and obtaining the phase change information of the metal sample at the ignition moment by analyzing the mutation characteristic of the Raman spectrum line of the metal sample at the ignition temperature of the combustion so as to obtain the metal combustion sensitivity characteristic.

Of course, not all advantages described above need to be achieved at the same time in the practice of any one product or method of the present application.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and it is also obvious for a person skilled in the art to obtain other embodiments according to the drawings.

FIG. 1 is a schematic diagram of a system for in situ testing of metal combustion sensitivity characteristics provided herein;

FIG. 2a is a graph showing the temperature change of pure titanium in the heating-ignition-severe combustion process of a metal sample in example 1 of the present application;

FIG. 2b is a graph of an in-situ Raman spectrum of pure titanium of a metal sample in example 1 of the present application during a heat-light-off-hard combustion process;

FIG. 3a is a graph showing the temperature change of a titanium alloy TC4 in example 11 during heating-ignition-vigorous combustion;

FIG. 3b is a graph of an in situ Raman spectrum of a metal sample TC4 titanium alloy during heat-light-off-hard combustion in example 11 of the present application;

FIG. 4 is a graph showing the temperature change of pure titanium in a metal sample during heating-ignition-severe combustion under pure oxygen condition in example 14 of the present application;

FIG. 5 is a graph showing the temperature change of a metal sample TC17 titanium alloy during heating-ignition-vigorous combustion in pure oxygen condition according to example 15 of the present application;

FIG. 6a is a graph showing the temperature change of pure titanium of a metal sample in comparative example 1 of the present application during heating;

FIG. 6b is an in-situ Raman spectrum of pure titanium of a metal sample in comparative example 1 of the present application during heating;

FIG. 7a is a photograph of pure titanium of a metal sample at a temperature-raising stage in example 1 of the present application;

FIG. 7b is a photograph of a metal sample, pure titanium, taken before the moment of ignition, in example 1 of the present application;

FIG. 7c is a photograph of pure titanium of the metal sample at the moment of ignition in example 1 of the present application;

FIG. 7d is a photograph of a metal sample, pure titanium, taken during vigorous combustion as in example 1 of the present application;

fig. 8a to 8d are photographs of pure titanium of a metal sample in comparative example 1 of the present application taken during heating.

Detailed Description

The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the description herein are intended to be within the scope of the present disclosure.

In a first aspect, the present application provides a method for in-situ testing of metal combustion sensitivity characteristics, comprising the steps of:

(1) heating the metal sample to burn;

(2) monitoring the surface temperature of the metal sample from heating to the end of combustion in real time;

(3) irradiating the surface of a metal sample by adopting short-wavelength pulse laser to generate a Raman signal; collecting and processing Raman signals of the metal sample from heating to combustion ending to obtain a Raman spectrum; wherein, the collection of the pulse of the short-wavelength pulse laser and the Raman signal is carried out in a time sequence synchronization mode;

(4) and analyzing the surface temperature and the Raman spectrum of the metal sample in the process from heating to combustion ending to obtain the phase change information of the metal sample at the ignition moment, thereby obtaining the metal combustion sensitivity characteristic.

In the application, the step (1), the step (2) and the step (3) are not in sequence, when the metal sample starts to be heated, the surface temperature of the metal sample is monitored in real time, and the short-wavelength pulse laser light irradiates the surface of the metal sample to generate a Raman signal.

In the step (1), before the metal sample is heated, the metal sample needs to be fixed on a sample table, so that the sample is prevented from physically moving in the heating process; and the position irradiated by the short-wavelength pulse laser on the metal sample needs to be calibrated by adopting a temperature measuring device and a Raman signal acquisition device, so that the temperature measuring position of the temperature measuring device, the position irradiated by the short-wavelength pulse laser and the position acquired by the Raman signal are the same in the heating process, and the accuracy of the result is improved.

To obtain the combustion sensitivity characteristics of metals in air, the metal samples can be directly placed in air for testing, such as at a standard atmospheric pressure (0.1 MPa).

To obtain the metal combustion sensitivity characteristics in the pure oxygen state, the metal sample can be placed in a closed container, such as a closed chamber. Of course, in order to ensure that the short-wavelength pulse laser can irradiate the surface of the metal sample, the closed container is provided with an observation window. In order to obtain the metal combustion sensitivity characteristic in a pure oxygen state, the closed container needs to be filled with pure oxygen, and in some embodiments, the pressure of the filled pure oxygen is 0.09MPa to 0.17 MPa.

