CN102030544B - Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating - Google Patents

Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating Download PDF

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CN102030544B
CN102030544B CN201010500871A CN201010500871A CN102030544B CN 102030544 B CN102030544 B CN 102030544B CN 201010500871 A CN201010500871 A CN 201010500871A CN 201010500871 A CN201010500871 A CN 201010500871A CN 102030544 B CN102030544 B CN 102030544B
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张跃
王广海
肖世月
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Beihang University
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Abstract

本发明公开了一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,该方法用正硅酸己酯、乙醇、去离子水和盐酸制溶胶;用正硅酸己酯、异丙醇、去离子水、氨水合成直径在0.3~3μm的氧化硅微球,然后在氧化硅微球生长30~500nm厚高折射率的氧化钛壳层,获得核壳结构填料。以制备的核壳结构颗粒作为填料分散到溶胶中,经热处理后可获得致密均匀的无机涂层。本发明所添加的核壳结构颜料对1~10μm的红外热辐射有很高的反射能力,而且填料的添加量很小,涂层的介电常数增加不多,使得涂层有较高的热反射率同时不影响透微波能力,可用于1200℃的高温防护。

Figure 201010500871

The invention discloses a preparation method for forming an inorganic coating with high temperature resistance, radiation heat transfer and microwave transmission compatibility. Ester, isopropanol, deionized water, and ammonia water synthesize silica microspheres with a diameter of 0.3-3 μm, and then grow a 30-500 nm thick titanium oxide shell with a high refractive index on the silica microspheres to obtain a core-shell structure filler. The prepared core-shell particles are dispersed into the sol as a filler, and a dense and uniform inorganic coating can be obtained after heat treatment. The core-shell structure pigment added in the present invention has a high reflection ability to 1-10 μm infrared heat radiation, and the addition amount of the filler is very small, and the dielectric constant of the coating does not increase much, so that the coating has a higher thermal conductivity. At the same time, the reflectivity does not affect the ability of microwave transmission, which can be used for high temperature protection of 1200 ℃.

Figure 201010500871

Description

一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法A preparation method for forming an inorganic coating compatible with high temperature resistance, radiation heat transfer and microwave transmission

技术领域 technical field

本发明涉及一种耐高温隔辐射传热与透微波兼容涂层材料制备方法,具体是指,用溶胶凝胶方法制备无机涂层基体材料,并加入合成的核壳结构的功能性填料,以实现隔辐射传热与透微波的兼容。The invention relates to a method for preparing a high-temperature-resistant, radiation-insulated, heat-transfer and microwave-permeable coating material, specifically, an inorganic coating matrix material is prepared by a sol-gel method, and a synthesized functional filler with a core-shell structure is added to obtain Realize the compatibility of radiation heat transfer and microwave transmission.

背景技术 Background technique

传热的基本方式有热传导、热对流和热辐射三种。热辐射是热量传递的三种基本方式之一,随着温度升高,辐射传热所占比重逐渐增加。因此发展耐高温隔热材料需有效抑制辐射传热。高温下材料发射大量热射线,这些热射线集中在0.76~10μm波段的红外区,屏蔽0.76~10μm的红外热辐射即可有效阻隔辐射传热,提高高温隔热材料的使用温度和时间。There are three basic ways of heat transfer: heat conduction, heat convection and heat radiation. Thermal radiation is one of the three basic ways of heat transfer. As the temperature increases, the proportion of radiation heat transfer gradually increases. Therefore, the development of high-temperature-resistant insulation materials needs to effectively suppress radiative heat transfer. Materials emit a large number of heat rays at high temperatures, and these heat rays are concentrated in the infrared region of the 0.76-10 μm band. Shielding the infrared heat radiation of 0.76-10 μm can effectively block radiation heat transfer and increase the use temperature and time of high-temperature insulation materials.

石英、氮化硅等陶瓷材料,作为高温结构材料能经受高温、不怕氧化、耐酸碱腐蚀,在建筑、汽车及航空航天等领域得到了广泛的应用。但是这些材料在红外波段有透过段,因此高温的辐射传热非常明显。不仅使石英、氮化硅等陶瓷材料在高温下迅速升温,降低使用时间,而且向内发射大量热射线,内部的设备会因此而失效。因此实现对此类材料高温下的辐射传热有效屏蔽,可以延长材料使用时间,保护内部设备。另外,石英、氮化硅等陶瓷材料的介电常数很低,是优良的耐高温透微波材料,在同时要求热、电性能的场合,需要在有效屏蔽辐射传热的同时不影响其电性能,即要求涂层具有隔辐射传热与透微波兼容的性能。Ceramic materials such as quartz and silicon nitride, as high-temperature structural materials, can withstand high temperatures, are not afraid of oxidation, and are resistant to acid and alkali corrosion, and have been widely used in construction, automotive, aerospace and other fields. However, these materials have a transparent section in the infrared band, so the high-temperature radiation heat transfer is very obvious. It not only makes ceramic materials such as quartz and silicon nitride heat up rapidly at high temperature, shortening the service time, but also emits a large amount of heat rays inward, which will cause the internal equipment to fail. Therefore, the effective shielding of radiation heat transfer of such materials at high temperatures can prolong the service life of materials and protect internal equipment. In addition, the dielectric constant of ceramic materials such as quartz and silicon nitride is very low, and they are excellent high-temperature-resistant and microwave-transparent materials. When thermal and electrical properties are required at the same time, it is necessary to effectively shield radiation heat transfer without affecting its electrical properties. , that is, the coating is required to be compatible with radiation heat transfer and microwave transmission.

