CN109142227B - Sample cavity for spectrum experiment - Google Patents
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- CN109142227B CN109142227B CN201811084091.6A CN201811084091A CN109142227B CN 109142227 B CN109142227 B CN 109142227B CN 201811084091 A CN201811084091 A CN 201811084091A CN 109142227 B CN109142227 B CN 109142227B
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- 238000002474 experimental method Methods 0.000 title claims abstract description 21
- 238000001228 spectrum Methods 0.000 title abstract description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 51
- 239000004917 carbon fiber Substances 0.000 claims abstract description 51
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000006073 displacement reaction Methods 0.000 claims abstract description 15
- 239000006096 absorbing agent Substances 0.000 claims description 40
- 239000007789 gas Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 18
- 230000005855 radiation Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003990 capacitor Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 thermal sensor Substances 0.000 description 1
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
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Abstract
本发明涉及物理实验领域，一种用于光谱实验的样品腔，包括进气管、上盖、毛细管、连接管、出气管、样品管、下盖、样品、碳纤维管、加热灯、热屏蔽腔、辐射热计、温度计、导热基座、水冷台和位移装置，在进行光谱实验时需要与储气罐、光源及光谱仪一起使用，采用的样品管结构紧凑，样品准备过程简单，可靠性高，采用简单的结构通过气流来控制样品温度，通过加热灯的辐射热对样品均匀加热，结合气流能够精确控制样品温度，并采用特殊设计的辐射热计准确测量入射光的辐射功率，精度较高，整个装置的发热量小，对周围实验环境影响小。
The invention relates to the field of physical experiments, and is a sample cavity used for spectrum experiments, including an air inlet pipe, an upper cover, a capillary tube, a connecting pipe, an air outlet pipe, a sample tube, a lower cover, a sample, a carbon fiber tube, a heating lamp, and a heat shielding cavity. The bolometer, thermometer, thermal base, water-cooling stage and displacement device need to be used together with the gas tank, light source and spectrometer when performing spectroscopic experiments. The sample tube used has a compact structure, a simple sample preparation process and high reliability. It is used The simple structure controls the sample temperature through air flow. The sample is evenly heated by the radiant heat of the heating lamp. Combined with the air flow, the sample temperature can be accurately controlled. A specially designed bolometer is used to accurately measure the radiant power of the incident light with high accuracy. The device generates little heat and has little impact on the surrounding experimental environment.
Description
技术领域Technical field
本发明涉及物理实验领域，尤其是一种可靠性高且样品准备过程简单的一种用于光谱实验的样品腔。The invention relates to the field of physical experiments, in particular to a sample cavity for spectroscopic experiments with high reliability and simple sample preparation process.
背景技术Background technique
光谱实验如吸收光谱、激发光谱、衍射实验等是研究物质特性的常用实验手段，通常是将不同波长的光入射到样品上，并探测反射的光。通常样品放置在特殊的样品腔中，对于不同的样品及不同的实验要求，样品腔的结构不同。现有技术缺陷一：在某些需要对样品加热的实验中，某些现有技术通过陶瓷或金属元件加热、微波共振等方法来加热样品，测温器件通常位于样品附近位置，由于热源距离样品较近，会受到热源的辐射热的影响而较难测准样品温度，而另一些现有技术中，样品位于一个加热腔内，测温器件能够与周围环境达到热平衡，能够较准确地测量样品温度，但是加热腔的尺寸较大，某些对样品周围空间尺寸要求较高的实验无法进行；现有技术缺陷二：在某些光谱实验中需要精确测量入射光的功率，而受限于样品腔的结构及温度等因素，入射光功率的测量精度不高，所述一种用于光谱实验的样品腔能够解决问题。Spectral experiments such as absorption spectrum, excitation spectrum, diffraction experiment, etc. are commonly used experimental methods to study the properties of materials. Usually, light of different wavelengths is incident on the sample and the reflected light is detected. Usually the sample is placed in a special sample chamber. For different samples and different experimental requirements, the structure of the sample chamber is different. Defect 1 of the existing technology: In some experiments that require heating of the sample, some existing technologies heat the sample through ceramic or metal element heating, microwave resonance, etc. The temperature measuring device is usually located near the sample. Since the heat source is far away from the sample Recently, it will be affected by the radiant heat of the heat source and it is difficult to accurately measure the sample temperature. In other existing technologies, the sample is located in a heating chamber, and the temperature measurement device can achieve thermal equilibrium with the surrounding environment, and can measure the sample more accurately. temperature, but the size of the heating cavity is large, and some experiments that require high space dimensions around the sample cannot be carried out; flaw 2 of the existing technology: in some spectroscopic experiments, the power of the incident light needs to be accurately measured, which is limited by the sample Due to factors such as the structure and temperature of the cavity, the measurement accuracy of the incident light power is not high. The above-mentioned sample cavity for spectroscopic experiments can solve the problem.
发明内容Contents of the invention
为了解决上述问题，本发明装置采用简单的结构通过气流来控制样品温度，能够精确测量样品温度，并能够精确测量入射光的辐射功率，另外，整个装置的发热量小，对周围实验环境影响小。本发明装置为光谱实验的样品腔，在进行光谱实验时需要与储气罐、光源及光谱仪一起使用。In order to solve the above problems, the device of the present invention uses a simple structure to control the sample temperature through air flow, can accurately measure the sample temperature, and can accurately measure the radiant power of incident light. In addition, the entire device generates little heat and has little impact on the surrounding experimental environment. . The device of the invention is a sample cavity for spectrum experiments, and needs to be used together with a gas storage tank, a light source and a spectrometer when conducting spectrum experiments.
