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CN100552396C - Radiation-absorbing composite diamond heat exchange membrane and its preparation method - Google Patents

Radiation-absorbing composite diamond heat exchange membrane and its preparation method Download PDF

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Publication number
CN100552396C
CN100552396C CNB2008100505015A CN200810050501A CN100552396C CN 100552396 C CN100552396 C CN 100552396C CN B2008100505015 A CNB2008100505015 A CN B2008100505015A CN 200810050501 A CN200810050501 A CN 200810050501A CN 100552396 C CN100552396 C CN 100552396C
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diamond
heat sink
sheet
heat exchange
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CN101251421A (en
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梁中翥
梁静秋
王维彪
方伟
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Abstract

本发明涉及一种适用于测量辐射设备的吸收辐射复合金刚石热交换膜片及其制备方法，该复合金刚石热交换膜片是由含有石墨相的黑色金刚石膜层与纯金刚石片层复合而成，纯金刚石片层作为热沉材料，含有石墨相的黑色金刚石膜层作为光辐射吸收材料。其制备方法是通过一次化学气相沉积制备热沉金刚石片，再在金刚石片上通过二次化学气相沉积含有石墨相的黑色金刚石膜层。本发明复合金刚石热交换膜片具有抗热冲击能力强、吸收辐射材料层受辐射后吸收率稳定无变化的优点，对辐射的吸收率较高，达99%～99.2%，提高了辐射计的测量精度和灵敏度。The invention relates to a radiation-absorbing composite diamond heat exchange diaphragm suitable for measuring radiation equipment and a preparation method thereof. The composite diamond heat exchange diaphragm is composed of a black diamond film layer containing a graphite phase and a pure diamond sheet layer. The pure diamond sheet is used as the heat sink material, and the black diamond film layer containing the graphite phase is used as the light radiation absorbing material. The preparation method is to prepare a heat-sink diamond sheet by one-time chemical vapor deposition, and then deposit a black diamond film layer containing graphite phase on the diamond sheet by secondary chemical vapor deposition. The composite diamond heat exchange diaphragm of the present invention has the advantages of strong thermal shock resistance and stable absorption rate of the radiation-absorbing material layer after being irradiated. Measurement accuracy and sensitivity.

Description

Absorbed radiation composite diamond heat-exchanging diaphragm and preparation method thereof
Technical field
The present invention relates to a kind of absorbed radiation composite diamond heat-exchanging diaphragm that is applicable to measuring radiation equipment and preparation method thereof.
Background technology
In order to study earth radiation budget and energy circulation and, to need accurately to measure and the long term monitoring solar irradiance to the influence of global environment and climate change.Being used for observing the instrument of solar irradiance on satellite is the absolute measuring bolometer, its measuring principle is to utilize the photoelectricity equivalence, it is the electrothermic type detector of electric power nominal light power, the thermal effect of the thermal effect that shines the unknown radiant illumination on the absolute measuring bolometer with known electric power (measuring heating current intensity and voltage) compared, make the electric power of heating be equivalent to the radiation power of reception, the method that electric power reproduces is demarcated the radiation scale.Therefore, needing to absorb the black-materials layer on the absolute measuring bolometer of measuring solar irradiance comes radiation is absorbed.Owing to will inevitably be subjected to the interference of atmosphere, cloud layer etc. when testing solar irradiance on the ground, observe so the absolute measuring bolometer is placed on the weather satellite.This just requires black absorption radiative material and the heat sink material on the absolute measuring bolometer not only will be in conjunction with tight, good mechanical property, and will have high thermal conductivity and ultraviolet irradiation changes little.Before the present invention, it is pitch-dark to be used for black absorption radiative material on the electric calibration absolute measuring bolometer and to be to be coated with the skim direct reflection with the thin-walled silver conical cavity of electroplating technology special facture and inner cavity surface, and heat sink material is the metal aluminum barrel.The thermal conductivity of this different materials is not too high, the adhesiveness that reflects pitch-dark and silver-colored chamber is not strong, and reflecting the pitch-dark ultraviolet ray irradiation back that is subjected to for a long time on satellite can reduce gradually to the absorptivity of radiation, this all can influence the measurement of absolute measuring bolometer to solar irradiance, causes the measuring accuracy of radiometer to reduce, sensitivity is low and Measuring Time is long.
