CN104553102A - Ultrahigh-temperature gradient heat insulation material and preparation method thereof - Google Patents
Ultrahigh-temperature gradient heat insulation material and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种超高温梯度隔热材料及其制备方法,其中超高温梯度隔热材料包括:超高温隔热材料层,其位于高温一侧;相变吸热隔热材料层,位于超高温隔热材料层的外侧;中温隔热层,位于相变吸热隔热材料层的外侧;低温隔热层,位于中温隔热层的外侧;辐射屏蔽层,分别设于超高温隔热材料层、相变吸热隔热材料层、中温隔热层和低温隔热层相邻两层之间以及设于低温隔热层的外侧,所述辐射屏蔽层用于阻挡红外辐射;上述各层复合为一体。本发明的超高温梯度隔热材料具有耐超高温,使用时间长的特点。
The invention discloses an ultra-high temperature gradient heat insulation material and a preparation method thereof, wherein the ultra high temperature gradient heat insulation material comprises: an ultra high temperature heat insulation material layer located on the high temperature side; a phase change heat absorption heat insulation material layer located on the ultra high temperature side The outer side of the high temperature heat insulation layer; the medium temperature heat insulation layer is located outside the phase change heat absorption heat insulation material layer; the low temperature heat insulation layer is located outside the medium temperature heat insulation layer; the radiation shielding layer is respectively arranged on the ultra high temperature heat insulation material layer Layer, phase-change heat-absorbing and heat-insulating material layer, medium-temperature heat-insulating layer and low-temperature heat-insulating layer between two adjacent layers and outside the low-temperature heat-insulating layer, the radiation shielding layer is used to block infrared radiation; the above-mentioned layers Composite as one. The ultra-high temperature gradient thermal insulation material of the present invention has the characteristics of ultra-high temperature resistance and long service life.
Description
技术领域technical field
本发明涉及隔热材料技术领域,尤其涉及一种超高温梯度隔热材料及其制备方法。The invention relates to the technical field of thermal insulation materials, in particular to an ultra-high temperature gradient thermal insulation material and a preparation method thereof.
背景技术Background technique
随着航空航天技术的迅猛发展,热防护系统和材料已成为制约飞行器研发能否成功的最重要的关键技术之一。随着飞行马赫数的不断提高,对热防护材料的使用温度的要求越来越高,工作时,燃烧室外壁的温度高达2000K以上,为了保护发动机金属壳体及其周边的电子设备,同时减少热量的散耗及其带来的明显的红外信号特征,燃烧室外壁采用超高温隔热材料进行热防护。With the rapid development of aerospace technology, thermal protection systems and materials have become one of the most important key technologies that restrict the success of aircraft research and development. With the continuous improvement of the flight Mach number, the requirements for the temperature of the thermal protection material are getting higher and higher. During operation, the temperature of the outer wall of the combustion chamber is as high as 2000K or more. In order to protect the metal shell of the engine and its surrounding electronic equipment, reduce Heat dissipation and the obvious infrared signal characteristics brought by it, the outer wall of the combustion chamber is protected by ultra-high temperature heat insulation materials.
现有的火箭发动机所用耐热防护材料,一般为石墨布/酚醛、碳布/酚醛、高硅氧布/酚醛、玻璃布/酚醛,绝热层材料常为玻璃纤维、高硅氧或石棉增强的酚醛或环氧树脂,及石棉或二氧化硅填充的丁腈橡胶和三元已丙橡胶等。但此类耐热防护材料耐温较低。The heat-resistant protective materials used in existing rocket engines are generally graphite cloth/phenolic, carbon cloth/phenolic, high-silica cloth/phenolic, glass cloth/phenolic, and the insulation layer material is often glass fiber, high-silica or asbestos reinforced Phenolic or epoxy resin, and asbestos or silica-filled nitrile rubber and EPDM rubber, etc. However, such heat-resistant protective materials have low temperature resistance.
随着航空航天技术的发展,耐温更高等级的热防护材料逐渐开发出来,其中ZrC/气凝胶和树脂聚合物叠层复合材料耐温较高,但是该材料具有长时间使用隔热性能下降的缺点。还有采用了氧化锆类材料,但是该材料具有高温下辐射传热较严重的缺点。With the development of aerospace technology, thermal protection materials with higher temperature resistance are gradually developed, among which ZrC/aerogel and resin polymer laminated composite materials have higher temperature resistance, but the material has long-term heat insulation performance Downsides. Zirconia-based materials are also used, but this material has the disadvantage of relatively serious radiation heat transfer at high temperatures.