对于耐高温隔辐射传热与透微波兼容涂层的制备尚未见到相关的文献。There is no relevant literature on the preparation of high temperature resistant radiation heat transfer and microwave transparent coatings.

发明内容 Contents of the invention

本发明的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,该制备过程中以氧化硅或氧化铝为基体,通过添加具有反红外热辐射性能的核壳结构颗粒为填料,使其具有优异的隔辐射传热的能力,同时不影响其透微波性能。经本发明方法制得的无机涂层能够作为1200℃工作环境的高温隔热透微波涂层材料。耐高温隔热透微波涂层材料是一种全新的耐高温隔热材料,兼有隔热和透微波的功能。隔热的机理为屏蔽高温下的红外热辐射,来达到高温隔热的目的。A preparation method of the present invention to form an inorganic coating with high temperature resistance, radiation heat transfer and microwave transmission compatibility. In the preparation process, silicon oxide or aluminum oxide is used as the substrate, and a core-shell structure with anti-infrared heat radiation performance is added. The particles are fillers, which make it have excellent radiation and heat transfer capabilities without affecting its microwave transmission performance. The inorganic coating prepared by the method of the invention can be used as a high-temperature, heat-insulating, and microwave-transmitting coating material in a working environment of 1200°C. High temperature resistant heat insulation microwave transparent coating material is a brand new high temperature resistant heat insulation material, which has the functions of heat insulation and microwave transmission. The mechanism of heat insulation is to shield the infrared heat radiation at high temperature to achieve the purpose of high temperature heat insulation.

耐高温隔辐射传热与透微波兼容涂料,原料组分主要有无机溶胶和核壳结构颗粒填料。本发明选用无机溶胶作为耐高温成膜物质,具体选自氧化硅溶胶,氧化钛溶胶,氧化铝溶胶或氧化锆溶胶中的一种或几种。所述的核壳结构填料颗粒为球形,半径在0.3~3μm,壳的厚度在30~500nm之间。High temperature resistant radiation heat transfer and microwave transparent coating, the raw material components mainly include inorganic sol and core-shell structure particle filler. In the present invention, inorganic sol is selected as the high-temperature-resistant film-forming material, specifically selected from one or more of silica sol, titania sol, alumina sol or zirconia sol. The core-shell structure filler particles are spherical, with a radius of 0.3-3 μm and a shell thickness of 30-500 nm.

以上原料无机溶胶,核壳结构颗粒均为自制。The above raw material inorganic sol and core-shell structure particles are all self-made.

本发明的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,制备该无机涂层通过下列步骤实现:A preparation method of the present invention to form an inorganic coating with high temperature resistance, radiation heat transfer and microwave transmission compatibility, the preparation of the inorganic coating is achieved by the following steps:

步骤一:制备无机溶胶Step 1: Preparation of Inorganic Sol

(A)在10ml的第一溶剂中加入5~10g的前驱体,并搅拌均匀,得到前驱体溶液;(A) Add 5 to 10 g of precursor to 10 ml of the first solvent, and stir evenly to obtain a precursor solution;

(B)在10ml的去离子水中加入20~50ml的第二溶剂和5~6滴的盐酸(HCl)(摩尔浓度为1mol/L),并搅拌均匀,得到溶胶反应物溶液;(B) Add 20 to 50 ml of the second solvent and 5 to 6 drops of hydrochloric acid (HCl) (molar concentration is 1 mol/L) in 10 ml of deionized water, and stir evenly to obtain a sol reactant solution;

(C)将步骤(B)制得的溶胶反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为400~800r/min的条件下反应1~12h,反应结束后制得无机溶胶;(C) Add the sol reactant solution prepared in step (B) to the precursor solution prepared in step (A), and react for 1 to 12 hours at a stirring speed of 400 to 800 r/min. After the reaction, prepare Inorganic sol;

所述前驱体是正硅酸己酯(TEOS)或者异丙醇铝(C9H21AlO3)。The precursor is orthohexyl silicate (TEOS) or aluminum isopropoxide (C 9 H 21 AlO 3 ).

所述第一溶剂是乙醇(C2H5OH)、丙酮(C3H6O)和乙醚(C4H10O)中的一种。The first solvent is one of ethanol (C 2 H 5 OH), acetone (C 3 H 6 O) and ether (C 4 H 10 O).

所述第二溶剂是乙醇(C2H5OH)、丙酮(C3H6O)和乙醚(C4H10O)中的一种。The second solvent is one of ethanol (C 2 H 5 OH), acetone (C 3 H 6 O) and ether (C 4 H 10 O).

在本发明中,在配制过程中,第一溶剂与第二溶剂要用相同的用料。In the present invention, in the preparation process, the first solvent and the second solvent should use the same materials.