Adamantine structure cell characteristics make it have the highest hardness, the highest thermal conductivity and radiation resistance, are the insulator of electricity, are again the good conductors of heat.So the heat sink material on the absolute measuring bolometer is preferably selected high-purity adamas diaphragm for use, and the material that is used for the optical radiation absorption adopts black to contain the diamond film of high graphite phase carbon, but at present because the diamond film of the chemical gaseous phase depositing process that adopts growth can only have a kind of character usually, promptly can only be the high-purity diamond film or the black diamond film of graphitiferous phase carbon, high but the absorbed radiation not of high-purity diamond film thermal conductivity, and the black diamond film absorbed radiation of graphitiferous phase but thermal conductivity is not high enough, therefore, the adamas diaphragm of this single character can not satisfy the requirement of heat-exchanging diaphragm simultaneously: not only absorbed radiation but also have high thermal conductivity.Prior art is difficult to carry out the adamantine growth simultaneously of two kinds of character, if because growth conditions changes in growth course, can cause aura instability or different grown layers to come off.
Summary of the invention
The objective of the invention is in order to solve at present in measuring radiation equipment, the shortcoming that used absorbed radiation heat-exchanging diaphragm exists on the absolute radiometer as the monitoring solar irradiance proposes a kind of absorbed radiation composite diamond heat-exchanging diaphragm and preparation method thereof.
Absorbed radiation composite diamond heat-exchanging diaphragm of the present invention, be to be composited by black diamond rete that contains graphite phase carbon and pure diamond lamella, the pure diamond lamella is as heat sink material, and the black diamond rete that contains the graphite phase is as the optical radiation absorbing material; The described black diamond rete that contains the graphite phase is to be evenly distributed in the diamond crystal by a large amount of graphite phase carbon atoms to form, and the thermal conductivity of this rete is that 6～8W/Kcm, resistivity are 10 8～10 12Ω cm, this film surface has micro-nano concaveconvex structure, roughness is 5nm～15 μ m, the adamantine crystal grain diameter of this rete is 1nm～10 μ m, intercrystalline forms pit, form the upright micro-nano size diamond crystals array based on (111) crystal face around pit, form light localization film, thicknesses of layers is between 100nm～30 μ m.Thermal conductivity 〉=the 15W/Kcm of described pure diamond lamella, resistivity are 10 13～10 15Ω cm.
The preparation method of absorbed radiation composite diamond heat-exchanging diaphragm of the present invention may further comprise the steps:
A. in MW-PCVD microwave plasma CVD system equipment, with H 2And CH 4Make stock media, the metal molybdenum sheet is made substrate, carry out a chemical vapor deposition in following process conditions and prepare water white heat sink diamond chip:
H 2Flow is 200sccm, CH 4Flow is 1～3sccm, and microwave power is 3.8～4.2KW, and deposition pressure is 11～17KPa, and underlayer temperature is 750～950 ℃.About 1～3 μ m/h of growth rate.Thermal conductivity 〉=the 15W/Kcm of the diamond film of preparation, its resistivity is 10 13～10 15Ω cm, 0.4mm is thick, is colourless transparent film.
B. because the difference on the thermal expansivity that existence is bigger between metal molybdenum and the adamas, therefore the adamas diaphragm is easy to break away from automatically from substrate in cooling procedure, the heat sink diamond chip that a step is obtained carries out grinding and polishing, making one side surface roughness is 50～100nm, and the opposite side surfaceness is less than 40nm;
C. the heat sink diamond chip after will polishing cuts into required geomery;
D. the heat sink diamond chip after the cutting is carried out following surface preparation, soak more than 30 minutes with chromic acid solution earlier, use deionized water rinsing then, impurity and grease on heat sink have promptly been removed, be placed in the acetone soln ultrasonic cleaning again 15 minutes, placed the alcoholic solution ultrasonic cleaning again 15 minutes; Place deionized water for ultrasonic to clean at last 15 minutes, place on 150 ℃ of hot plates and dry;
E. on being the side of 50～100nm, the surfaceness of the heat sink diamond chip after the above-mentioned processing carries out the black diamond film of secondary chemical vapor deposition graphitiferous phase carbon, the diamond heat-sink sheet that is about to after the above-mentioned processing is placed on the sample bench of HC-PCVD hot cathode DC plasma and chemical gas-phase deposition system, carry out the black diamond depositing of thin film in following process conditions: hydrogen flowing quantity is 160sccm, the flow of methane is 15～5sccm, temperature in the settling chamber is 750～850 ℃, air pressure in the settling chamber is 125～135Torr, apply bias voltage 700～750V, electric current is 8.2～8.8A.