本发明所采用的技术方案是：The technical solution adopted by the present invention is:
所述一种用于光谱实验的样品腔主要包括进气管、上盖、毛细管、连接管、出气管、样品管、下盖、样品、碳纤维管、加热灯、热屏蔽腔、辐射热计、辐射热计控制电路、温度计、导热基座、水冷台和位移装置，xyz为三维空间坐标系，进气管连接储气罐，储气罐中储存有氩气，并能够调节氩气的流速；实验设施有真空腔、储气罐、光源和光谱仪，所述碳纤维管、加热灯、热屏蔽腔、辐射热计、温度计、导热基座、水冷台和位移装置均位于真空腔中，真空腔上具有小孔，水冷台固定于位移装置上，导热基座固定于水冷台上，上盖和下盖均具有内螺纹，连接管具有外螺纹，上盖、连接管和下盖依次螺纹连接，连接管侧面连接有出气管，样品管为包括上段和下段的漏斗形，上段为漏斗部、下段为细管，细管的下端封闭，所述上段嵌套在下盖内，所述下段穿透下盖的下面，所述下段外径为0.9毫米、内径为0.7毫米，当连接管连接下盖时，能够压紧并固定样品管上段，样品管下段能够通过真空腔上的小孔插入真空腔；毛细管包括粗段和细段，所述粗段位于连接管与上盖之间，当上盖旋紧连接管时，能够压紧并固定毛细管粗段，粗段上方连接进气管，所述细段向下穿过连接管并嵌套在样品管中，所述细段的下端开口，所述细段外径为0.5毫米、内径为0.3毫米；碳纤维管呈竖直状态固定于导热基座上，碳纤维管外嵌套有热屏蔽腔，热屏蔽腔内固定有一对分别位于碳纤维管两侧的加热灯，样品位于所述样品管的下段内底部，样品管的下段插入并嵌套于碳纤维管的内部中心位置，辐射热计位于热屏蔽腔内，并能够移动，碳纤维管内中心位置附近具有温度计，所述碳纤维管内径为1.5毫米、外径为2.5毫米，所述碳纤维管的中心位置的侧面具有一对水平方向的通孔，光源发射的光能够通过其中一个所述通孔照射到样品上，样品上发生散射的光能够通过另一个所述通孔离开碳纤维管，并最终进入光谱仪；辐射热计主要包括外屏蔽罩、内屏蔽罩、热吸收器、热感应器、金属片、加热器和隔热片，所述外屏蔽罩和内屏蔽罩均为一侧底面具有小孔的圆筒形，内屏蔽罩同轴地连接于外屏蔽罩内，热吸收器为圆筒形并通过隔热片与内屏蔽罩的一侧底面连接，热感应器位于热吸收器内部侧壁，热吸收器内部具有金属片和加热器，加热器固定于金属片的一面，光能够依次通过外屏蔽罩的小孔、内屏蔽罩的小孔和热感应器入射到金属片；辐射热计控制电路主要包括电阻I、直流电源、可变电容、电阻II、电阻III、电阻IV、交流电源和锁相放大器，所述锁相放大器具有输入端和输出端，直流电源、电阻I和加热器循环连接并能够形成电流回路，所述直流电源具有信号端，能够根据输入的信号大小来控制直流电源输出电流的大小，所述电阻I阻值为1.0千欧，所述热感应器、电阻II、电阻III、电阻IV、锁相放大器和交流电源以惠斯通电桥形式连接，热感应器、电阻II、电阻III和电阻IV分别为惠斯通电桥的桥臂，惠斯通电桥的输出信号进入锁相放大器的输入端，锁相放大器的输出端与直流电源的信号端连接，可变电容与电阻II并联，可变电容范围为300pF至600pF，热感应器为热敏电阻，在20摄氏度时的电阻值为9.2千欧，电阻II和电阻IV的阻值均为10.0千欧，电阻III为可变电阻，电阻范围为8.0千欧至12.0千欧。The sample chamber used for spectroscopic experiments mainly includes an air inlet pipe, an upper cover, a capillary tube, a connecting pipe, an air outlet pipe, a sample tube, a lower cover, a sample, a carbon fiber tube, a heating lamp, a heat shielding cavity, a bolometer, a radiation Heat meter control circuit, thermometer, heat conduction base, water cooling platform and displacement device. xyz is a three-dimensional spatial coordinate system. The air inlet pipe is connected to a gas storage tank. Argon gas is stored in the gas storage tank and can adjust the flow rate of argon gas; experimental facilities There is a vacuum chamber, a gas tank, a light source and a spectrometer. The carbon fiber tube, heating lamp, heat shielding chamber, bolometer, thermometer, thermal conductive base, water cooling stage and displacement device are all located in the vacuum chamber. There is a small hole, the water-cooling stage is fixed on the displacement device, the heat-conducting base is fixed on the water-cooling stage, the upper cover and the lower cover both have internal threads, the connecting tube has external threads, the upper cover, connecting tube and lower cover are threaded in sequence, and the side of the connecting tube An air outlet pipe is connected. The sample tube is funnel-shaped and includes an upper section and a lower section. The upper section is a funnel and the lower section is a thin tube. The lower end of the thin tube is closed. The upper section is nested in the lower cover, and the lower section penetrates the bottom of the lower cover. , the outer diameter of the lower section is 0.9 mm and the inner diameter is 0.7 mm. When the connecting tube is connected to the lower cover, the upper section of the sample tube can be pressed and fixed, and the lower section of the sample tube can be inserted into the vacuum chamber through the small hole on the vacuum chamber; the capillary tube includes a thick The thick section is located between the connecting pipe and the upper cover. When the upper cover tightens the connecting pipe, the thick section of the capillary tube can be pressed and fixed. The upper section of the thick section is connected to the air inlet pipe, and the thin section passes downward. Through the connecting tube and nested in the sample tube, the lower end of the thin section is open, the outer diameter of the thin section is 0.5 mm, and the inner diameter is 0.3 mm; the carbon fiber tube is fixed on the thermal conductive base in a vertical state, and the outer diameter of the carbon fiber tube There is a heat shielding cavity nested inside. A pair of heating lamps located on both sides of the carbon fiber tube are fixed in the heat shielding cavity. The sample is located at the inner bottom of the lower section of the sample tube. The lower section of the sample tube is inserted and nested in the inner center of the carbon fiber tube. , the bolometer is located in the heat shielding cavity and can move. There is a thermometer near the center of the carbon fiber tube. The inner diameter of the carbon fiber tube is 1.5 mm and the outer diameter is 2.5 mm. The side of the center of the carbon fiber tube has a pair of horizontal The light emitted by the light source can illuminate the sample through one of the through holes, and the light scattered on the sample can leave the carbon fiber tube through the other through hole and finally enter the spectrometer; the bolometer mainly includes Outer shielding cover, inner shielding cover, heat absorber, thermal sensor, metal sheet, heater and heat insulation sheet. The outer shielding cover and the inner shielding cover are both cylindrical shapes with a small hole on the bottom surface of one side, and the inner shielding cover The cover is coaxially connected to the outer shielding cover. The heat absorber is cylindrical and is connected to the bottom surface of one side of the inner shielding cover through a heat insulation sheet. The thermal sensor is located on the internal side wall of the heat absorber. There is a metal inside the heat absorber. The heater is fixed on one side of the metal sheet, and the light can be incident on the metal sheet through the small holes of the outer shielding cover, the small holes of the inner shielding cover and the thermal sensor in sequence; the bolometer control circuit mainly includes resistors I, DC power supply, variable capacitor, resistor II, resistor III, resistor IV, AC power supply and lock-in amplifier. The lock-in amplifier has an input end and an output end. The DC power supply, resistor I and heater are cyclically connected and can form a current loop. , the DC power supply has a signal terminal, which can control the output current of the DC power supply according to the input signal size. The resistance of the resistor I is 1.0 kiloohms. The thermal sensor, resistor II, resistor III, resistor IV, The lock-in amplifier and the AC power supply are connected in the form of a Wheatstone bridge. The thermal sensor, resistor II, resistor III and resistor IV are the bridge arms of the Wheatstone bridge respectively. The output signal of the Wheatstone bridge enters the input end of the lock-in amplifier. , the output end of the lock-in amplifier is connected to the signal end of the DC power supply, the variable capacitor is connected in parallel with the resistor II, the variable capacitance range is 300pF to 600pF, the thermal sensor is a thermistor, the resistance value at 20 degrees Celsius is 9.2k The resistance values of resistor II and resistor IV are both 10.0 kilo ohms. Resistor III is a variable resistor with a resistance range of 8.0 kilo ohms to 12.0 kilo ohms.