步骤二:制备核壳结构填料Step 2: Preparation of core-shell structure packing

(A)在50ml的乙醇(C2H5OH)中加入0.2~2ml的无机盐和2~10g的氧化硅粉(粒径0.3~5μm),并搅拌均匀,得到填料前驱体溶液;(A) Add 0.2-2 ml of inorganic salt and 2-10 g of silicon oxide powder (0.3-5 μm in particle size) to 50 ml of ethanol (C 2 H 5 OH), and stir evenly to obtain a filler precursor solution;

所述无机盐是钛酸四丁酯(TBOT)或者氧氯化锆(ZrOCl2);The inorganic salt is tetrabutyl titanate (TBOT) or zirconium oxychloride (ZrOCl 2 );

(B)在10ml的去离子水中加入25~50ml的乙醇(C2H5OH)和1~10滴的百分比浓度为99%的浓硝酸(HNO3),并搅拌均匀,得到填料反应物溶液;(B) Add 25 to 50 ml of ethanol (C 2 H 5 OH) and 1 to 10 drops of concentrated nitric acid (HNO 3 ) with a percentage concentration of 99% in 10 ml of deionized water, and stir evenly to obtain a filler reactant solution ;

(C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为25~100℃、搅拌速度为400~800r/min的条件下反应2~5h,反应结束后制得填料溶液;(C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), under the condition that the reaction temperature is 25-100°C and the stirring speed is 400-800r/min React for 2 to 5 hours, and prepare a filler solution after the reaction;

(D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理3~10min,并在水热釜温度为140~180℃条件下水热2~24h;然后进行离心干燥得到填料;(D) ultrasonically treat the filler solution obtained in step (C) for 3 to 10 minutes under the condition of ultrasonic power of 1000 W, and heat it for 2 to 24 hours in a hydrothermal kettle at a temperature of 140 to 180 ° C; then perform centrifugal drying to obtain the filler ;

离心干燥的条件为:转速400~800r/min、干燥温度70~90℃、干燥时间2~6h;The conditions of centrifugal drying are: rotating speed 400~800r/min, drying temperature 70~90℃, drying time 2~6h;

(E)将步骤(D)制得的填料在马弗炉中以300~700℃的温度下保温2~10h,得到核壳结构填料;(E) keeping the filler prepared in step (D) in a muffle furnace at a temperature of 300-700°C for 2-10 hours to obtain a core-shell structure filler;

步骤三:制备涂层材料Step 3: Preparation of Coating Material

将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,并搅拌均匀,得到无机涂层材料;adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material;

用量:50ml的无机溶胶中加入2~10g的核壳结构填料。Dosage: Add 2-10g of core-shell structure filler to 50ml of inorganic sol.

本发明的优良效果如下:The excellent effects of the present invention are as follows:

1、本发明的耐高温隔辐射传热与透微波兼容涂层材料,其成膜性好,不开裂,不脱落,制备工艺简单。1. The high-temperature-resistant radiation heat-transfer and microwave-transparent coating material of the present invention has good film-forming properties, no cracking, no falling off, and a simple preparation process.

2、本发明通过添加核壳结构填料颗粒制备隔辐射传热材料,相对于单一成分球形填料而言,具有很高的隔辐射传热的作用,且对介电性能的影响较小。2. In the present invention, the radiation and heat-transfer material is prepared by adding core-shell structure filler particles. Compared with the single-component spherical filler, it has a high effect of radiation and heat-transfer, and has little influence on the dielectric properties.

3、本发明的涂层材料是一种多功能的涂层材料,一方面能满足高温下隔辐射传热的要求,同时满足透微波的要求。3. The coating material of the present invention is a multifunctional coating material, which can meet the requirements of radiation heat transfer at high temperature on the one hand, and meet the requirements of microwave transmission at the same time.

4、本发明的耐高温隔辐射传热与透微波兼容涂层可用于1200℃的高温保护。4. The high-temperature-resistant radiation heat-transfer and microwave-transparent coating of the present invention can be used for high temperature protection at 1200°C.

附图说明 Description of drawings

图1是本发明实施例1核壳结构填料扫描电镜图片。Fig. 1 is a scanning electron microscope picture of a core-shell structure filler according to Example 1 of the present invention.

图1A是本发明实施例1核壳结构填料透射电镜图片。FIG. 1A is a transmission electron microscope image of a core-shell structure filler according to Example 1 of the present invention.

图2是本发明实施例1是本发明实施例1100μm厚涂层的表面SEM图。Fig. 2 is an SEM image of the surface of the 1100 μm thick coating in Example 1 of the present invention.

图2A是本发明实施例1是本发明实施例1100μm厚涂层的断面SEM图。Fig. 2A is a cross-sectional SEM image of the 1100 μm thick coating in Example 1 of the present invention.

图3是本发明实施例1本发明实施例1涂层在波数1000~4000cm-1的红外透过率图谱。Fig. 3 is the infrared transmittance spectrum of the coating in Example 1 of the present invention at a wave number of 1000-4000 cm −1 .

图4是本发明实施例1制得100μm厚涂层的介电常数随频率变化图谱。Fig. 4 is a graph showing the variation of dielectric constant with frequency of the 100 μm thick coating prepared in Example 1 of the present invention.

图5是本发明实施例1涂层的介电损耗随频率变化图谱。Fig. 5 is a diagram showing the variation of dielectric loss with frequency of the coating according to Example 1 of the present invention.