由此可见,现有的热防护材料耐温低,约为1800-2000K,使用时间短,约几十秒到400秒左右,已不能满足高速飞行器高马赫数、长时间的飞行需要。It can be seen that the existing thermal protection materials have low temperature resistance, about 1800-2000K, and short service time, about tens of seconds to about 400 seconds, which can no longer meet the high Mach number and long-term flight needs of high-speed aircraft.
发明内容Contents of the invention
有鉴于此,本发明实施例提供一种超高温梯度隔热材料及其制备方法,主要目的是提高耐温温度,延长使用时间。In view of this, an embodiment of the present invention provides an ultra-high temperature gradient thermal insulation material and a preparation method thereof, the main purpose of which is to increase the temperature resistance and prolong the use time.
为达到上述目的,本发明主要提供如下技术方案:In order to achieve the above object, the present invention mainly provides the following technical solutions:
一方面,本发明实施例提供了一种超高温梯度隔热材料,包括:On the one hand, an embodiment of the present invention provides an ultra-high temperature gradient thermal insulation material, including:
超高温隔热材料层,其位于高温一侧;Ultra-high temperature insulation material layer, which is located on the high temperature side;
相变吸热隔热材料层,位于超高温隔热材料层的外侧;The phase-change heat-absorbing and heat-insulating material layer is located outside the ultra-high temperature heat-insulating material layer;
中温隔热层,位于相变吸热隔热材料层的外侧;The medium-temperature heat-insulating layer is located outside the phase-change heat-absorbing heat-insulating material layer;
低温隔热层,位于中温隔热层的外侧;The low temperature insulation layer is located outside the medium temperature insulation layer;
辐射屏蔽层,分别设于超高温隔热材料层、相变吸热隔热材料层、中温隔热层和低温隔热层相邻两层之间以及设于低温隔热层的外侧,所述辐射屏蔽层用于阻挡红外辐射;The radiation shielding layer is respectively arranged between the ultra-high temperature heat insulating material layer, the phase change heat absorbing heat insulating material layer, the medium temperature heat insulating layer and the low temperature heat insulating layer and the outer side of the low temperature heat insulating layer. The radiation shield is used to block infrared radiation;
上述各层复合为一体。The above layers are combined into one.
作为优选,所述超高温隔热材料层的材料为碳纤维/氧化锆纤维超高温隔热材料、氧化锆纤维超高温隔热材料、碳纤维毡或超细孔炭材料。Preferably, the material of the ultra-high temperature insulation material layer is carbon fiber/zirconia fiber ultra-high temperature insulation material, zirconia fiber ultra-high temperature insulation material, carbon fiber felt or ultra-fine porous carbon material.
作为优选,所述相变吸热隔热材料层的材料为氟化镍高温相变材料、氟化镁相变材料或碳酸盐中温相变材料。Preferably, the material of the phase-change heat-absorbing and heat-insulating material layer is nickel fluoride high-temperature phase-change material, magnesium fluoride phase-change material or carbonate medium-temperature phase-change material.
作为优选,所述中温隔热层的材料为氧化铝纤维隔热材料、莫来石纤维隔热材料、石英纤维隔热材料、硅酸钙隔热材料或高硅氧纤维隔热材料。Preferably, the material of the medium-temperature heat insulation layer is alumina fiber heat insulation material, mullite fiber heat insulation material, quartz fiber heat insulation material, calcium silicate heat insulation material or high silica fiber heat insulation material.
作为优选,所述低温隔热层的材料为氧化硅气凝胶隔热材料、硅酸铝纤维隔热材料、岩棉或超细玻璃棉。Preferably, the material of the low-temperature heat insulation layer is silica airgel heat insulation material, aluminum silicate fiber heat insulation material, rock wool or ultra-fine glass wool.
作为优选,所述辐射屏蔽层的材料为钼箔、铝箔、石墨纸或金箔。Preferably, the material of the radiation shielding layer is molybdenum foil, aluminum foil, graphite paper or gold foil.