辐射热计的工作原理：How a bolometer works:
辐射热计的控制电路为加热灯提供电能，并使得热吸收器的温度保持恒定；在没有光照辐射的情况下，辐射热计达到热平衡；有光照辐射入射到热吸收器的情况，光辐射热能被热吸收器吸收，从而产生热负载，热吸收器的温度上升；辐射热计的控制电路通过减少输出到加热灯的电流，使得热吸收器的温度保持恒定；辐射热计的控制电路输出的电能的减少量与热吸收器吸收的光辐射热能相等，通过计算辐射热计的控制电路输出的电能的减少量，来确定热吸收器吸收的光辐射热能。The control circuit of the bolometer provides electrical energy to the heating lamp and keeps the temperature of the heat absorber constant; when there is no light radiation, the bolometer reaches thermal equilibrium; when light radiation is incident on the heat absorber, the light radiates heat energy is absorbed by the heat absorber, thereby generating a heat load, and the temperature of the heat absorber rises; the control circuit of the bolometer keeps the temperature of the heat absorber constant by reducing the current output to the heating lamp; the control circuit of the bolometer outputs The reduction in electrical energy is equal to the optical radiation heat energy absorbed by the heat absorber. By calculating the reduction in electrical energy output by the control circuit of the bolometer, the optical radiation heat energy absorbed by the heat absorber is determined.
辐射热计的控制电路的工作原理：The working principle of the bolometer control circuit:
热感应器、电阻II、电阻III、电阻IV、锁相放大器和交流电源以惠斯通电桥形式连接，热感应器、电阻II、电阻III和电阻IV分别为惠斯通电桥的桥臂，惠斯通电桥的输出信号进入锁相放大器的输入端，锁相放大器的输出端与直流电源连接；交流电源输出有效电压0.1V的交流信号，所述交流信号频率为731Hz，惠斯通电桥的输出信号经过锁相放大器处理，锁相放大器的输出信号进入直流电源的信号端，在有光照辐射入射到热吸收器的情况下，热吸收器的温度上升，热感应器的电阻产生变化，导致惠斯通电桥的输出信号变化，从而锁相放大器输出至直流电源的信号端的信号产生变化，继而控制直流电源的输出电流，减少输出到加热灯的电流，使得热吸收器的温度保持恒定。The thermal sensor, resistor II, resistor III, resistor IV, lock-in amplifier and AC power supply are connected in the form of a Wheatstone bridge. The thermal sensor, resistor II, resistor III and resistor IV are the bridge arms of the Wheatstone bridge respectively. The output signal of the Stone bridge enters the input end of the lock-in amplifier, and the output end of the lock-in amplifier is connected to the DC power supply; the AC power supply outputs an AC signal with an effective voltage of 0.1V, and the frequency of the AC signal is 731Hz. The output of the Wheatstone bridge The signal is processed by the lock-in amplifier, and the output signal of the lock-in amplifier enters the signal end of the DC power supply. When light radiation is incident on the heat absorber, the temperature of the heat absorber rises, and the resistance of the thermal sensor changes, causing the The output signal of the Stone bridge changes, so that the signal output by the lock-in amplifier to the signal terminal of the DC power supply changes, and then controls the output current of the DC power supply, reducing the current output to the heating lamp, so that the temperature of the heat absorber remains constant.
分别测量电阻I和加热灯两端的电压VR和VH，计算得到加热灯的电功率VHVR/RR，其中RR为电阻I的阻值，通过加热灯的电功率的变化量即得到入射到辐射热计的光的辐射热能。Measure the voltage VR and V H at both ends of the resistor I and the heating lamp respectively, and calculate the electric power V H V R / RR of the heating lamp, where RR is the resistance of the resistor I, which is obtained by the change in the electric power of the heating lamp. The radiant heat energy of light incident on a bolometer.
利用所述一种用于光谱实验的样品腔进行光谱实验的步骤为：The steps of using the sample cavity for spectral experiments to conduct spectral experiments are:
一.将样品放置于样品管下段内底部，将样品管上段嵌套在下盖内、下段穿透下盖的下面，旋紧连接管与下盖之间螺纹并固定样品管上段，将毛细管细段向下穿过连接管并嵌套在样品管中，旋紧上盖与连接管之间螺纹并固定毛细管粗段，将样品管下段插入并嵌套于碳纤维管中，并使得样品位于碳纤维管的内部中心位置；1. Place the sample at the bottom of the lower section of the sample tube, nest the upper section of the sample tube inside the lower cover, and the lower section penetrates the bottom of the lower cover. Tighten the thread between the connecting tube and the lower cover and fix the upper section of the sample tube. Place the thin section of the capillary tube. Go down through the connecting tube and nest it in the sample tube. Tighten the thread between the upper cover and the connecting tube and fix the thick section of the capillary tube. Insert the lower section of the sample tube into the carbon fiber tube and nest it in the carbon fiber tube, so that the sample is located at the end of the carbon fiber tube. internal center position;
二.调节加热灯的温度、加热焦点大小和位置，使得加热焦点位于热屏蔽腔中心附近位置；2. Adjust the temperature, heating focus size and position of the heating lamp so that the heating focus is located near the center of the heat shield cavity;
三.调节光源位置，使得光源发射出的光射到加热灯的焦点位置，移动辐射热计到加热灯的焦点位置，使得光依次通过外屏蔽罩的小孔、内屏蔽罩的小孔和热感应器，入射到金属片，以此测量光在加热灯焦点位置的辐射热能；3. Adjust the position of the light source so that the light emitted by the light source hits the focus position of the heating lamp. Move the bolometer to the focus position of the heating lamp so that the light passes through the small holes of the outer shielding cover, the small holes of the inner shielding cover and the heat sink in sequence. The sensor is incident on the metal sheet to measure the radiated heat energy of the light at the focal point of the heating lamp;
四.将辐射热计从加热灯的焦点位置移开，调节位移装置，使得碳纤维管中心移动到加热灯的焦点位置，并使得光源发射出的光能够通过碳纤维管侧面的通孔射到样品上；4. Move the bolometer away from the focus position of the heating lamp, and adjust the displacement device so that the center of the carbon fiber tube moves to the focus position of the heating lamp, so that the light emitted by the light source can pass through the through hole on the side of the carbon fiber tube and hit the sample. ;