具体实施方式 Detailed ways

本发明的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,制备该无机涂层通过下列步骤实现:A preparation method of the present invention to form an inorganic coating with high temperature resistance, radiation heat transfer and microwave transmission compatibility, the preparation of the inorganic coating is achieved by the following steps:

步骤一:制备无机溶胶Step 1: Preparation of Inorganic Sol

(A)在10ml的第一溶剂中加入5~10g的前驱体,并搅拌均匀,得到前驱体溶液;(A) Add 5 to 10 g of precursor to 10 ml of the first solvent, and stir evenly to obtain a precursor solution;

(B)在10ml的去离子水中加入20~50ml的第二溶剂和5~6滴的盐酸(HCl)(摩尔浓度为1mol/L),并搅拌均匀,得到溶胶反应物溶液;(B) Add 20 to 50 ml of the second solvent and 5 to 6 drops of hydrochloric acid (HCl) (molar concentration is 1 mol/L) in 10 ml of deionized water, and stir evenly to obtain a sol reactant solution;

(C)将步骤(B)制得的溶胶反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为400~800r/min的条件下反应1~12h,反应结束后制得无机溶胶;(C) Add the sol reactant solution prepared in step (B) to the precursor solution prepared in step (A), and react for 1 to 12 hours at a stirring speed of 400 to 800 r/min. After the reaction, prepare Inorganic sol;

所述前驱体是正硅酸己酯(TEOS)或者异丙醇铝(C9H21AlO3)。The precursor is orthohexyl silicate (TEOS) or aluminum isopropoxide (C 9 H 21 AlO 3 ).

所述第一溶剂是乙醇(C2H5OH)、丙酮(C3H6O)和乙醚(C4H10O)中的一种。The first solvent is one of ethanol (C 2 H 5 OH), acetone (C 3 H 6 O) and ether (C 4 H 10 O).

所述第二溶剂是乙醇(C2H5OH)、丙酮(C3H6O)和乙醚(C4H10O)中的一种。The second solvent is one of ethanol (C 2 H 5 OH), acetone (C 3 H 6 O) and ether (C 4 H 10 O).

在本发明中,在配制过程中,第一溶剂与第二溶剂要用相同的用料。In the present invention, in the preparation process, the first solvent and the second solvent should use the same materials.

步骤二:制备核壳结构填料Step 2: Preparation of core-shell structure packing

(A)在50ml的乙醇(C2H5OH)中加入0.2~2ml的无机盐和2~10g的氧化硅粉(粒径0.3~5μm),并搅拌均匀,得到填料前驱体溶液;(A) Add 0.2-2 ml of inorganic salt and 2-10 g of silicon oxide powder (0.3-5 μm in particle size) to 50 ml of ethanol (C 2 H 5 OH), and stir evenly to obtain a filler precursor solution;

所述无机盐是钛酸四丁酯(TBOT)或者氧氯化锆(ZrOCl2);The inorganic salt is tetrabutyl titanate (TBOT) or zirconium oxychloride (ZrOCl 2 );

(B)在10ml的去离子水中加入25~50ml的乙醇(C2H5OH)和1~10滴的百分比浓度为99%的浓硝酸(HNO3),并搅拌均匀,得到填料反应物溶液;(B) Add 25 to 50 ml of ethanol (C 2 H 5 OH) and 1 to 10 drops of concentrated nitric acid (HNO 3 ) with a percentage concentration of 99% in 10 ml of deionized water, and stir evenly to obtain a filler reactant solution ;

(C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为25~100℃、搅拌速度为400~800r/min的条件下反应2~5h,反应结束后制得填料溶液;(C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), under the condition that the reaction temperature is 25-100°C and the stirring speed is 400-800r/min React for 2 to 5 hours, and prepare a filler solution after the reaction;

(D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理3~10min,并在水热釜温度为140~180℃条件下水热2~24h;然后进行离心干燥得到填料;(D) ultrasonically treat the filler solution obtained in step (C) for 3 to 10 minutes under the condition of ultrasonic power of 1000 W, and heat it for 2 to 24 hours in a hydrothermal kettle at a temperature of 140 to 180 ° C; then perform centrifugal drying to obtain the filler ;

离心干燥的条件为:转速400~800r/min、干燥温度70~90℃、干燥时间2~6h;The conditions of centrifugal drying are: rotating speed 400~800r/min, drying temperature 70~90℃, drying time 2~6h;

(E)将步骤(D)制得的填料在马弗炉中以300~700℃的温度下保温2~10h,得到核壳结构填料;(E) keeping the filler prepared in step (D) in a muffle furnace at a temperature of 300-700°C for 2-10 hours to obtain a core-shell structure filler;

步骤三:制备涂层材料Step 3: Preparation of Coating Material

将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,并搅拌均匀,得到无机涂层材料;adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material;

用量:50ml的无机溶胶中加入2~10g的核壳结构填料。Dosage: Add 2-10g of core-shell structure filler to 50ml of inorganic sol.

实施例1:Example 1:

步骤一:制备无机溶胶Step 1: Preparation of Inorganic Sol

(A)在10ml的乙醇中加入5.7g的正硅酸己酯,并搅拌均匀,得到前驱体溶液;(A) Add 5.7 g of hexyl orthosilicate in 10 ml of ethanol, and stir evenly to obtain a precursor solution;

(B)在10ml的去离子水中加入20ml的乙醇和1mol/L盐酸溶液(HCl)5滴,并搅拌均匀,得到溶胶反应物溶液;(B) Add 20 ml of ethanol and 5 drops of 1mol/L hydrochloric acid solution (HCl) in 10 ml of deionized water, and stir evenly to obtain a sol reactant solution;

(C)将步骤(B)制得的反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为600r/min的条件下反应12h,反应结束后制得无机溶胶;(C) adding the reactant solution prepared in step (B) to the precursor solution prepared in step (A), reacting for 12 hours at a stirring speed of 600 r/min, and preparing an inorganic sol after the reaction;