作为优选,所述超高温隔热材料层厚度为2-20mm;所述相变吸热隔热材料层的厚度为2-10mm;所述中温隔热层的厚度为2-30mm;所述低温隔热层的厚度为2-40mm;所述辐射屏蔽层的厚度为0.01-0.5mm。Preferably, the thickness of the ultra-high temperature heat insulation material layer is 2-20mm; the thickness of the phase change heat absorption heat insulation material layer is 2-10mm; the thickness of the medium temperature heat insulation layer is 2-30mm; the low temperature The thickness of the heat insulating layer is 2-40mm; the thickness of the radiation shielding layer is 0.01-0.5mm.
作为优选,所述各层之间通过胶黏剂粘合,然后通过压力成形和高温处理复合为一体。Preferably, the layers are bonded with an adhesive, and then composited into one through pressure forming and high-temperature treatment.
作为优选,所述胶黏剂选自磷酸铝系胶黏剂、磷酸铬铝系高温粘结剂、铝溶胶系胶黏剂和硅溶胶系中温粘结剂。Preferably, the adhesive is selected from aluminum phosphate-based adhesives, chromium-aluminum phosphate-based high-temperature adhesives, aluminum sol-based adhesives and silica sol-based medium-temperature adhesives.
作为优选,所述超高温隔热材料层至相变吸热隔热层之间采用高温粘结剂连接;相变吸热隔热层至最外侧的辐射屏蔽层之间采用中温粘结剂粘结。Preferably, a high temperature adhesive is used to connect the ultra-high temperature heat insulating material layer to the phase change heat absorbing heat insulating layer; a medium temperature adhesive is used to bond the phase change heat absorbing heat insulating layer to the outermost radiation shielding layer. Knot.
另一方面,本发明实施例提供了一种上述任一种超高温梯度隔热材料的制备方法,包括如下步骤:On the other hand, an embodiment of the present invention provides a method for preparing any one of the above ultra-high temperature gradient heat insulation materials, including the following steps:
根据应用环境,利用传热理论确定各隔热材料层的具体材料和厚度;According to the application environment, use the heat transfer theory to determine the specific material and thickness of each insulation material layer;
根据确定的材料制备相应厚度的各隔热材料层;According to the determined material, each insulation material layer is prepared with a corresponding thickness;
将各隔热材料层采用胶黏剂连接起来,然后通过压力成形和高温处理复合为一体,得到超高温组合隔热材料。The heat insulation material layers are connected by adhesive, and then compounded into one through pressure forming and high temperature treatment to obtain an ultra-high temperature combined heat insulation material.
作为优选,各隔热材料层复合为一体的步骤如下:Preferably, the steps of compounding each thermal insulation material layer as a whole are as follows:
采用刷涂或喷涂,在各层之间涂覆粘结剂;Apply adhesive between layers by brushing or spraying;
压力成形的压力范围为0.1MPa~5MPa之间,高温处理的温度在50℃~400℃之间,处理时间为2h~24h。The pressure range of pressure forming is between 0.1MPa and 5MPa, the temperature of high temperature treatment is between 50°C and 400°C, and the treatment time is between 2h and 24h.
与现有技术相比,本发明的有益效果在于:Compared with prior art, the beneficial effect of the present invention is:
本发明实施例的超高温梯度隔热材料耐温2300-2500K。防护使用时间可达2500秒。本发明生产周期短,约2~3周即可完成选材、制备及成型。本发明实施例的超高温梯度隔热材料在超高温条件下原材料的选择范围更广。The ultra-high temperature gradient heat insulation material of the embodiment of the present invention has a temperature resistance of 2300-2500K. The protective use time can reach 2500 seconds. The production cycle of the invention is short, and material selection, preparation and molding can be completed in about 2 to 3 weeks. The ultra-high temperature gradient thermal insulation material of the embodiment of the present invention has a wider selection range of raw materials under ultra-high temperature conditions.