The physical form of the metal sample is not limited, and may be any form, such as a test piece or a test bar.

The material of the metal sample is not limited, and can be any metal material or a mixture of a plurality of metal materials, the surface oxide of which can generate Raman scattering; in some embodiments of the present application, the metal sample comprises one or more of titanium, titanium alloys, iron alloys, nickel, and nickel alloys.

The heating source is not limited, and may be any high-temperature heat source that burns metal, such as flame, high-temperature plasma torch, resistance wire, or a combination of a plurality of them. The heating method is not limited, and any heating method for burning the metal may be used, and in some embodiments of the present application, the heating method includes flame heating, laser heating, resistance heating, or a combination of a plurality of heating methods.

The maximum temperature for heating is not limited, and any temperature sufficient to cause combustion of the metal specimen may be used, and may be limited to a temperature slightly higher than the temperature at which combustion of the metal specimen occurs. In some embodiments herein, the maximum temperature of heating is from 700 ℃ to 2400 ℃, further from 1500 ℃ to 2400 ℃.

In some embodiments of the present application, the heating rate should be no less than 200 ℃/min, further 200 ℃/min to 800 ℃/min, and further 200 ℃/min to 500 ℃/min.

In step (2), the type of the adopted temperature measuring device is not limited, and the purpose of temperature measurement can be realized, for example, a double-colorimetric infrared thermometer can be adopted.

In the step (3), the types of the adopted raman signal acquisition device and the raman signal processing device are not limited as long as the purpose of the application can be achieved, that is, the raman signal acquisition device can acquire the raman signal, and the raman signal processing device can process the raman signal acquired by the raman signal acquisition device; for example, the raman signal acquisition device may be a raman probe. In some embodiments, the frequency of acquisition of the raman signal is from 5 ms/time to 100 ms/time, further from 20 ms/time to 100 ms/time, and further from 40 ms/time to 100 ms/time.

In the present application, acquiring and processing the raman signal to obtain the corresponding raman spectrum is a conventional method in the art, and the present application is not limited thereto as long as the purpose of the present application can be achieved.

In some embodiments of the present application, the short wavelength pulsed laser has a pulse time of 500ns to 1500ns, further 500ns to 1000 ns. The short-wavelength pulse laser is used as a laser light source, so that the Raman scattering signal intensity at high temperature can be improved.

And carrying out time sequence synchronization on the acquisition of the pulse of the short-wavelength pulse laser and the Raman signal, namely respectively indicating the short-wavelength pulse laser light source and the Raman signal acquisition device to be started under different response times, and selecting a computer to receive and analyze the spectral data from the detector so as to obtain the phase change information of the sample to be detected. Furthermore, the control module also comprises a time sequence controller which is connected with and adjusts the pulse laser and the detector so as to synchronize the pulse time sequence of the pulse laser with the shutter time sequence of the detector. The shutter time of the spectral line acquisition is limited to the nanosecond magnitude of the pulse laser width, so that the influence of a black body radiation signal generated by the metal sample to be detected in a high-temperature state on a Raman signal is effectively eliminated, the Raman spectrum analysis precision under the high-temperature condition is improved, the obtained Raman spectrum line information of the metal sample is more accurate and reliable, and the phase change characteristic of the metal sample in the process of temperature rise, ignition, violent combustion and combustion ending is obtained in real time.

The kind of the device used for timing synchronization is not limited as long as the purpose of the present application can be achieved, and for example, a digital delay signal generator may be used.

In order to observe and record the dynamic process from the heating to the combustion end of the metal sample, including the change of the size of the metal sample and the like, an image pickup device can be used for picking up an image of the metal sample from the heating to the combustion end. The observation window on the closed container can also be used for the camera device to take a picture. The type of the imaging device is not limited as long as the object of the present application can be achieved, and for example, a high-speed infrared imaging device may be used.