步骤二:制备核壳结构填料Step 2: Preparation of core-shell structure packing

(A)在50ml的乙醇中加入0.4ml的钛酸四丁酯和2g的氧化硅粉(粒径0.3~5μm),并搅拌均匀,得到填料前驱体溶液;(A) Add 0.4 ml of tetrabutyl titanate and 2 g of silicon oxide powder (0.3 to 5 μm in particle size) in 50 ml of ethanol, and stir evenly to obtain a filler precursor solution;

(B)在10ml的去离子水中加入25ml乙醇和百分比浓度99%的浓硝酸(HNO3)4滴,并搅拌均匀,得到填料反应物溶液;(B) Add 25ml of ethanol and 4 drops of concentrated nitric acid (HNO 3 ) with a percentage concentration of 99% in 10ml of deionized water, and stir evenly to obtain a filler reactant solution;

(C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为25℃、搅拌速度为800r/min的条件下反应2h,反应结束后制得填料溶液;(C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), and react for 2 hours at a reaction temperature of 25°C and a stirring speed of 800r/min. Make filler solution after finishing;

(D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理5min,并在水热釜温度为180℃条件下水热20h;然后进行离心干燥得到填料;(D) ultrasonically treat the filler solution obtained in step (C) for 5 minutes under the condition of an ultrasonic power of 1000 W, and heat it in water for 20 hours at a temperature of 180° C. in a hydrothermal kettle; then perform centrifugal drying to obtain the filler;

离心干燥的条件为:转速400r/min、干燥温度90℃、干燥时间3h;The conditions of centrifugal drying are: rotating speed 400r/min, drying temperature 90°C, drying time 3h;

(E)将步骤(D)制得的填料在马弗炉中700℃保温2h,得到核壳结构填料;(E) keeping the filler prepared in step (D) in a muffle furnace at 700° C. for 2 hours to obtain a core-shell structure filler;

应用扫描电镜和透射电镜观察核壳结构填料的形貌,其核壳结构填料的粒径在0.3~5μm,壳的厚度在100~300nm之间,如图1、图1A所示。The morphology of the core-shell filler was observed by scanning electron microscopy and transmission electron microscopy. The particle size of the core-shell filler was 0.3-5 μm, and the thickness of the shell was between 100-300 nm, as shown in Figure 1 and Figure 1A.

步骤三:制备涂层材料Step 3: Preparation of Coating Material

将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,搅拌均匀,得到无机涂层材料;adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material;

用量:50ml的无机溶胶中加入8g的核壳结构填料。Dosage: Add 8g of core-shell structure filler to 50ml of inorganic sol.

采用刷涂工艺在玻璃基片上制得80μm厚的膜,使用CamScan公司的型号为Apollo300扫描电镜观察涂层形貌,涂层形貌如图2、图2A所示。图2为表面形貌,图2A为涂层断面形貌。从表面扫描电镜照片可以看出无机涂层表面均匀致密无裂纹,断面可看出涂层厚度约为80μm。A film with a thickness of 80 μm was prepared on a glass substrate by a brushing process, and the morphology of the coating was observed with a scanning electron microscope (model Apollo 300 from CamScan Company). The morphology of the coating is shown in Figure 2 and Figure 2A. Figure 2 is the surface morphology, and Figure 2A is the cross-sectional morphology of the coating. From the surface scanning electron microscope photos, it can be seen that the surface of the inorganic coating is uniform and dense without cracks, and the thickness of the coating can be seen to be about 80 μm in the cross section.

涂层的红外透微波和介电性能如图3、图4和图5所示。由图3可知,添加核壳结构填料的涂层对热辐射有明显的屏蔽作用,同时对介电性能的影响不大。因SiO2的熔点在1400℃左右,因此此涂层可在1200℃下长期使用。The infrared microwave transmission and dielectric properties of the coating are shown in Figure 3, Figure 4 and Figure 5. It can be seen from Figure 3 that the coating with core-shell structure filler has obvious shielding effect on thermal radiation, and has little effect on dielectric properties. Since the melting point of SiO2 is around 1400°C, this coating can be used for a long time at 1200°C.

涂层的隔辐射传热性能可用其红外透过率来表征,采用Nicolet公司生产,型号为NEXUS-470,智能傅立叶红外光谱仪(FTIR)测得的涂层红外透过率如图3所示。从图3可知,在石英片上涂有80μm后的无机涂层后,透过率减小到30%左右。即无机涂层能够屏蔽大部分红外热辐射,具有良好的隔辐射传热性能。The radiation heat transfer performance of the coating can be characterized by its infrared transmittance, which is produced by Nicolet Company, model NEXUS-470, and the infrared transmittance of the coating measured by an intelligent Fourier infrared spectrometer (FTIR) is shown in Figure 3. It can be seen from Figure 3 that the transmittance decreases to about 30% after the quartz plate is coated with an inorganic coating after 80 μm. That is to say, the inorganic coating can shield most of the infrared heat radiation and has good radiation insulation and heat transfer performance.