附图说明Description of drawings
图1是本发明实施例的超高温梯度隔热材料的结构示意图。Fig. 1 is a schematic structural diagram of an ultra-high temperature gradient thermal insulation material according to an embodiment of the present invention.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步详细描述,但不作为对本发明的限定。在下述说明中,不同的“一实施例”或“实施例”指的不一定是同一实施例。此外,一或多个实施例中的特定特征、结构、或特点可由任何合适形式组合。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments, but not as a limitation of the present invention. In the following description, different "one embodiment" or "embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
图1是本发明实施例的超高温梯度隔热材料的结构示意图。如图1所示,超高温梯度隔热材料,结构如下:Fig. 1 is a schematic structural diagram of an ultra-high temperature gradient thermal insulation material according to an embodiment of the present invention. As shown in Figure 1, the ultra-high temperature gradient heat insulation material has the following structure:
超高温隔热材料层1,其位于高温一侧;Ultra-high temperature insulation material layer 1, which is located on the high temperature side;
相变吸热隔热材料层2,位于超高温隔热材料层1的外侧;The phase-change heat-absorbing and heat-insulating material layer 2 is located outside the ultra-high-temperature heat-insulating material layer 1;
中温隔热层3,位于相变吸热隔热材料层2的外侧;The medium-temperature heat-insulation layer 3 is located outside the phase-change heat-absorbing heat-insulation material layer 2;
低温隔热层4,位于中温隔热层3的外侧;The low temperature heat insulation layer 4 is located outside the medium temperature heat insulation layer 3;
辐射屏蔽层5,分别设于超高温隔热材料层1、相变吸热隔热材料层2、中温隔热层3和低温隔热层4相邻两层之间,以及设于低温隔热层4的外侧,辐射屏蔽层5用于阻挡红外辐射;The radiation shielding layer 5 is respectively arranged between two adjacent layers of the ultra-high temperature heat insulating material layer 1, the phase change heat absorbing heat insulating material layer 2, the medium temperature heat insulating layer 3 and the low temperature heat insulating layer 4, and the low temperature heat insulating layer On the outside of layer 4, radiation shielding layer 5 is used to block infrared radiation;
上述各层复合为一体。The above layers are combined into one.
本发明实施例的超高温组合隔热材料考虑到将内部的高于2200℃的高温阻隔到外表面温度低温的要求,将接触高温端的一侧设置为能够经受住2200℃的高温的超高温隔热材料层,使其外侧的温度能够降至1000℃以下。通过在超高温隔热材料层的外侧设置相变吸热隔热材料层使温度迅速降低,这样再设置较低耐温的隔热材料层即可实现对超高温的隔热效果。并且通过设置辐射屏蔽层有效阻隔红外辐射。本发明实施例中将多个隔热材料层复合为一体形成新的隔热材料,通过各层不同的耐温性能和导热率,在整体上达到既耐高温,又具有低的平均导热率,满足整体隔热要求。其中超高温隔热材料层耐温达到3000℃;相变吸热隔热材料层耐温在2000℃以下即可;中温隔热层耐温在2000℃以下;低温隔热层耐温在1400℃以下。这样,外层的隔热材料层就具有更多的可选择性。The ultra-high temperature composite heat insulation material of the embodiment of the present invention considers the requirement of blocking the internal high temperature higher than 2200°C to the outer surface temperature of low temperature, and the side contacting the high temperature end is set as an ultra-high temperature insulation material capable of withstanding the high temperature of 2200°C. The thermal material layer enables the temperature on the outside to drop below 1000°C. By arranging a phase-change heat-absorbing and heat-insulating material layer outside the ultra-high-temperature heat-insulating material layer, the temperature is rapidly lowered, and then setting a lower temperature-resistant heat-insulating material layer can realize the heat-insulating effect on ultra-high temperature. And the infrared radiation is effectively blocked by setting the radiation shielding layer. In the embodiment of the present invention, multiple thermal insulation material layers are combined to form a new thermal insulation material. Through the different temperature resistance and thermal conductivity of each layer, it can achieve high temperature resistance and low average thermal conductivity as a whole. Meet the overall heat insulation requirements. Among them, the temperature resistance of the ultra-high temperature heat insulation material layer can reach 3000 °C; the temperature resistance of the phase change heat absorption heat insulation material layer is below 2000 °C; the temperature resistance of the medium temperature heat insulation layer is below 2000 °C; the temperature resistance of the low temperature heat insulation layer is 1400 °C the following. Like this, the thermal insulation material layer of outer layer just has more selectivity.
实施例1Example 1
根据应用环境,利用传热理论确定各隔热材料层的具体材料和厚度;根据确定的材料制备相应厚度的各隔热材料层;将各隔热材料层采用胶黏剂连接起来,得到超高温组合隔热材料。According to the application environment, use the heat transfer theory to determine the specific material and thickness of each heat insulation material layer; prepare each heat insulation material layer with a corresponding thickness according to the determined material; connect each heat insulation material layer with an adhesive to obtain a super high temperature Combined insulation.