In the step (4), monitoring the temperature change of the metal sample in the heating-ignition-violent combustion process in real time through a temperature measuring device to obtain a temperature curve of the whole process, capturing the temperature before the curve mutation, and obtaining the ignition temperature of the metal sample combustion; the method comprises the steps of analyzing the mutation characteristics of Raman spectrum lines of a metal sample at the ignition temperature of combustion to obtain phase change information of the metal sample at the ignition moment, and further obtaining metal combustion sensitivity characteristics including temperature, size and phase change. The method provided by the application can obtain the mutation characteristics and the oxide evolution law of the combustion process of the metal sample, and provides powerful means support for more clearly researching the ignition mechanism of metal combustion.

In a second aspect, the present application provides a system for in situ testing of metal combustion sensitivity characteristics, a schematic diagram of which is shown in fig. 1, comprising: the sample table is used for fixing a metal sample; a high temperature heat source for heating the metal sample to combustion; the temperature measuring device is used for monitoring the surface temperature of the metal sample in real time; the short-wavelength pulse laser light source is used for emitting short-wavelength pulse laser and irradiating the surface of the metal sample to generate a Raman signal; the Raman signal acquisition device is used for acquiring Raman signals; the Raman signal processing device is used for processing the collected Raman signals to obtain a Raman spectrum, and the Raman spectrum and the surface temperature of the metal sample are used for obtaining the metal combustion sensitivity characteristic; and the digital delay signal generator is used for carrying out time sequence synchronization on the pulse of the short-wavelength pulse laser and the acquisition of the Raman signal.

The sample platform that this application adopted is for fixed metal sample, prevents that metal sample from taking place physical removal in the heating process.

To obtain the metal combustion sensitivity characteristics in the pure oxygen state, the metal sample can be placed in a closed container, such as a closed chamber. Of course, in order to ensure that the short-wavelength pulse laser can irradiate the surface of the metal sample, the closed container is provided with an observation window.

The high-temperature heat source is used for heating the metal sample until the metal sample is burnt. The type of the high-temperature heat source is not limited, and the high-temperature heat source can be any high-temperature heat source which can burn metal, such as flame, a high-temperature plasma torch, a resistance wire or a combination of a plurality of the high-temperature heat sources.

The temperature measuring device that this application adopted is the surface temperature for real-time supervision metal sample. The type of the temperature measuring device is not limited, and the purpose of temperature measurement of the application can be realized, for example, a double-colorimetric infrared thermometer can be adopted.

The short-wavelength pulse laser light source is used for emitting short-wavelength pulse laser; short-wavelength pulse laser light is irradiated on the surface of a metal sample, and a Raman signal can be generated.

The Raman signal acquisition device is used for acquiring Raman signals, and the Raman signal processing device is used for processing the Raman signals acquired by the Raman signal acquisition device. The types of the raman signal acquisition device and the raman signal processing device are not limited as long as the purpose of the present application can be achieved, and for example, the raman signal acquisition device may be a raman probe.

The digital delay signal generator can be used for carrying out time sequence synchronization on the pulse of the short-wavelength pulse laser and the collection of the Raman signal, namely respectively indicating that the short-wavelength pulse laser light source and the Raman signal collection device are started under different response times, and selecting a computer to receive spectral data from the detector and analyzing the spectral data so as to obtain the phase change information of the sample to be detected. Furthermore, the control module also comprises a time sequence controller which is connected with and adjusts the pulse laser and the detector so as to synchronize the pulse time sequence of the pulse laser with the shutter time sequence of the detector. The shutter time of the spectral line acquisition is limited to the nanosecond magnitude of the pulse laser width, so that the influence of a black body radiation signal generated by the metal sample to be detected in a high-temperature state on a Raman signal is effectively eliminated, the Raman spectrum analysis precision under the high-temperature condition is improved, the obtained Raman spectrum line information of the metal sample is more accurate and reliable, and the phase change characteristic of the metal sample in the process of temperature rise, ignition, violent combustion and combustion ending is obtained in real time.

In some embodiments of the present application, the device further comprises a camera device for observing and recording the dynamic process of the metal sample from heating to combustion ending, including the change of the size of the metal sample and the like. The observation window on the closed container can also be used for the camera device to take a picture. The type of the imaging device is not limited as long as the object of the present application can be achieved, and for example, a high-speed infrared imaging device may be used.

The present application will be described in detail below with reference to specific examples and comparative examples.