五.通过储气罐调节进入进气管的氩气的流速，流速典型值为5SCCM至30SCCM，氩气流依次经过进气管、毛细管的粗段和细段后，到达样品，并依次通过样品管的下段、样品管的上段和连接管，从出气管排出，能够将毛细管上的热量传递到样品，通过温度计测量样品的温度；5. Adjust the flow rate of the argon gas entering the air inlet pipe through the gas storage tank. The typical value of the flow rate is 5SCCM to 30SCCM. The argon gas flow passes through the air inlet pipe, the thick section and the thin section of the capillary tube in sequence, then reaches the sample, and passes through the lower section of the sample tube in sequence. , the upper section of the sample tube and the connecting tube are discharged from the air outlet pipe, which can transfer the heat on the capillary tube to the sample, and measure the temperature of the sample through a thermometer;
六.进行光谱实验，光源发射出的光通过碳纤维管侧面的一个通孔射到样品上，经过样品散射的光通过碳纤维管侧面的另一个通孔射出碳纤维管，并最终进入光谱仪，分析光谱仪采集的光信息，得到样品相关的物理性质。6. Perform a spectrum experiment. The light emitted by the light source is emitted to the sample through a through hole on the side of the carbon fiber tube. The light scattered by the sample is emitted out of the carbon fiber tube through another through hole on the side of the carbon fiber tube, and finally enters the spectrometer. The analysis is collected by the spectrometer. The optical information is obtained to obtain the relevant physical properties of the sample.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明装置采用的样品管结构紧凑，样品准备过程简单，通过加热灯的辐射热结合气流来控制样品温度，能够精确测量样品温度，并通过特殊的辐射热计测量入射光的辐射功率，精度较高。The sample tube used in the device of the present invention has a compact structure, and the sample preparation process is simple. The sample temperature is controlled by combining the radiant heat of the heating lamp with the air flow, so that the sample temperature can be accurately measured, and the radiant power of the incident light is measured by a special bolometer with higher accuracy. high.
附图说明Description of the drawings
下面结合本发明的图形进一步说明：The following is further explained in conjunction with the graphics of the present invention:
图1是本发明侧视示意图；Figure 1 is a schematic side view of the present invention;
图2是辐射热计放大示意图；Figure 2 is an enlarged schematic diagram of the bolometer;
图3是辐射热计控制电路示意图。Figure 3 is a schematic diagram of the bolometer control circuit.
图中，1.进气管，2.上盖，3.毛细管，4.连接管，5.出气管，6.样品管，7.下盖，8.样品，9.碳纤维管，10.加热灯，11.热屏蔽腔，12.辐射热计，12-1.外屏蔽罩，12-2.内屏蔽罩，12-3.热吸收器，12-4.热感应器，12-5.金属片，12-6.加热器，12-7.隔热片，12-8.电阻I，12-9.直流电源，12-10.可变电容，12-11.电阻II，12-12.电阻III，12-13.电阻IV，12-14.交流电源，12-15.锁相放大器，13.温度计，14.导热基座，15.水冷台，16.位移装置。In the picture, 1. Air inlet pipe, 2. Upper cover, 3. Capillary tube, 4. Connecting pipe, 5. Air outlet pipe, 6. Sample tube, 7. Lower cover, 8. Sample, 9. Carbon fiber tube, 10. Heating lamp , 11. Heat shielding cavity, 12. Bolometer, 12-1. Outer shielding cover, 12-2. Inner shielding cover, 12-3. Heat absorber, 12-4. Thermal sensor, 12-5. Metal Chip, 12-6. Heater, 12-7. Heat insulation sheet, 12-8. Resistor I, 12-9. DC power supply, 12-10. Variable capacitor, 12-11. Resistor II, 12-12. Resistor III, 12-13. Resistor IV, 12-14. AC power supply, 12-15. Lock-in amplifier, 13. Thermometer, 14. Thermal conductive base, 15. Water cooling platform, 16. Displacement device.
具体实施方式Detailed ways
如图1是本发明侧视示意图，xyz为三维空间坐标系，包括进气管(1)、上盖(2)、毛细管(3)、连接管(4)、出气管(5)、样品管(6)、下盖(7)、样品(8)、碳纤维管(9)、加热灯(10)、热屏蔽腔(11)、辐射热计(12)、温度计(13)、导热基座(14)、水冷台(15)和位移装置(16)，上盖(2)和下盖(7)均具有内螺纹，连接管(4)具有外螺纹，上盖(2)、连接管(4)和下盖(7)依次螺纹连接，连接管(4)侧面连接有出气管(5)，样品管(6)为包括上段和下段的漏斗形，上段为漏斗部、下段为细管，细管的下端封闭，所述上段嵌套在下盖(7)内，所述下段穿透下盖(7)的下面，所述下段外径为0.9毫米、内径为0.7毫米，当连接管(4)连接下盖(7)时，能够压紧并固定样品管(6)上段，样品管(6)下段能够通过真空腔上的小孔插入真空腔；毛细管(3)包括粗段和细段，所述粗段位于连接管(4)与上盖(2)之间，当上盖(2)旋紧连接管(4)时，能够压紧并固定毛细管(3)粗段，粗段上方连接进气管(1)，所述细段向下穿过连接管(4)并嵌套在样品管(6)中，所述细段的下端开口，所述细段外径为0.5毫米、内径为0.3毫米；进气管(1)连接储气罐，储气罐中储存有氩气，并能够调节氩气的流速；所述碳纤维管(9)、加热灯(10)、热屏蔽腔(11)、辐射热计(12)、温度计(13)、导热基座(14)、水冷台(15)和位移装置(16)均位于真空腔中，真空腔上具有小孔，水冷台(15)固定于位移装置(16)上，导热基座(14)固定于水冷台(15)上，碳纤维管(9)呈竖直状态固定于导热基座(14)上，碳纤维管(9)外嵌套有热屏蔽腔(11)，热屏蔽腔(11)内固定有一对分别位于碳纤维管(9)两侧的加热灯(10)，样品(8)位于所述样品管(6)的下段内底部，样品管(6)的下段插入并嵌套于碳纤维管(9)的内部中心位置，辐射热计(12)位于热屏蔽腔(11)内，并能够移动，碳纤维管(9)内中心位置附近具有温度计(13)，所述碳纤维管(9)内径为1.5毫米、外径为2.5毫米，所述碳纤维管(9)的中心位置的侧面具有一对水平方向的通孔，光源发射的光能够通过其中一个所述通孔照射到样品(8)上，样品(8)上发生散射的光能够通过另一个所述通孔离开碳纤维管(9)，并最终进入光谱仪。Figure 1 is a schematic side view of the present invention. 6), lower cover (7), sample (8), carbon fiber tube (9), heating lamp (10), heat shielding cavity (11), bolometer (12), thermometer (13), thermal conductive base (14 ), water cooling stage (15) and displacement device (16), the upper cover (2) and lower cover (7) both have internal threads, the connecting pipe (4) has external threads, the upper cover (2) and the connecting pipe (4) It is threadedly connected to the lower cover (7) in sequence. The side of the connecting pipe (4) is connected with an air outlet pipe (5). The sample tube (6) is funnel-shaped including an upper section and a lower section. The upper section is a funnel and the lower section is a thin tube. The thin tube The lower end is closed, the upper section is nested in the lower cover (7), and the lower section penetrates the bottom of the lower cover (7). The outer diameter of the lower section is 0.9 mm and the inner diameter is 0.7 mm. When the connecting pipe (4) is connected When the cover (7) is lowered, the upper section of the sample tube (6) can be pressed and fixed, and the lower section of the sample tube (6) can be inserted into the vacuum chamber through the small hole in the vacuum chamber; the capillary tube (3) includes a thick section and a thin section. The thick section is located between the connecting pipe (4) and the upper cover (2). When the upper cover (2) tightens the connecting pipe (4), it can compress and fix the thick section of the capillary tube (3), and the upper section of the thick section is connected to the air inlet pipe. (1), the thin section passes downward through the connecting tube (4) and is nested in the sample tube (6). The lower end of the thin section