通过上述步骤确定的超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为碳纤维/氧化锆纤维超高温隔热材料,厚度为2mm;相变吸热隔热材料层采用氟化镁相变材料,厚度为2mm;中温隔热层所用材料为氧化铝纤维隔热材料,厚度为10mm;低温隔热层所用材料为氧化硅气凝胶隔热材料,厚度为15mm;辐射屏蔽层所用材料为钼箔,厚度为0.02mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用铝溶胶低温粘结剂粘结。其中粘结剂采用刷涂或喷涂。采用加压和高温处理工艺将材料复合为一体,然后在0.1MPa~5MPa的压力下压力成形,成形后在50℃~400℃的温度下进行高温处理,处理时间为2h~24h。The material and thickness of each layer of the ultra-high temperature composite heat insulation material determined through the above steps are as follows: the material used for the ultra-high temperature heat insulation material layer is carbon fiber/zirconia fiber ultra-high temperature heat insulation material with a thickness of 2mm; phase change heat absorption and heat insulation The material layer is made of magnesium fluoride phase-change material with a thickness of 2mm; the material used for the medium temperature insulation layer is alumina fiber insulation material with a thickness of 10mm; the material used for the low temperature insulation layer is silica airgel insulation material with a thickness of 15mm; the radiation shielding layer is made of molybdenum foil with a thickness of 0.02mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Aluminum sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer. The binder is applied by brushing or spraying. The material is compounded by pressure and high-temperature treatment process, and then press-formed under a pressure of 0.1MPa-5MPa. After forming, high-temperature treatment is carried out at a temperature of 50°C-400°C, and the treatment time is 2h-24h.
实施例2Example 2
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层的厚度为2mm;相变吸热隔热材料层的厚度为10mm;中温隔热层的厚度为30mm;低温隔热层所用材料为硅酸铝纤维隔热材料,厚度为40mm;辐射屏蔽层所用材料为铝箔,厚度为0.01mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用硅溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the materials and thicknesses used for each layer of the ultra-high temperature composite heat insulation material are as follows: the thickness of the ultra-high temperature heat insulation material layer is 2mm; the thickness of the phase change heat absorption heat insulation material layer is 10mm; The thickness of the heat insulation layer is 30mm; the material used for the low temperature heat insulation layer is aluminum silicate fiber heat insulation material with a thickness of 40mm; the material used for the radiation shielding layer is aluminum foil with a thickness of 0.01mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Silica sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例3Example 3
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为氧化锆纤维超高温隔热材料,厚度为2mm;相变吸热隔热材料层采用氟化镍相变材料,厚度为10mm;中温隔热层所用材料为莫来石纤维隔热材料,厚度为2mm;低温隔热层所用材料为氧化硅气凝胶隔热材料,厚度为2mm;辐射屏蔽层所用材料为金箔,厚度为0.1mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用铝溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is a zirconia fiber ultra-high temperature heat insulation material with a thickness of 2 mm; The heat insulation material layer is made of nickel fluoride phase change material with a thickness of 10mm; the material used for the medium temperature heat insulation layer is mullite fiber heat insulation material with a thickness of 2mm; the material used for the low temperature heat insulation layer is silica airgel heat insulation Material, the thickness is 2mm; the material used for the radiation shielding layer is gold foil, the thickness is 0.1mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Aluminum sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例4Example 4
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为碳纤维/氧化锆纤维超高温隔热材料,厚度为10mm;相变吸热隔热材料层采用氟化镁相变材料,厚度为8mm;中温隔热层所用材料为氧化铝纤维隔热材料,厚度为10mm;低温隔热层所用材料为氧化硅气凝胶隔热材料,厚度为15mm;辐射屏蔽层所用材料为钼箔,厚度为0.025mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用铝溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is a carbon fiber/zirconia fiber ultra-high temperature heat insulation material with a thickness of 10 mm; The variable heat-absorbing heat insulation layer is made of magnesium fluoride phase change material with a thickness of 8mm; the material used for the medium temperature heat insulation layer is alumina fiber heat insulation material with a thickness of 10mm; the material used for the low temperature heat insulation layer is silica airgel insulation Thermal material with a thickness of 15mm; the material used for the radiation shielding layer is molybdenum foil with a thickness of 0.025mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Aluminum sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例5Example 5