Metal molybdenum substrate described in the step a carries out pre-service: ground 15 minutes sonicated 10 minutes in acetone soln then, sonicated 10 minutes in alcoholic solution again with diamond paste in the following manner before the heat sink diamond chip of vapour deposition.
The grinding and polishing of the described heat sink diamond chip of step b is to adopt the surface chemistry etching earlier, and mechanical lapping polishing then is to the diamond film twin polishing.
The described heat sink diamond chip cutting of step c is to adopt the YAG laser cutting technique that diamond chip is carried out the high precision cutting.
The described chromic acid solution of steps d is Cr 2O 3Be dissolved in resulting saturated solution behind the concentrated sulphuric acid.
Described in the step e when secondary chemical vapor deposition black diamond film, before deposition, the heating source tantalum electrode in the HC-PCVD hot cathode DC plasma and chemical gas-phase deposition system is carried out the surface finish purified treatment, and with hydrogen and acetone heating pretreatment 30 minutes, make tantalum electrode surface removal oxide layer impurity, and at tantalum electrode surface formation one deck tantalum carbide overlayer, with the volatilization of tantalum in the process of inhibition and the introducing of minimizing metallic impurity.
The present invention has the composite diamond heat-exchanging diaphragm of the black material layer of heat sink material layer and absorbed radiation when adopting the secondary chemical gaseous phase depositing process to make, have that thermal shock resistance is strong, absorptivity is stablized unconverted advantage after the raying of absorbed radiation material layer, absorptivity to radiation is higher, reach 99%～99.2%, be specially adapted to the heat exchange device of absolute measuring bolometer, the measuring accuracy and the sensitivity of radiometer have been improved, shorten measuring period, improved the adaptability of absolute measuring bolometer condition of work on satellite greatly.
Description of drawings
Fig. 1 is the configuration of surface of the black diamond film of absorbed radiation composite diamond heat-exchanging diaphragm of the present invention.
Embodiment
The present invention is further elaborated by the following examples.
Embodiment 1
The preparation method of absorbed radiation composite diamond heat-exchanging diaphragm, specific embodiment is as follows:
A. heat sink diamond chip of chemical vapor deposition.
Adopt the heat sink diamond chip of MW-PCVD microwave plasma CVD systems produce, with H 2And CH 4Make stock media, the metal molybdenum sheet is made substrate, it belongs to the electrodless discharge method, than obtaining the high high-purity transparent diamond film of quality under the infrabar.Method of processing a substrate is to adopt diamond paste to grind 15 minutes, uses acetone, each sonicated of alcohol 10 minutes then.Hydrogen and methane all are by mass flowmeter Control Flow, H 2Flow is 200sccm, CH 4Flow is 3sccm, and microwave power is 4.2KW, and deposition pressure is 11KPa, and underlayer temperature is 850 ℃, the about 3 μ m/h of growth rate.The thermal conductivity of the adamas diaphragm of preparation is 15W/Kcm, and its resistivity is 10 13Ω cm, 0.4mm is thick, is colourless transparent film.
B. the heat sink diamond chip of grinding and polishing.Owing to there is the difference on the bigger thermal expansivity between metal molybdenum and the adamas, therefore diamond film is easy to break away from automatically from substrate in cooling procedure, then the thick diamond film of 0.4mm with the MW-PCVD preparation is adopted the surface chemistry etching earlier, the method that combines of mechanical lapping polishing (diamond film mirror polish machine) is to the diamond film twin polishing then, obtaining adamas diaphragm thickness is 0.35mm, one side surface roughness of diamond chip is 50～100nm (rms), and the opposite side surfaceness is less than 40nm (rms).
C. cut heat sink diamond chip.Adopt the YAG cut to realize the high precision cutting of diamond film, scale error obtains the heat sink diamond chip of 1.5 * 12 * 0.35mm at last between 0.05～0.1mm.