is open. The outer diameter of the thin section is 0.5 mm and the inner diameter is 0.3 mm. ; The air inlet pipe (1) is connected to a gas storage tank, which stores argon gas and can adjust the flow rate of the argon gas; the carbon fiber tube (9), heating lamp (10), heat shielding cavity (11), radiation The heat meter (12), thermometer (13), thermal conductive base (14), water cooling stage (15) and displacement device (16) are all located in the vacuum chamber. There are small holes in the vacuum chamber, and the water cooling stage (15) is fixed in the displacement On the device (16), the heat-conducting base (14) is fixed on the water-cooling platform (15), and the carbon fiber tube (9) is fixed on the heat-conducting base (14) in a vertical state. There is a heat conductor embedded outside the carbon fiber tube (9). Shielding cavity (11). A pair of heating lamps (10) located on both sides of the carbon fiber tube (9) are fixed in the heat shielding cavity (11). The sample (8) is located at the inner bottom of the lower section of the sample tube (6). The sample The lower section of the tube (6) is inserted and nested in the inner center of the carbon fiber tube (9). The bolometer (12) is located in the heat shielding cavity (11) and can move. There is a bolometer (12) near the inner center of the carbon fiber tube (9). Thermometer (13), the inner diameter of the carbon fiber tube (9) is 1.5 mm and the outer diameter is 2.5 mm. The side of the center position of the carbon fiber tube (9) has a pair of horizontal through holes through which the light emitted by the light source can pass. One of the through holes illuminates the sample (8), and the light scattered on the sample (8) can leave the carbon fiber tube (9) through the other through hole and finally enter the spectrometer.
如图2是辐射热计放大示意图，辐射热计(12)主要包括外屏蔽罩(12-1)、内屏蔽罩(12-2)、热吸收器(12-3)、热感应器(12-4)、金属片(12-5)、加热器(12-6)和隔热片(12-7)，所述外屏蔽罩(12-1)和内屏蔽罩(12-2)均为一侧底面具有小孔的圆筒形，内屏蔽罩(12-2)同轴地连接于外屏蔽罩(12-1)内，热吸收器(12-3)为圆筒形并通过隔热片(12-7)与内屏蔽罩(12-2)的一侧底面连接，热感应器(12-4)位于热吸收器(12-3)内部侧壁，热吸收器(12-3)内部具有金属片(12-5)和加热器(12-6)，加热器(12-6)固定于金属片(12-5)的一面，光能够依次通过外屏蔽罩(12-1)的小孔、内屏蔽罩(12-2)的小孔和热感应器(12-4)入射到金属片(12-5)。Figure 2 is an enlarged schematic diagram of a bolometer. The bolometer (12) mainly includes an outer shielding cover (12-1), an inner shielding cover (12-2), a heat absorber (12-3), and a thermal sensor (12 -4), metal sheet (12-5), heater (12-6) and heat insulation sheet (12-7), the outer shielding cover (12-1) and the inner shielding cover (12-2) are The bottom surface of one side is cylindrical with a small hole. The inner shielding cover (12-2) is coaxially connected to the outer shielding cover (12-1). The heat absorber (12-3) is cylindrical and is insulated by The piece (12-7) is connected to the bottom surface of one side of the inner shielding cover (12-2), the thermal sensor (12-4) is located on the inner side wall of the heat absorber (12-3), and the heat absorber (12-3) There is a metal sheet (12-5) and a heater (12-6) inside. The heater (12-6) is fixed on one side of the metal sheet (12-5), and the light can pass through the outer shielding cover (12-1) in sequence. The small hole, the small hole of the inner shielding cover (12-2) and the thermal sensor (12-4) are incident on the metal sheet (12-5).
如图3是辐射热计控制电路示意图，辐射热计(12)控制电路主要包括电阻I(12-8)、直流电源(12-9)、可变电容(12-10)、电阻II(12-11)、电阻III(12-12)、电阻IV(12-13)、交流电源(12-14)和锁相放大器(12-15)，所述锁相放大器(12-15)具有输入端和输出端，直流电源(12-9)、电阻I(12-8)和加热器(12-6)循环连接并能够形成电流回路，所述直流电源(12-9)具有信号端，能够根据输入的信号大小来控制直流电源(12-9)输出电流的大小，所述电阻I(12-8)阻值为1.0千欧，所述热感应器(12-4)、电阻II(12-11)、电阻III(12-12)、电阻IV(12-13)、锁相放大器(12-15)和交流电源(12-14)以惠斯通电桥形式连接，热感应器(12-4)、电阻II(12-11)、电阻III(12-12)和电阻IV(12-13)分别为惠斯通电桥的桥臂，惠斯通电桥的输出信号进入锁相放大器(12-15)的输入端，锁相放大器(12-15)的输出端与直流电源(12-9)的信号端连接，可变电容(12-10)与电阻II(12-11)并联，可变电容范围为300pF至600pF，热感应器(12-4)为热敏电阻，在20摄氏度时的电阻值为9.2千欧，电阻II(12-11)和电阻IV(12-13)的阻值均为10.0千欧，电阻III(12-12)为可变电阻，电阻范围为8.0千欧至12.0千欧。Figure 3 is a schematic diagram of the bolometer control circuit. The bolometer (12) control circuit mainly includes resistor I (12-8), DC power supply (12-9), variable capacitor (12-10), resistor II (12 -11), resistor III (12-12), resistor IV (12-13), AC power supply (12-14) and lock-in amplifier (12-15), the lock-in amplifier (12-15) has an input terminal and the output terminal, the DC power supply (12-9), the resistor I (12-8) and the heater (12-6) are cyclically connected and can form a current loop. The DC power supply (12-9) has a signal terminal and can be The size of the input signal controls the size of the output current of the DC power supply (12-9). The resistance of the resistor I (12-8) is 1.0 kiloohms. The thermal sensor (12-4) and the resistor II (12- 11), resistor III (12-12), resistor IV (12-13), lock-in amplifier (12-15) and AC power supply (12-14) are connected in the form of a Wheatstone bridge, and the thermal sensor (12-4 ), resistor II (12-11), resistor III (12-12) and resistor IV (12-13) are the arms of the Wheatstone bridge respectively. The output signal of the Wheatstone bridge enters the lock-in amplifier (12-15 ), the output end of the lock-in amplifier (12-15) is connected to the signal end of the DC power supply (12-9), the variable capacitor (12-10) is connected in parallel with the resistor II (12-11), the variable capacitor The range is 300pF to 600pF. The thermal sensor (12-4) is a thermistor with a resistance value of 9.2 kΩ at 20 degrees Celsius. The resistance values of resistor II (12-11) and resistor IV (12-13) are both is 10.0 kiloohms, and resistor III (12-12) is a variable resistor with a resistance range of 8.0 kiloohms to 12.0 kiloohms.