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为碳纤维毡,厚度为10mm;相变吸热隔热材料层采用碳酸盐相变材料,厚度为10mm;中温隔热层所用材料为石英纤维隔热材料,厚度为10mm;低温隔热层所用材料为岩棉隔热材料,厚度为2mm;辐射屏蔽层所用材料为石墨纸,厚度为0.2mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用硅溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is carbon fiber felt with a thickness of 10 mm; the phase change heat absorption heat insulation material layer is made of Carbonate phase change material with a thickness of 10mm; the material used for the medium temperature insulation layer is quartz fiber insulation material with a thickness of 10mm; the material used for the low temperature insulation layer is rock wool insulation material with a thickness of 2mm; the material used for the radiation shielding layer It is graphite paper with a thickness of 0.2mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Silica sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例6Example 6
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为超细孔炭材料,厚度为10mm;相变吸热隔热材料层采用氟化镁相变材料,厚度为8mm;中温隔热层所用材料为硅酸钙隔热材料,厚度为5mm;低温隔热层所用材料为岩棉隔热材料,厚度为40mm;辐射屏蔽层所用材料为石墨纸,厚度为0.3mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用硅溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is an ultra-fine porous carbon material with a thickness of 10 mm; The material layer is made of magnesium fluoride phase change material with a thickness of 8mm; the material used for the medium temperature insulation layer is calcium silicate insulation material with a thickness of 5mm; the material used for the low temperature insulation layer is rock wool insulation material with a thickness of 40mm; The material used for the shielding layer is graphite paper with a thickness of 0.3mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Silica sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例7Example 7
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为碳纤维毡,厚度为40mm;相变吸热隔热材料层采用碳酸盐相变材料,厚度为10mm;中温隔热层所用材料为高硅氧纤维隔热材料,厚度为6mm;低温隔热层所用材料为超细玻璃棉隔热材料,厚度为20mm;辐射屏蔽层所用材料为铝箔,厚度为0.03mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用铝溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is carbon fiber felt with a thickness of 40 mm; the phase change heat absorption heat insulation material layer is made of Carbonate phase change material with a thickness of 10mm; the material used for the medium temperature insulation layer is high silica fiber insulation material with a thickness of 6mm; the material used for the low temperature insulation layer is ultrafine glass wool insulation material with a thickness of 20mm; The shielding layer is made of aluminum foil with a thickness of 0.03mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Aluminum sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例8Example 8
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为氧化锆纤维超高温隔热材料,厚度为10mm;相变吸热隔热材料层采用氟化镁相变材料,厚度为8mm;中温隔热层所用材料为氧化铝纤维隔热材料,厚度为10mm;低温隔热层所用材料为硅酸铝纤维隔热材料,厚度为20mm;辐射屏蔽层所用材料为金箔,厚度为0.03mm。其中各层之间均用磷酸铝系高温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is a zirconia fiber ultra-high temperature heat insulation material with a thickness of 10 mm; The thermal insulation material layer is made of magnesium fluoride phase change material with a thickness of 8mm; the material used for the medium-temperature thermal insulation layer is alumina fiber thermal insulation material with a thickness of 10mm; the material used for the low-temperature thermal insulation layer is aluminum silicate fiber thermal insulation material. The thickness is 20mm; the material used for the radiation shielding layer is gold foil with a thickness of 0.03mm. Each layer is bonded with aluminum phosphate high-temperature adhesive.