加入核壳填料后无机涂层的介电性能会有所变化,采用美国安捷伦(Agilent)公司生产型号为8722ES的矢量网络分析仪分析其介电性能变化,测试结果如图4,5所示。有图可知,加入核壳结构填料后无机涂层的介电常数和介电损耗变化不大,不会影响其微波透过性能。After adding core-shell fillers, the dielectric properties of inorganic coatings will change. A vector network analyzer (model 8722ES) produced by Agilent (USA) was used to analyze the changes in dielectric properties. The test results are shown in Figures 4 and 5. It can be seen from the figure that the dielectric constant and dielectric loss of the inorganic coating do not change much after adding the core-shell structure filler, which will not affect its microwave transmission performance.

实施例2:Example 2:

步骤一:制备无机溶胶Step 1: Preparation of Inorganic Sol

(A)在10ml的丙酮中加入10g的异丙醇铝,并搅拌均匀,得到前驱体溶液;(A) Add 10 g of aluminum isopropoxide to 10 ml of acetone, and stir evenly to obtain a precursor solution;

(B)在10ml的去离子水中加入50ml的丙酮和6滴的盐酸(1mol/L),并搅拌均匀,得到溶胶反应物溶液;(B) Add 50ml of acetone and 6 drops of hydrochloric acid (1mol/L) to 10ml of deionized water, and stir evenly to obtain a sol reactant solution;

(C)将步骤(B)制得的反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为800r/min的条件下反应2h,反应结束后制得无机溶胶;(C) adding the reactant solution prepared in step (B) to the precursor solution prepared in step (A), reacting for 2 hours at a stirring speed of 800r/min, and preparing an inorganic sol after the reaction;

步骤二:制备核壳结构填料Step 2: Preparation of core-shell structure packing

(A)在50ml的乙醇中加入2ml的氧氯化锆和10g的氧化硅粉(粒径0.3~5μm),并搅拌均匀,得到填料前驱体溶液;(A) Add 2ml of zirconium oxychloride and 10g of silicon oxide powder (0.3-5 μm in particle size) in 50ml of ethanol, and stir evenly to obtain a filler precursor solution;

(B)在10ml的去离子水中加入35ml乙醇和百分比浓度99%的浓硝酸(HNO3)10滴,并搅拌均匀,得到填料反应物溶液;(B) Add 35ml of ethanol and 10 drops of concentrated nitric acid (HNO 3 ) with a percentage concentration of 99% in 10ml of deionized water, and stir evenly to obtain a filler reactant solution;

(C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为60℃、搅拌速度为700r/min的条件下反应3h,反应结束后制得填料溶液;(C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), and react for 3 hours at a reaction temperature of 60°C and a stirring speed of 700r/min. Make filler solution after finishing;

(D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理8min,并在水热釜温度为150℃条件下水热10h;然后进行离心干燥得到填料;(D) Ultrasonic treatment of the filler solution obtained in step (C) for 8 minutes under the condition of ultrasonic power of 1000 W, and hydrothermal heating at a temperature of 150° C. for 10 hours in a hydrothermal kettle; and then centrifugally drying to obtain the filler;

离心干燥的条件为:转速800r/min、干燥温度70℃、干燥时间2h;The conditions of centrifugal drying are: rotating speed 800r/min, drying temperature 70°C, drying time 2h;

(E)将步骤(D)制得的填料在马弗炉中300℃保温10h,得到核壳结构填料;(E) keeping the filler prepared in step (D) in a muffle furnace at 300° C. for 10 hours to obtain a core-shell structure filler;

应用扫描电镜和透射电镜观察核壳结构填料的形貌,其核壳结构的粒径在0.3~5μm,壳的厚度在300~500nm之间。The morphology of the core-shell structure filler was observed by scanning electron microscope and transmission electron microscope. The particle size of the core-shell structure was 0.3-5 μm, and the thickness of the shell was between 300-500 nm.

步骤三:制备涂层材料Step 3: Preparation of Coating Material

将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,搅拌均匀,得到无机涂层材料;adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material;

用量:50ml的无机溶胶中加入2~10g的核壳结构填料。Dosage: Add 2-10g of core-shell structure filler to 50ml of inorganic sol.

按照实施例2方法制得的涂层的隔辐射传热性能可用其红外透过率来表征,在石英片上涂有80μm后的涂层后,透过率减小到30%左右。即涂层能够屏蔽大部分红外热辐射,具有良好的隔辐射传热性能。The radiation and heat transfer performance of the coating prepared according to the method in Example 2 can be characterized by its infrared transmittance, and the transmittance is reduced to about 30% after the 80 μm coating is coated on the quartz plate. That is, the coating can shield most of the infrared heat radiation and has good radiation insulation and heat transfer performance.

加入核壳结构填料后涂层的介电常数和介电损耗变化不大,不会影响其微波透过性能。The dielectric constant and dielectric loss of the coating do not change much after adding the core-shell structure filler, which will not affect its microwave transmission performance.