D. the surface preparation of heat sink diamond chip.Be heated to 300 ℃ with the chromic acid immersion earlier, be 50 minutes heat time heating time, and used chromic acid is Cr 2O 3Be dissolved in resulting saturated solution behind the concentrated sulphuric acid; Use a large amount of deionized water rinsings immediately, removed impurity and grease on heat sink like this; Placed the acetone soln ultrasonic cleaning then 15 minutes; Placed the alcohol ultrasonic cleaning again 15 minutes; Place deionized water for ultrasonic to clean at last 15 minutes, place on 150 ℃ of hot plates and dry.
E. secondary chemical vapor deposition black diamond film.Above-mentioned treated heat sink diamond chip is placed on the sample bench of HC-PCVD hot cathode DC plasma and chemical gas-phase deposition system, is to carry out the black diamond depositing of thin film on the side surface of 50～100nm in roughness.Before the deposition heating source tantalum electrode in the HC-PCVD hot cathode DC plasma and chemical gas-phase deposition system is carried out the surface finish purified treatment, and with hydrogen and acetone heating pretreatment 30 minutes, make tantalum electrode surface removal oxide layer impurity, and at tantalum electrode surface formation one deck tantalum carbide overlayer, with the volatilization of tantalum in the process of inhibition and the introducing of minimizing impurity.The technological parameter of secondary chemical vapor deposition black diamond film is: the flow of hydrogen and methane is respectively: H 2=160sccm, CH 4=5sccm; Temperature in the settling chamber is 700 ℃; Air pressure in the settling chamber is 130Torr; Apply bias voltage 700V, electric current is 8.2A; Sedimentation time is 2 hours.Obtaining thickness is the black diamond rete of 20 μ m.This film is the black diamond rete that contains the graphite phase, and its thermal conductivity is that 6W/Kcm, resistivity are 10 8Ω cm, this film surface has micro-nano concaveconvex structure, and roughness is 15 μ m, the adamantine crystal grain diameter of this rete is 1nm～10 μ m, intercrystalline forms pit, forms the upright micro-nano size diamond crystals array based on (111) crystal face around pit, forms light localization film.
Promptly obtain the absorbed radiation composite diamond heat-exchanging diaphragm that is composited by black diamond rete that contains the graphite phase and pure diamond lamella.
Embodiment 2
Prepare the absorbed radiation composite diamond heat-exchanging diaphragm by embodiment 1 same method step, its difference only is:
The deposition process conditions of (1) heat sink diamond chip of chemical vapor deposition is: H 2Flow is 200sccm, CH 4Flow is 1sccm, and microwave power is 3.8KW, and deposition pressure is 17KPa, and underlayer temperature is 950 ℃, the about 1 μ m/h of growth rate.The thermal conductivity of the adamas diaphragm that is obtained is that 18W/Kcm, resistivity are 10 15Ω cm.
(2) deposition process conditions of secondary chemical vapor deposition black diamond rete is: the flow of hydrogen and methane is respectively: H 2=160sccm, CH 4=15sccm; Temperature in the settling chamber is 750 ℃; Air pressure in the settling chamber is 135Torr; Apply bias voltage 750V, electric current is 8.8A; Sedimentation time 3 hours.The thermal conductivity of the black diamond rete that obtains is that 8W/Kcm, its resistivity are 10 12Ω cm, roughness is 10 μ m, and the crystal grain diameter of black diamond is 10nm～10 μ m, and thickness is 100nm～30 μ m.
Embodiment 3
Prepare the absorbed radiation composite diamond heat-exchanging diaphragm by embodiment 1 same method step, its difference only is:
The deposition process conditions of (1) heat sink diamond chip of chemical vapor deposition is: H 2Flow is 200sccm, CH 4Flow is 2sccm, and microwave power is 4KW, and deposition pressure is 13KPa, and underlayer temperature is 750 ℃, the about 2 μ m/h of growth rate.The thermal conductivity of the diamond chip of preparation is 17W/Kcm, and its resistivity is 10 14Ω cm.