Example 1

The system adopted comprises: the device comprises a sample table, a high-temperature plasma spray gun, a double-colorimetric infrared thermometer, a short-wavelength pulse laser light source, a Raman probe, a Raman signal processing device, a digital delay signal generator and a high-speed infrared photographic device.

The method for testing the metal combustion sensitivity characteristic in situ comprises the following steps.

Fixing pure titanium of a metal sample on a sample table, and placing the sample table in air with the pressure of 0.10 MPa. And a short-wavelength pulse laser light source is used for emitting short-wavelength pulse laser and irradiating the short-wavelength pulse laser on the surface of the metal sample, and a double colorimetric infrared thermometer and a Raman probe are used for calibrating a pure titanium part of the metal sample, so that the temperature measuring position of the double colorimetric infrared thermometer, the position irradiated by the short-wavelength pulse laser and the position acquired by a Raman signal are the same in the heating process. And (3) providing an ultrahigh temperature environment by adopting a high-temperature plasma torch, setting the heating maximum temperature to be 2400 ℃, and setting the heating rate to be 200 ℃/min until the pure titanium of the metal sample is ignited.

And in the process from heating to combustion ending, monitoring the surface temperature of the pure titanium of the metal sample in real time by using a double-colorimetric infrared thermometer.

In the process from heating to combustion ending, a Raman signal is generated on the surface of the pure titanium of the metal sample by adopting short-wavelength pulse laser irradiation, and the pulse time is 500 ns; collecting Raman signals by a Raman probe, wherein the collection frequency is 40 ms/time, and processing the collected Raman signals by a Raman signal processing device to obtain a Raman spectrum; wherein, a digital delay signal generator is adopted to carry out time sequence synchronization on the acquisition of the pulse of the short-wavelength pulse laser and the Raman signal.

And in the process from heating to combustion ending, observing and recording the dynamic process of the pure titanium of the metal sample from heating to combustion ending by adopting a high-speed infrared photographic device, wherein the dynamic process comprises the change situation of the size of the pure titanium of the metal sample.

Monitoring the surface temperature change of the pure titanium of the metal sample in the heating-ignition-violent combustion process in real time through a temperature measuring device to obtain a temperature curve of the whole process, capturing the temperature before the curve mutation, and obtaining the ignition temperature of the pure titanium combustion of the metal sample; the method comprises the steps of analyzing the mutation characteristics of a Raman spectrum line of the metal sample pure titanium at the ignition temperature of the combustion of the metal sample to obtain phase change information of the metal sample pure titanium at the ignition moment, and further obtaining the combustion sensitivity characteristics of the metal pure titanium, including temperature, size and phase change.

Examples 2 to 15

Referring to the apparatus and method of example 1, the metal combustion sensitivity characteristics were tested in situ using the metal samples, gas type, pressure, heating regime, maximum temperature of heating, heating rate, pulse time and spectral frequency test conditions in Table 1. Wherein, the metal samples of the embodiments 13-15 are placed in a closed cabin with an observation window, and pure oxygen of 0.09MPa, 0.17MPa and 0.17MPa is respectively filled after the vacuum pumping is finished, so that the metal samples are combusted under the condition of the pure oxygen; the metal samples of the other examples were placed in air at a pressure of 0.10MPa for combustion.

Comparative example 1

Referring to the apparatus and method of example 1, the metal combustion sensitivity characteristics were tested in situ using the metal samples, gas species, pressure, heating regime, maximum temperature of heating, heating rate, pulse time and spectral frequency test conditions of comparative example 1 of Table 1. The metal sample of comparative example 1 was placed in air at a pressure of 0.10MPa for combustion.

TABLE 1 test conditions

As a result: in example 1, (1) temperature: the temperature change curve of the pure titanium of the metal sample in the heating-ignition-violent combustion process is shown in figure 2a, and it can be obtained from figure 2a that the pure titanium of the metal sample has a temperature mutation phenomenon in the ignition process, the temperature of the mutation starting point is 1497.59 ℃, and the temperature is defined as the ignition temperature of the pure titanium; (2) phase change: the in-situ Raman spectrum of pure titanium in the heating-ignition-violent combustion process is shown in FIG. 2b, and it can be seen from FIG. 2b that in the temperature-raising stage, the oxide is mainly rutile TiO₂And Ti₂O₃In the light-off phase, metastable Ti newly appears₃O₅Characteristic peak of (A) indicating that TiO occurred at the moment of light-off₂、Ti₂O₃To Ti₃O₅Phase transition of (2).