实施例3:Example 3:

步骤一:制备无机溶胶Step 1: Preparation of Inorganic Sol

(A)在10ml的乙醚中加入8g的正硅酸己酯,并搅拌均匀,得到前驱体溶液;(A) Add 8g of hexyl orthosilicate in 10ml of diethyl ether, and stir evenly to obtain a precursor solution;

(B)在10ml的去离子水中加入30ml的乙醚和1mol/L盐酸溶液(HCl)5滴,并搅拌均匀,得到溶胶反应物溶液;(B) Add 30 ml of ether and 5 drops of 1mol/L hydrochloric acid solution (HCl) in 10 ml of deionized water, and stir evenly to obtain a sol reactant solution;

(C)将步骤(B)制得的反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为500r/min的条件下反应6h,反应结束后制得无机溶胶;(C) adding the reactant solution prepared in step (B) to the precursor solution prepared in step (A), reacting for 6 hours at a stirring speed of 500 r/min, and preparing an inorganic sol after the reaction;

步骤二:制备核壳结构填料Step 2: Preparation of core-shell structure packing

(A)在50ml的乙醇中加入1ml的钛酸四丁酯和5g的氧化硅粉(粒径0.3~5μm),并搅拌均匀,得到填料前驱体溶液;(A) Add 1 ml of tetrabutyl titanate and 5 g of silicon oxide powder (0.3-5 μm in particle size) into 50 ml of ethanol, and stir evenly to obtain a filler precursor solution;

(B)在10ml的去离子水中加入35ml乙醇和百分比浓度99%的浓硝酸(HNO3)7滴,并搅拌均匀,得到填料反应物溶液;(B) Add 35ml of ethanol and 7 drops of concentrated nitric acid (HNO 3 ) with a percentage concentration of 99% in 10ml of deionized water, and stir evenly to obtain a filler reactant solution;

(C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为60℃、搅拌速度为500r/min的条件下反应5h,反应结束后制得填料溶液;(C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), and react for 5 hours at a reaction temperature of 60°C and a stirring speed of 500r/min. Make filler solution after finishing;

(D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理6min,并在水热釜温度为160℃条件下水热12h;然后进行离心干燥得到填料;(D) ultrasonically treat the filler solution obtained in step (C) for 6 minutes under the condition of ultrasonic power of 1000 W, and heat it in water for 12 hours at a temperature of 160° C. in a hydrothermal kettle; then perform centrifugal drying to obtain the filler;

离心干燥的条件为:转速600r/min、干燥温度80℃、干燥时间4h;The conditions of centrifugal drying are: rotating speed 600r/min, drying temperature 80°C, drying time 4h;

(E)将步骤(D)制得的填料在马弗炉中600℃保温6h,得到核壳结构填料;(E) keeping the filler prepared in step (D) in a muffle furnace at 600° C. for 6 hours to obtain a core-shell structure filler;

应用扫描电镜和透射电镜观察核壳结构填料的形貌,其核壳结构的粒径在0.3~5μm,壳的厚度在350~500nm之间。The morphology of the core-shell structure filler was observed by scanning electron microscope and transmission electron microscope. The particle size of the core-shell structure was 0.3-5 μm, and the thickness of the shell was between 350-500 nm.

步骤三:制备涂层材料Step 3: Preparation of Coating Material

将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,搅拌均匀,得到无机涂层材料;adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material;

用量:50ml的无机溶胶中加入2~10g的核壳结构填料Dosage: Add 2-10g of core-shell structure filler to 50ml of inorganic sol

按照实施例3方法制得的涂层的隔辐射传热性能可用其红外透过率来表征,在石英片上涂有80μm后的涂层后,透过率减小到30%左右。即涂层能够屏蔽大部分红外热辐射,具有良好的隔辐射传热性能。The radiation and heat transfer performance of the coating prepared according to the method of Example 3 can be characterized by its infrared transmittance, and the transmittance is reduced to about 30% after the 80 μm coating is coated on the quartz plate. That is, the coating can shield most of the infrared heat radiation and has good radiation insulation and heat transfer performance.

加入核壳结构填料后涂层的介电常数和介电损耗变化不大,不会影响其微波透过性能。The dielectric constant and dielectric loss of the coating do not change much after adding the core-shell structure filler, which will not affect its microwave transmission performance.

Claims (6)