辐射热计(12)的工作原理：How the bolometer (12) works:
辐射热计(12)的控制电路为加热器(12-6)提供电能，并使得热吸收器(12-3)的温度保持恒定；在没有光照辐射的情况下，辐射热计(12)达到热平衡；有光照辐射入射到热吸收器(12-3)的情况，光辐射热能被热吸收器(12-3)吸收，从而产生热负载，热吸收器(12-3)的温度上升；辐射热计(12)的控制电路通过减少输出到加热器(12-6)的电流，使得热吸收器(12-3)的温度保持恒定；辐射热计(12)的控制电路输出的电能的减少量与热吸收器(12-3)吸收的光辐射热能相等，通过计算辐射热计(12)的控制电路输出的电能的减少量，来确定热吸收器(12-3)吸收的光辐射热能。The control circuit of the bolometer (12) provides electric energy to the heater (12-6) and keeps the temperature of the heat absorber (12-3) constant; in the absence of light radiation, the bolometer (12) reaches Thermal balance; when light radiation is incident on the heat absorber (12-3), the heat energy of the light radiation is absorbed by the heat absorber (12-3), thereby generating a heat load, and the temperature of the heat absorber (12-3) rises; radiation The control circuit of the heat meter (12) keeps the temperature of the heat absorber (12-3) constant by reducing the current output to the heater (12-6); the control circuit of the bolometer (12) reduces the electric energy output The amount is equal to the optical radiation heat energy absorbed by the heat absorber (12-3). By calculating the reduction in the electric energy output by the control circuit of the bolometer (12), the optical radiation heat energy absorbed by the heat absorber (12-3) is determined. .
辐射热计(12)的控制电路的工作原理：The working principle of the control circuit of the bolometer (12):
热感应器(12-4)、电阻II(12-11)、电阻III(12-12)、电阻IV(12-13)、锁相放大器(12-15)和交流电源(12-14)以惠斯通电桥形式连接，热感应器(12-4)、电阻II(12-11)、电阻III(12-12)和电阻IV(12-13)分别为惠斯通电桥的桥臂，惠斯通电桥的输出信号进入锁相放大器(12-15)的输入端，锁相放大器(12-15)的输出端与直流电源(12-9)连接；交流电源(12-14)输出有效电压0.1V的交流信号，所述交流信号频率为731Hz，惠斯通电桥的输出信号经过锁相放大器(12-15)处理，锁相放大器(12-15)的输出信号进入直流电源(12-9)的信号端，在有光照辐射入射到热吸收器(12-3)的情况下，热吸收器(12-3)的温度上升，热感应器(12-4)的电阻产生变化，导致惠斯通电桥的输出信号变化，从而锁相放大器(12-15)输出至直流电源(12-9)的信号端的信号产生变化，继而控制直流电源(12-9)的输出电流，减少输出到加热器(12-6)的电流，使得热吸收器(12-3)的温度保持恒定。Thermal sensor (12-4), resistor II (12-11), resistor III (12-12), resistor IV (12-13), lock-in amplifier (12-15) and AC power supply (12-14) and The connection is in the form of a Wheatstone bridge. The thermal sensor (12-4), resistor II (12-11), resistor III (12-12) and resistor IV (12-13) are the bridge arms of the Wheatstone bridge respectively. The output signal of the Stone bridge enters the input end of the lock-in amplifier (12-15), and the output end of the lock-in amplifier (12-15) is connected to the DC power supply (12-9); the AC power supply (12-14) outputs an effective voltage 0.1V AC signal, the AC signal frequency is 731Hz, the output signal of the Wheatstone bridge is processed by the lock-in amplifier (12-15), and the output signal of the lock-in amplifier (12-15) enters the DC power supply (12-9 ) signal end, when light radiation is incident on the heat absorber (12-3), the temperature of the heat absorber (12-3) rises, and the resistance of the heat sensor (12-4) changes, resulting in The output signal of the Stone bridge changes, so that the signal output from the lock-in amplifier (12-15) to the signal terminal of the DC power supply (12-9) changes, and then controls the output current of the DC power supply (12-9) to reduce the output to the heating The current of the heat absorber (12-6) is kept constant so that the temperature of the heat absorber (12-3) is kept constant.
分别测量电阻I(12-8)和加热器(12-6)两端的电压VR和VH，计算得到加热器(12-6)的电功率VHVR/RR，其中RR为电阻I(12-8)的阻值，通过加热器(12-6)的电功率的变化量即得到入射到辐射热计(12)的光的辐射热能。Measure the voltage VR and V H at both ends of the resistor I (12-8) and the heater (12-6) respectively, and calculate the electric power V H V R / RR of the heater (12-6), where R R is the resistance The resistance value of I (12-8) and the change in the electric power of the heater (12-6) are the radiant heat energy of the light incident on the bolometer (12).