In example 11, (1) temperature: the temperature change curve of the metal sample TC4 titanium alloy in the heating-ignition-violent combustion process is shown in FIG. 3a, and it can be obtained from FIG. 3a that the metal sample TC4 titanium alloy has a temperature jump phenomenon in the ignition process, the temperature of the jump starting point is 1322.06 ℃, and is defined as the ignition temperature of the TC4 titanium alloy; (2) phase change: metal sample TC4 titanium alloy heating-igniting-heatingThe in-situ Raman spectrum during the hard burn is shown in FIG. 3b, and it can be seen from FIG. 3b that during the ramp-up phase, the oxide is mainly rutile TiO₂And Ti₂O₃，V₂O₅(ii) a In the light-off phase, metastable Ti newly appears₃O₅Characteristic peak of (A) indicating that TiO occurred at the moment of light-off₂、Ti₂O₃To Ti₃O₅Phase transition of (2).

In example 14, temperature: the temperature change curve of the pure titanium of the metal sample in the heating-ignition-violent combustion process under the pure oxygen condition is shown in fig. 4, and it can be obtained from fig. 4 that the pure titanium of the metal sample has a temperature mutation phenomenon in the ignition process, the temperature at the starting point of the mutation is 873.41 ℃, and the temperature is defined as the ignition temperature of the pure titanium.

In example 15, temperature: the temperature change curve of the metal sample TC17 titanium alloy in the heating-ignition-violent combustion process under the pure oxygen condition is shown in FIG. 5, and it can be obtained from FIG. 5 that the metal sample TC17 titanium alloy has a temperature jump phenomenon in the ignition process, the temperature of the jump starting point is 855.82 ℃, and the jump starting point is defined as the ignition temperature of pure titanium.

In comparative example 1, (1) temperature: the temperature change curve of the pure titanium of the metal sample in the heating process is shown in fig. 6a, and it can be found from fig. 6a that the temperature does not change, which indicates that the pure titanium of the metal sample does not burn; (2) phase change: the in-situ raman spectrum of pure titanium in the metal sample during heating is shown in fig. 6b, and it can be seen from fig. 6b that the in-situ raman spectrum of each stage has no obvious change.

The light-off temperature and the change in light-off transient oxide of each of the metal samples of examples 1 to 15 of the present application and comparative example 1 are shown in Table 2 below. Wherein, TiO₂(A) Expressed as (Anatase) Anatase TiO₂，TiO₂(R) is (Rutile) Rutile type TiO₂。

TABLE 2 light-off temperature and light-off transient oxide Change for each of the metal samples

Note: in the parentheses, A represents anatase, and R represents rutile

Fig. 7a, 7b, 7c and 7d show photographs of pure titanium of a metal sample in a combustion process in example 1 of the present application, where fig. 7a is a photograph of pure titanium of the metal sample at a temperature rise stage, fig. 7b is a photograph of pure titanium of the metal sample before a light-off moment, fig. 7c is a photograph of pure titanium of the metal sample at the light-off moment, and fig. 7d is a photograph of pure titanium of the metal sample during a violent combustion. From fig. 7a to 7d, it can be seen that the size of the pure titanium of the metal sample before combustion has not changed significantly, and the size of the pure titanium of the metal sample gradually decreases during the combustion process until the pure titanium is burnt out.

The photographs of the pure titanium of the metal sample in the comparative example 1 of the present application taken during the heating process are shown in fig. 8a to 8d, and the photographs taken during the gradual heating process are sequentially shown from left to right in fig. 8a to 8 d. As can be seen from fig. 8a to 8d, pure titanium of the metal sample did not burn, and the sample size did not change significantly.

As can be seen from the above examples, the light-off temperature at which the metal sample was burned can be obtained by capturing the temperature before the sudden change in the temperature curve; the mutation oxide of the metal sample at the ignition moment can be obtained by analyzing the mutation characteristics of the Raman spectrum line of the metal sample at the ignition temperature of the combustion.

All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments.

The above description is only for the preferred embodiment of the present application and is not intended to limit the scope of the present application. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application are included in the protection scope of the present application.