1.一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于制备该无机涂层通过下列步骤实现: 1. A preparation method for forming an inorganic coating with high temperature resistance, radiation heat transfer and microwave penetration compatibility, characterized in that the preparation of the inorganic coating is achieved through the following steps: 步骤一:制备无机溶胶 Step 1: Preparation of Inorganic Sol (A)在10ml的第一溶剂中加入5~10g的前驱体,并搅拌均匀,得到前驱体溶液; (A) Add 5 to 10 g of precursor to 10 ml of the first solvent, and stir evenly to obtain a precursor solution; (B)在10ml的去离子水中加入20~50ml的第二溶剂和5~6滴的摩尔浓度为1mol/L的盐酸,并搅拌均匀,得到溶胶反应物溶液; (B) adding 20 to 50 ml of the second solvent and 5 to 6 drops of hydrochloric acid with a molar concentration of 1 mol/L in 10 ml of deionized water, and stirring evenly to obtain a sol reactant solution; (C)将步骤(B)制得的溶胶反应物溶液加入至步骤(A)制得的前驱体溶液中,在搅拌速度为400~800r/min的条件下反应1~12h,反应结束后制得无机溶胶; (C) Add the sol reactant solution prepared in step (B) to the precursor solution prepared in step (A), and react for 1 to 12 hours at a stirring speed of 400 to 800 r/min. After the reaction, prepare Inorganic sol; 所述前驱体是正硅酸乙酯TEOS或者异丙醇铝C9H21AlO3; The precursor is ethyl orthosilicate TEOS or aluminum isopropoxide C 9 H 21 AlO 3 ; 所述第一溶剂是乙醇C2H5OH、丙酮C3H6O和乙醚C4H10O中的一种; The first solvent is one of ethanol C 2 H 5 OH, acetone C 3 H 6 O and ether C 4 H 10 O; 所述第二溶剂是乙醇C2H5OH、丙酮C3H6O和乙醚C4H10O中的一种; The second solvent is one of ethanol C 2 H 5 OH, acetone C 3 H 6 O and ether C 4 H 10 O; 步骤二:制备核壳结构填料 Step 2: Preparation of core-shell structure packing (A)在50ml的乙醇C2H5OH中加入0.2~2ml的无机盐和2~10g的粒径0.3~5μm氧化硅粉,并搅拌均匀,得到填料前驱体溶液; (A) Add 0.2-2ml of inorganic salt and 2-10g of silicon oxide powder with a particle size of 0.3-5μm to 50ml of ethanol C 2 H 5 OH, and stir evenly to obtain a filler precursor solution; 所述无机盐是钛酸四丁酯TBOT或者氧氯化锆ZrOCl2The inorganic salt is tetrabutyl titanate TBOT or zirconium oxychloride ZrOCl 2 ; (B)在10ml的去离子水中加入25~50ml的乙醇C2H5OH和1~10滴的百分比浓度为99%的浓硝酸HNO3,并搅拌均匀,得到填料反应物溶液; (B) Add 25-50 ml of ethanol C 2 H 5 OH and 1-10 drops of concentrated nitric acid HNO 3 with a percentage concentration of 99% in 10 ml of deionized water, and stir evenly to obtain a filler reactant solution; (C)将步骤(B)制得的填料反应物溶液加入至步骤(A)制得的填料前驱体溶液中,在反应温度为25~100℃、搅拌速度为400800r/min的条件下反应2~5h,反应结束后制得填料溶液; (C) Add the filler reactant solution prepared in step (B) to the filler precursor solution prepared in step (A), and react at a reaction temperature of 25-100°C and a stirring speed of 400800r/min. ~5h, the filler solution was prepared after the reaction; (D)将步骤(C)得到的填料溶液在超声功率为1000W的条件下超声处理3~10min,并在水热釜温度为140~180℃条件下水热2~24h;然后进行离心干燥得到填料; (D) ultrasonically treat the filler solution obtained in step (C) for 3 to 10 minutes under the condition of ultrasonic power of 1000 W, and heat it for 2 to 24 hours in a hydrothermal kettle at a temperature of 140 to 180 ° C; then perform centrifugal drying to obtain the filler ; 离心干燥的条件为:转速400~800r/min、干燥温度70~90℃、干燥时间2~6h; The conditions of centrifugal drying are: rotating speed 400~800r/min, drying temperature 70~90℃, drying time 2~6h; (E)将步骤(D)制得的填料在马弗炉中在300~700℃的温度下保温2~10h,得到核壳结构填料;  (E) keeping the filler prepared in step (D) in a muffle furnace at a temperature of 300 to 700°C for 2 to 10 hours to obtain a core-shell structure filler; 步骤三:制备涂层材料 Step 3: Preparation of Coating Material 将步骤二制得的核壳结构填料加入到步骤一制得的无机溶胶中,并搅拌均匀,得到无机涂层材料; adding the core-shell structure filler prepared in step 2 to the inorganic sol prepared in step 1, and stirring evenly to obtain an inorganic coating material; 用量:50ml的无机溶胶中加入2~10g的核壳结构填料。 Dosage: Add 2-10g of core-shell structure filler to 50ml of inorganic sol. 2.根据权利要求1所述的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于:步骤二中制得的核壳结构填料的粒径在0.3~5μm,壳的厚度在30~500nm之间。 2. A preparation method for forming an inorganic coating compatible with high temperature resistance, radiation heat transfer and microwave transmission according to claim 1, characterized in that: the particle size of the core-shell structure filler prepared in step 2 is between 0.3 ~5μm, the thickness of the shell is between 30~500nm. 3.根据权利要求1所述的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于:在步骤一配制过程中,第一溶剂与第二溶剂要用相同的用料。 3. A preparation method for forming an inorganic coating compatible with high temperature resistance, radiation heat transfer and microwave transmission according to claim 1, characterized in that: in the preparation process of step 1, the first solvent and the second solvent must be Use the same materials. 4.根据权利要求1所述的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于:制得的无机涂层表面均匀致密无裂纹。 4. A preparation method for forming an inorganic coating with high temperature resistance, radiation heat insulation and microwave transmission compatibility according to claim 1, characterized in that: the surface of the prepared inorganic coating is uniform and dense without cracks. 5.根据权利要求1所述的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于:100μm厚的无机涂层能够屏蔽28~60%的红外光谱,说明所述的无机涂层具有良好的隔辐射传热性能。 5. A preparation method for forming an inorganic coating with high temperature resistance, radiation heat transfer and microwave penetration compatibility according to claim 1, characterized in that: a 100 μm thick inorganic coating can shield 28 to 60% of the infrared spectrum , indicating that the inorganic coating has good radiation and heat transfer performance. 6.根据权利要求1所述的一种形成具有耐高温隔辐射传热与透微波兼容的无机涂层的制备方法,其特征在于:制得的无机涂层在介电性能上的介电常数升高低于2%和介电损耗增加5%以内,不会影响其微波透过性能。  6. A preparation method for forming an inorganic coating with high temperature resistance, radiation heat transfer and microwave penetration compatibility according to claim 1, characterized in that: the dielectric constant of the prepared inorganic coating on the dielectric property If the increase is less than 2% and the dielectric loss increases within 5%, it will not affect its microwave transmission performance. the
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Title
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