所述一种用于光谱实验的样品腔主要包括进气管(1)、上盖(2)、毛细管(3)、连接管(4)、出气管(5)、样品管(6)、下盖(7)、样品(8)、碳纤维管(9)、加热灯(10)、热屏蔽腔(11)、辐射热计(12)、辐射热计(12)控制电路、温度计(13)、导热基座(14)、水冷台(15)和位移装置(16)，xyz为三维空间坐标系，进气管(1)连接储气罐，储气罐中储存有氩气，并能够调节氩气的流速；实验设施有真空腔、储气罐、光源和光谱仪，所述碳纤维管(9)、加热灯(10)、热屏蔽腔(11)、辐射热计(12)、温度计(13)、导热基座(14)、水冷台(15)和位移装置(16)均位于真空腔中，真空腔上具有小孔，水冷台(15)固定于位移装置(16)上，导热基座(14)固定于水冷台(15)上，上盖(2)和下盖(7)均具有内螺纹，连接管(4)具有外螺纹，上盖(2)、连接管(4)和下盖(7)依次螺纹连接，连接管(4)侧面连接有出气管(5)，样品管(6)为包括上段和下段的漏斗形，上段为漏斗部、下段为细管，细管的下端封闭，所述上段嵌套在下盖(7)内，所述下段穿透下盖(7)的下面，所述下段外径为0.9毫米、内径为0.7毫米，当连接管(4)连接下盖(7)时，能够压紧并固定样品管(6)上段，样品管(6)下段能够通过真空腔上的小孔插入真空腔；毛细管(3)包括粗段和细段，所述粗段位于连接管(4)与上盖(2)之间，当上盖(2)旋紧连接管(4)时，能够压紧并固定毛细管(3)粗段，粗段上方连接进气管(1)，所述细段向下穿过连接管(4)并嵌套在样品管(6)中，所述细段的下端开口，所述细段外径为0.5毫米、内径为0.3毫米；碳纤维管(9)呈竖直状态固定于导热基座(14)上，碳纤维管(9)外嵌套有热屏蔽腔(11)，热屏蔽腔(11)内固定有一对分别位于碳纤维管(9)两侧的加热灯(10)，样品(8)位于所述样品管(6)的下段内底部，样品管(6)的下段插入并嵌套于碳纤维管(9)的内部中心位置，辐射热计(12)位于热屏蔽腔(11)内，并能够移动，碳纤维管(9)内中心位置附近具有温度计(13)，所述碳纤维管(9)内径为1.5毫米、外径为2.5毫米，所述碳纤维管(9)的中心位置的侧面具有一对水平方向的通孔，光源发射的光能够通过其中一个所述通孔照射到样品(8)上，样品(8)上发生散射的光能够通过另一个所述通孔离开碳纤维管(9)，并最终进入光谱仪；辐射热计(12)主要包括外屏蔽罩(12-1)、内屏蔽罩(12-2)、热吸收器(12-3)、热感应器(12-4)、金属片(12-5)、加热器(12-6)和隔热片(12-7)，所述外屏蔽罩(12-1)和内屏蔽罩(12-2)均为一侧底面具有小孔的圆筒形，内屏蔽罩(12-2)同轴地连接于外屏蔽罩(12-1)内，热吸收器(12-3)为圆筒形并通过隔热片(12-7)与内屏蔽罩(12-2)的一侧底面连接，热感应器(12-4)位于热吸收器(12-3)内部侧壁，热吸收器(12-3)内部具有金属片(12-5)和加热器(12-6)，加热器(12-6)固定于金属片(12-5)的一面，光能够依次通过外屏蔽罩(12-1)的小孔、内屏蔽罩(12-2)的小孔和热感应器(12-4)入射到金属片(12-5)；辐射热计(12)控制电路主要包括电阻I(12-8)、直流电源(12-9)、可变电容(12-10)、电阻II(12-11)、电阻III(12-12)、电阻IV(12-13)、交流电源(12-14)和锁相放大器(12-15)，所述锁相放大器(12-15)具有输入端和输出端，直流电源(12-9)、电阻I(12-8)和加热器(12-6)循环连接并能够形成电流回路，所述直流电源(12-9)具有信号端，能够根据输入的信号大小来控制直流电源(12-9)输出电流的大小，所述电阻I(12-8)阻值为1.0千欧，所述热感应器(12-4)、电阻II(12-11)、电阻III(12-12)、电阻IV(12-13)、锁相放大器(12-15)和交流电源(12-14)以惠斯通电桥形式连接，热感应器(12-4)、电阻II(12-11)、电阻III(12-12)和电阻IV(12-13)分别为惠斯通电桥的桥臂，惠斯通电桥的输出信号进入锁相放大器(12-15)的输入端，锁相放大器(12-15)的输出端与直流电源(12-9)的信号端连接，可变电容(12-10)与电阻II(12-11)并联，可变电容范围为300pF至600pF，热感应器(12-4)为热敏电阻，在20摄氏度时的电阻值为9.2千欧，电阻II(12-11)和电阻IV(12-13)的阻值均为10.0千欧，电阻III(12-12)为可变电阻，电阻范围为8.0千欧至12.0千欧。The sample chamber used for spectroscopic experiments mainly includes an air inlet pipe (1), an upper cover (2), a capillary tube (3), a connecting pipe (4), an air outlet pipe (5), a sample tube (6), and a lower cover. (7), sample (8), carbon fiber tube (9), heating lamp (10), heat shielding chamber (11), bolometer (12), bolometer (12) control circuit, thermometer (13), heat conduction The base (14), the water cooling platform (15) and the displacement device (16), xyz is the three-dimensional spatial coordinate system, the air inlet pipe (1) is connected to the gas storage tank, the gas storage tank stores argon gas, and can adjust the flow rate of the argon gas Flow rate; the experimental facilities include a vacuum chamber, a gas tank, a light source and a spectrometer. The carbon fiber tube (9), heating lamp (10), heat shielding chamber (11), bolometer (12), thermometer (13), thermal conductivity The base (14), water cooling platform (15) and displacement device (16) are all located in the vacuum chamber. The vacuum chamber has small holes. The water cooling platform (15) is fixed on the displacement device (16). The thermal conductive base (14) Fixed on the water cooling platform (15), the upper cover (2) and lower cover (7) both have internal threads, the connecting pipe (4) has external threads, the upper cover (2), the connecting pipe (4) and the lower cover (7) ) are threaded in sequence. The connecting pipe (4) is connected to an air outlet pipe (5) on the side. The sample tube (6) is funnel-shaped including an upper section and a lower section. The upper section is a funnel and the lower section is a thin tube. The lower end of the thin tube is closed. The upper section is nested in the lower cover (7), and the lower section penetrates the bottom of the lower cover (7). The outer diameter of the lower section is 0.9 mm and the inner diameter is 0.7 mm. When the connecting pipe (4) is connected to the lower cover (7) When, the upper section of the sample tube (6) can be pressed and fixed, and the lower section of the sample tube (6) can be inserted into the vacuum chamber through the small hole on the vacuum chamber; the capillary tube (3) includes a thick section and a thin section, and the thick section is located in the connecting tube. (4) and the upper cover (2), when the upper cover (2) tightens the connecting pipe (4), the thick section of the capillary tube (3) can be pressed and fixed, and the upper section of the thick section is connected to the air inlet pipe (1), so The thin section passes downward through the connecting tube (4) and is nested in the sample tube (6). The lower end of the thin section is open. The outer diameter of the thin section is 0.5 mm and the inner diameter is 0.3 mm; the carbon fiber tube (9) ) is vertically fixed on the thermal base (14). A heat shielding cavity (11) is nested outside the carbon fiber tube (9). A pair of heat shielding chambers (11) are fixed on both sides of the carbon fiber tube (9). The heating lamp (10), the sample (8) is located at the inner bottom of the lower section of the sample tube (6), the lower section of the sample tube (6) is inserted and nested in the inner center of the carbon fiber tube (9), and the bolometer ( 12) It is located in the heat shielding cavity (11) and can move. There is a thermometer (13) near the center of the carbon fiber tube (9). The inner diameter of the carbon fiber tube (9) is 1.5 mm and the outer diameter is 2.5 mm. There is a pair of horizontal through holes on the side of the center of the carbon fiber tube (9). The light emitted by the light source can shine on the sample (8) through one of the through holes, and the light scattered on the sample (8) can pass through. The other through hole leaves