(2) deposition process conditions of secondary chemical vapor deposition black diamond rete is: the flow of hydrogen and methane is respectively: H 2=160sccm, CH 4=10sccm; Temperature in the settling chamber is 850 ℃; Air pressure in the settling chamber is 125Torr; Sedimentation time is 2 hours.The thermal conductivity of the black diamond rete that obtains is that 7W/Kcm, resistivity are 10 11Ω cm, roughness is 12 μ m, and the crystal grain diameter of black diamond is 10nm～10 μ m, and thickness is 100nm～25 μ m.

Claims (7)

1.一种吸收辐射复合金刚石热交换膜片，其特征在于，是由含有石墨相的黑色金刚石膜层与纯金刚石片层复合而成，纯金刚石片层作为热沉材料，含有石墨相的黑色金刚石膜层作为光辐射吸收材料；所述含有石墨相的黑色金刚石膜层是由石墨相碳原子均匀分布在金刚石晶体中形成，该膜层的热导率为6～8W/K·cm、电阻率为108～1012Ω·cm，该膜层表面具有微纳米凹凸结构，粗糙度为5nm～15μm；所述纯金刚石膜片层的热导率≥15W/K·cm、电阻率为1013～1015Ω·cm。1. A radiation-absorbing composite diamond heat exchange diaphragm is characterized in that it is composed of a black diamond film layer containing a graphite phase and a pure diamond sheet, and the pure diamond sheet is used as a heat sink material, and the black diamond layer containing a graphite phase is formed. The diamond film layer is used as light radiation absorbing material; the black diamond film layer containing graphite phase is formed by graphite phase carbon atoms evenly distributed in the diamond crystal, the thermal conductivity of the film layer is 6～8W/K cm, the resistance The ratio is 10 8 to 10 12 Ω·cm, and the surface of the film layer has a micro-nano concave-convex structure with a roughness of 5nm to 15μm; the thermal conductivity of the pure diamond diaphragm layer is ≥15W/K·cm, and the resistivity is 10 13-10 15 Ω·cm. 2.一种制备权利要求1所述的热交换膜片的方法，其特征包括以下步骤：2. A method for preparing the heat exchange membrane according to claim 1, characterized in that it comprises the following steps: a.在MW-PCVD微波等离子体化学气相沉积系统设备中，以H2和CH4作原料介质、金属钼片作衬底，在以下工艺条件下进行一次化学气相沉积制备无色透明的热沉金刚石片：H2流量为200sccm，CH4流量为1～3sccm，微波功率为3.8～4.2KW，沉积气压为11～17KPa，衬底温度为750～950℃；a. In the MW-PCVD microwave plasma chemical vapor deposition system equipment, H 2 and CH 4 are used as the raw material medium, and the metal molybdenum sheet is used as the substrate, and a colorless and transparent heat sink is prepared by a chemical vapor deposition under the following process conditions Diamond wafer: H 2 flow rate is 200 sccm, CH 4 flow rate is 1-3 sccm, microwave power is 3.8-4.2KW, deposition pressure is 11-17KPa, substrate temperature is 750-950°C; b.将a步骤获得的热沉金刚石片进行研磨抛光，使其一侧表面粗糙度为50～100nm，另一侧表面粗糙度为＜40nm；b. Grinding and polishing the heat sink diamond sheet obtained in step a, so that the surface roughness of one side is 50-100nm, and the surface roughness of the other side is <40nm; c.将抛光后的热沉金刚石片切割成所需的形状尺寸；c. Cut the polished heat sink diamond sheet into the desired shape and size; d.对切割后的热沉金刚石片进行下述表面预处理，先用铬酸溶液浸泡30分钟以上，然后用去离子水冲洗，即去除了热沉片上的杂质和油脂，再将其置于丙酮溶液中超声清洗15分钟，再置于酒精溶液中超声清洗15分钟；最后置于去离子水中超声清洗15分钟，置于150℃热板上烘干；d. Carry out the following surface pretreatment on the heat sink diamond sheet after cutting, first soak it with chromic acid solution for more than 30 minutes, then rinse it with deionized water, that is, remove the impurities and grease on the heat sink sheet, and then place it in Ultrasonic cleaning in acetone solution for 15 minutes, then ultrasonic cleaning in alcohol solution for 15 minutes; finally ultrasonic cleaning in deionized water for 15 minutes, and drying on a hot plate at 150°C; e.