实施例9Example 9
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为超细孔炭材料,厚度为10mm;相变吸热隔热材料层采用氟化镍相变材料,厚度为10mm;中温隔热层所用材料为硅酸钙隔热材料,厚度为5mm;低温隔热层所用材料为氧化硅气凝胶隔热材料,厚度为20mm;辐射屏蔽层所用材料为钼箔,厚度为0.1mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用硅溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is an ultra-fine porous carbon material with a thickness of 10 mm; The material layer is made of nickel fluoride phase change material with a thickness of 10mm; the material used for the medium temperature insulation layer is calcium silicate insulation material with a thickness of 5mm; the material used for the low temperature insulation layer is silica airgel insulation material with a thickness of 20mm; the material used for the radiation shielding layer is molybdenum foil with a thickness of 0.1mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Silica sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
实施例10Example 10
本实施例与实施例1不同在于,超高温组合隔热材料的各层所用材料及厚度如下:超高温隔热材料层所用材料为氧化锆纤维超高温隔热材料,厚度为10mm;相变吸热隔热材料层采用氟化镁相变材料,厚度为8mm;中温隔热层所用材料为硅酸钙隔热材料,厚度为5mm;低温隔热层所用材料为岩棉隔热材料,厚度为40mm;辐射屏蔽层所用材料为石墨纸,厚度为0.1mm。其中超高温隔热材料层与相变吸热隔热材料层之间用磷酸铝系高温粘结剂粘结,相变吸热隔热层与中温隔热层之间、中温隔热层与低温隔热层之间以及低温隔热层与辐射屏蔽层之间采用铝溶胶低温粘结剂粘结。The difference between this embodiment and Embodiment 1 is that the material and thickness of each layer of the ultra-high temperature composite heat insulation material are as follows: the material used for the ultra-high temperature heat insulation material layer is a zirconia fiber ultra-high temperature heat insulation material with a thickness of 10 mm; The thermal insulation material layer is made of magnesium fluoride phase change material with a thickness of 8 mm; the material used for the medium temperature thermal insulation layer is calcium silicate thermal insulation material with a thickness of 5 mm; the material used for the low temperature thermal insulation layer is rock wool thermal insulation material with a thickness of 40mm; The material used for the radiation shielding layer is graphite paper with a thickness of 0.1mm. Among them, the ultra-high temperature heat insulation material layer and the phase change heat absorption heat insulation material layer are bonded with an aluminum phosphate high-temperature adhesive, and the phase change heat absorption heat insulation layer and the medium temperature heat insulation layer, and the medium temperature heat insulation layer and the low temperature heat insulation layer are bonded together. Aluminum sol low-temperature adhesive is used to bond between the heat insulation layers and between the low temperature heat insulation layer and the radiation shielding layer.
上述实施例中各隔热材料层的制备过程如下:The preparation process of each insulation material layer in the above-mentioned embodiment is as follows:
其中碳纤维/氧化锆纤维超高温隔热材料或氧化锆纤维超高温隔热材料加去离子水混合搅拌进行纤维分散,然后抽滤成形和高温热处理得到。超细孔炭材料纤维与烧结助剂共混、高温烧结得到。碳纤维毡通过碳纤维编织成毯,或有机先驱体制备后发泡或超临界干燥等。The carbon fiber/zirconia fiber ultra-high temperature heat insulation material or the zirconia fiber ultra-high temperature heat insulation material is mixed and stirred with deionized water to disperse the fibers, and then formed by suction filtration and heat treated at high temperature. It is obtained by blending ultra-fine porous carbon material fibers with sintering aids and sintering at high temperature. Carbon fiber mats are woven into blankets through carbon fibers, or organic precursors are prepared and then foamed or supercritically dried.
相变吸热隔热材料层的制备:相变物质的熔炼,熔炼后得到的相变颗粒的粉碎,粉碎后的相变材料与基体材料和增强纤维共混,然后经过压力成形,高温烧结即得。Preparation of phase change heat absorbing and heat insulating material layer: melting of phase change material, crushing of phase change particles obtained after smelting, blending of crushed phase change material with matrix material and reinforcing fiber, and then forming under pressure, high temperature sintering have to.
中温隔热层的制备:纤维用去离子水分散,抽滤成形,高温热处理得到,或动态水热合成料浆后压滤、干燥成形得到。Preparation of medium-temperature insulation layer: fibers are dispersed with deionized water, formed by suction filtration, and obtained by high-temperature heat treatment, or obtained by dynamic hydrothermal synthesis of slurry, press-filtered, and dried to form.
低温隔热层的制备可采用与中温隔热层相同的方法。The preparation of the low-temperature heat-insulating layer can adopt the same method as that of the medium-temperature heat-insulating layer.