the carbon fiber tube (9) and finally enters the spectrometer; the bolometer (12) mainly includes an outer shielding cover (12-1), an inner shielding cover (12-2), and a heat absorber (12- 3), thermal sensor (12-4), metal sheet (12-5), heater (12-6) and heat insulation sheet (12-7), the outer shielding cover (12-1) and the inner shielding The covers (12-2) are all cylindrical with a small hole on one side of the bottom surface. The inner shielding cover (12-2) is coaxially connected to the outer shielding cover (12-1), and the heat absorber (12-3) It is cylindrical and is connected to the bottom surface of one side of the inner shielding cover (12-2) through the heat insulation sheet (12-7). The thermal sensor (12-4) is located on the internal side wall of the heat absorber (12-3). The heat absorber (12-3) has a metal sheet (12-5) and a heater (12-6) inside. The heater (12-6) is fixed on one side of the metal sheet (12-5), and the light can pass through the outside in sequence. The small holes of the shielding cover (12-1), the small holes of the inner shielding cover (12-2) and the thermal sensor (12-4) are incident on the metal sheet (12-5); the main control circuit of the bolometer (12) Including resistor I (12-8), DC power supply (12-9), variable capacitor (12-10), resistor II (12-11), resistor III (12-12), resistor IV (12-13), AC power supply (12-14) and lock-in amplifier (12-15), the lock-in amplifier (12-15) has an input terminal and an output terminal, a DC power supply (12-9), a resistor I (12-8) and The heater (12-6) is connected cyclically and can form a current loop. The DC power supply (12-9) has a signal terminal and can control the output current of the DC power supply (12-9) according to the input signal size. Resistor I (12-8) has a resistance value of 1.0 kiloohms. The thermal sensor (12-4), resistor II (12-11), resistor III (12-12), resistor IV (12-13), lock Phase amplifier (12-15) and AC power supply (12-14) are connected in the form of a Wheatstone bridge, thermal sensor (12-4), resistor II (12-11), resistor III (12-12) and resistor IV (12-13) are the bridge arms of the Wheatstone bridge respectively. The output signal of the Wheatstone bridge enters the input end of the lock-in amplifier (12-15). The output end of the lock-in amplifier (12-15) is connected to the DC power supply ( 12-9) is connected to the signal end, the variable capacitor (12-10) is connected in parallel with the resistor II (12-11), the variable capacitance range is 300pF to 600pF, the thermal sensor (12-4) is a thermistor, in The resistance value at 20 degrees Celsius is 9.2 kiloohms. The resistance values of resistor II (12-11) and resistor IV (12-13) are both 10.0 kiloohms. Resistor III (12-12) is a variable resistor with a resistance range of 8.0 kΩ to 12.0 kΩ.
本发明的样品管结构简单，样品准备过程较为省时，通过加热灯的辐射热对样品均匀加热，结合气流能够精确控制样品温度，并采用特殊设计的辐射热计准确测量入射光的辐射功率。The sample tube of the present invention has a simple structure, and the sample preparation process is relatively time-saving. The sample is uniformly heated by the radiant heat of the heating lamp, and the sample temperature can be accurately controlled by combining with air flow. The specially designed bolometer is used to accurately measure the radiant power of the incident light.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0417791A2 (en) * | 1989-09-14 | 1991-03-20 | ULTRAKUST electronic GmbH | Method and apparatus for the compensation of the temperature of the housing or the ambiant temperature of a pyrometer |
| CN101458124A (en) * | 2007-12-12 | 2009-06-17 | Ulis股份公司 | Device and system for detecting infrared radiation, method of reading imaging bolometer |
| CN102042993A (en) * | 2010-11-23 | 2011-05-04 | 清华大学 | System for measuring normal spectral emissivity of high-temperature material |
| CN202563360U (en) * | 2011-12-06 | 2012-11-28 | 广西科学院 | Sample temperature regulating device for spectrum analysis experiments |
| RU2593445C1 (en) * | 2015-06-09 | 2016-08-10 | Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) | Device for determining spectral emissivity of heat-shielding materials at high temperatures |
| CN107727247A (en) * | 2017-11-18 | 2018-02-23 | 南京理工大学 | A kind of hot conditions trnaslucent materials spectral emissivity measurement apparatus and method |
| CN212622183U (en) * | 2018-09-06 | 2021-02-26 | 金华职业技术学院 | A sample cavity for spectroscopic experiments |
-
2018
- 2018-09-06 CN CN201811084091.6A patent/CN109142227B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0417791A2 (en) * | 1989-09-14 | 1991-03-20 | ULTRAKUST electronic GmbH | Method and apparatus for the compensation of the temperature of the housing or the ambiant temperature of a pyrometer |
| CN101458124A (en) * | 2007-12-12 | 2009-06-17 | Ulis股份公司 | Device and system for detecting infrared radiation, method of reading imaging bolometer |
| CN102042993A (en) * | 2010-11-23 | 2011-05-04 | 清华大学 | System for measuring normal spectral emissivity of high-temperature material |
| CN202563360U (en) * | 2011-12-06 | 2012-11-28 | 广西科学院 | Sample temperature regulating device for spectrum analysis experiments |
| RU2593445C1 (en) * | 2015-06-09 | 2016-08-10 | Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) | Device for determining spectral emissivity of heat-shielding materials at high temperatures |
| CN107727247A (en) * | 2017-11-18 | 2018-02-23 | 南京理工大学 | A kind of hot conditions trnaslucent materials spectral emissivity measurement apparatus and method |
| CN212622183U (en) * | 2018-09-06 | 2021-02-26 | 金华职业技术学院 | A sample cavity for spectroscopic experiments |
Non-Patent Citations (1)
| Title |
|---|
| 微型化绝对辐射计研制;方伟 等;科技创新导报(25);第2-3页 * |
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