在上述处理后的热沉金刚石片的表面粗糙度为50～100nm的一侧面上进行二次化学气相沉积含石墨相碳的黑色金刚石膜，即将上述处理后的热沉金刚石片放置在HC-PCVD热阴极直流等离子体化学气相沉积系统的试样台上在以下工艺条件下进行黑色金刚石薄膜的沉积：氢气流量为160sccm、甲烷的流量为15～5sccm，沉积室内的温度为750～850℃、沉积室内的气压为125～135Torr，施加偏压700～750V，电流为8.2～8.8A。e. Carry out secondary chemical vapor deposition of a black diamond film containing graphite phase carbon on the side surface of the heat sink diamond sheet after the above treatment with a surface roughness of 50-100 nm, that is, place the heat sink diamond sheet after the above treatment on the HC -On the sample stage of the PCVD hot cathode direct current plasma chemical vapor deposition system, the black diamond film is deposited under the following process conditions: the flow rate of hydrogen gas is 160 sccm, the flow rate of methane is 15-5 sccm, and the temperature in the deposition chamber is 750-850°C 1. The gas pressure in the deposition chamber is 125-135 Torr, the applied bias voltage is 700-750V, and the current is 8.2-8.8A. 3.根据权利要求2所述的制备权利要求1所述的热交换膜片的方法，其特征在于步骤a所述的金属钼衬底，在气相沉积热沉金刚石片前按以下方式进行预处理：用金刚石研磨膏研磨15分钟，然后在丙酮溶液中超声处理10分钟，再在酒精溶液中超声处理10分钟。3. the method for preparing the heat exchange membrane according to claim 1 according to claim 2, characterized in that the metal molybdenum substrate described in step a is pretreated in the following manner before the vapor deposition heat sink diamond sheet : Grind with diamond paste for 15 minutes, then sonicate in acetone solution for 10 minutes, then in alcohol solution for 10 minutes. 4.根据权利要求2所述的制备权利要求1所述的热交换膜片的方法，其特征在于步骤b所述的热沉金刚石片的研磨抛光是先采用表面化学刻蚀，然后机械研磨抛光，对金刚石膜双面抛光。4. The method for preparing the heat exchange membrane according to claim 1, characterized in that the grinding and polishing of the heat sink diamond sheet described in step b is to first adopt surface chemical etching, and then mechanical grinding and polishing , polishing the diamond film on both sides. 5.根据权利要求2所述的制备权利要求1所述的热交换膜片的方法，其特征在于步骤c所述的热沉金刚石片切割是采用YAG激光切割技术对金刚石片进行高精度切割。5. The method for preparing the heat exchange membrane according to claim 1, wherein the cutting of the heat sink diamond sheet in step c is to use YAG laser cutting technology to cut the diamond sheet with high precision. 6.根据权利要求2所述的制备权利要求1所述的热交换膜片的方法，其特征在于步骤d所述的铬酸溶液为Cr2O3溶于浓硫酸后所得到的饱和溶液。6. The method for preparing the heat exchange membrane according to claim 1, characterized in that the chromic acid solution in step d is a saturated solution obtained by dissolving Cr2O3 in concentrated sulfuric acid. 7.根据权利要求2所述的制备权利要求1所述的热交换膜片的方法，其特征在于步骤e中所述在二次化学气相沉积黑色金刚石膜时，在沉积前对HC-PCVD热阴极直流等离子体化学气相沉积系统中的加热源钽电极进行表面打磨净化处理，并用氢气和丙酮加热预处理30分钟，使钽电极表面去除氧化层杂质，并在钽电极表面形成一层碳化钽覆盖层，以抑制过程中钽的挥发和减少金属杂质的引入。7. the method for preparing the heat exchange membrane described in claim 1 according to claim 2, is characterized in that described in the step e when secondary chemical vapor deposition black diamond film, before depositing to HC-PCVD heat The heating source tantalum electrode in the cathodic direct current plasma chemical vapor deposition system is subjected to surface grinding and purification treatment, and pre-treated with hydrogen and acetone for 30 minutes to remove oxide layer impurities on the surface of the tantalum electrode and form a layer of tantalum carbide on the surface of the tantalum electrode. layer to suppress the volatilization of tantalum and reduce the introduction of metal impurities during the process.
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CN102538958B (en) * 2011-12-23 2013-09-25 中国科学院长春光学精密机械与物理研究所 High-absorptivity radiation absorption chamber
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