本发明实施例中,碳纤维/氧化锆纤维超高温隔热材料制成的超高温隔热材料层为半刚性材料,耐温2500℃,密度为0.2-1.2g/cm3,导热系数为0.02-0.2W/m·K;氧化锆纤维超高温隔热材料制成的超高温隔热材料层为刚性材料,耐温2500℃,密度为0.2-1.8g/cm3,导热系数为0.02-0.2W/m·K;碳纤维毡制成的超高温隔热材料层为柔性材料,耐温3000℃,密度为0.1-1.2g/cm3,导热系数为0.05-0.5W/m·K;超细孔炭材料制成的超高温隔热材料层为刚性材料,耐温3000℃,密度为0.1-1.2g/cm3,导热系数为0.05-0.5W/m·K。氟化镁相变材料、氟化镍相变材料及碳酸盐相变材料制成的相变吸热隔热材料层,密度为0.2-3.0g/cm3,导热系数为0.05-0.5W/m·K。中温隔热层所用材料为氧化铝纤维隔热材料、莫来石纤维隔热材料、石英纤维隔热材料、硅酸钙隔热材料以及高硅氧纤维隔热材料等,可以是刚性材料,也可以是柔性材料。低温隔热层所用材料为氧化硅气凝胶隔热材料、硅酸铝纤维隔热材料、岩棉以及超细玻璃棉等,可以是刚性材料,也可以是柔性材料。钼箔,铝箔,石墨纸或金箔等为一定幅宽的箔片材料,厚度为0.01-0.5mm。In the embodiment of the present invention, the ultra-high temperature insulation material layer made of carbon fiber/zirconia fiber ultra-high temperature insulation material is a semi-rigid material with a temperature resistance of 2500°C, a density of 0.2-1.2g/cm 3 , and a thermal conductivity of 0.02- 0.2W/m·K; the ultra-high temperature insulation material layer made of zirconia fiber ultra-high temperature insulation material is a rigid material with a temperature resistance of 2500°C, a density of 0.2-1.8g/cm 3 , and a thermal conductivity of 0.02-0.2W /m·K; the ultra-high temperature insulation material layer made of carbon fiber felt is a flexible material with a temperature resistance of 3000°C, a density of 0.1-1.2g/cm 3 , and a thermal conductivity of 0.05-0.5W/m·K; ultra-fine pores The ultra-high temperature insulation material layer made of carbon material is a rigid material with a temperature resistance of 3000°C, a density of 0.1-1.2g/cm 3 , and a thermal conductivity of 0.05-0.5W/m·K. The phase change heat absorbing and insulating material layer made of magnesium fluoride phase change material, nickel fluoride phase change material and carbonate phase change material has a density of 0.2-3.0g/cm3 and a thermal conductivity of 0.05-0.5W/m ·K. The materials used for the medium temperature insulation layer are alumina fiber insulation materials, mullite fiber insulation materials, quartz fiber insulation materials, calcium silicate insulation materials and high silica fiber insulation materials, etc., which can be rigid materials or Can be a flexible material. The materials used for the low-temperature insulation layer are silica airgel insulation materials, aluminum silicate fiber insulation materials, rock wool and ultra-fine glass wool, etc., which can be rigid materials or flexible materials. Molybdenum foil, aluminum foil, graphite paper or gold foil are foil materials with a certain width, and the thickness is 0.01-0.5mm.
本发明实施例的超高温组合隔热材料的性能指标见下表1。其中隔热性能参照GB/T17911.3-1999耐火陶瓷纤维制品体积密度试验方法,YB/T4130-2005水流量平板法。The performance indicators of the ultra-high temperature combined heat insulation material of the embodiment of the present invention are shown in Table 1 below. The heat insulation performance refers to GB/T17911.3-1999 test method for bulk density of refractory ceramic fiber products, and YB/T4130-2005 water flow plate method.
表1Table 1
通过表1可以看出,本发明实施例的超高温组合隔热材料整体具有较高的隔热性,并且通过合理设置层结构,其外层的隔热材料就具有更多的可选择性,无论从原料取得及成本等方面均有较大的优势。本发明实施例的超高温组合隔热材料整体表现为半刚性,密度为0.20-2.0g/cm3,导热系数为0.02W/m·K-0.12W/m·K,耐温最高可达2200℃。防护使用时间可达2500秒。It can be seen from Table 1 that the ultra-high temperature combined heat insulation material of the embodiment of the present invention has relatively high heat insulation as a whole, and by rationally setting the layer structure, the heat insulation material of the outer layer has more options. It has great advantages in terms of raw material acquisition and cost. The ultra-high temperature combined heat insulation material of the embodiment of the present invention is semi-rigid as a whole, with a density of 0.20-2.0g/cm 3 , a thermal conductivity of 0.02W/m·K-0.12W/m·K, and a maximum temperature resistance of 2200 ℃. The protective use time can reach 2500 seconds.
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。The above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Anyone skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present invention. Should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be determined by the protection scope of the claims.
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