[go: up one dir, main page]

CN104860717B - A preparation method for the surface coating of rigid ceramic heat-insulating tiles - Google Patents

A preparation method for the surface coating of rigid ceramic heat-insulating tiles Download PDF

Info

Publication number
CN104860717B
CN104860717B CN201510178042.9A CN201510178042A CN104860717B CN 104860717 B CN104860717 B CN 104860717B CN 201510178042 A CN201510178042 A CN 201510178042A CN 104860717 B CN104860717 B CN 104860717B
Authority
CN
China
Prior art keywords
powder
parts
raw material
ceramic heat
spray
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510178042.9A
Other languages
Chinese (zh)
Other versions
CN104860717A (en
Inventor
钟业盛
史丽萍
李明伟
赫晓东
马晓亮
王祥宇
高岩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhu Deming New Material Technology Development Co ltd
Original Assignee
Harbin Institute of Technology Shenzhen
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology Shenzhen filed Critical Harbin Institute of Technology Shenzhen
Priority to CN201510178042.9A priority Critical patent/CN104860717B/en
Publication of CN104860717A publication Critical patent/CN104860717A/en
Application granted granted Critical
Publication of CN104860717B publication Critical patent/CN104860717B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Compositions Of Oxide Ceramics (AREA)

Abstract

The preparation method of a kind of rigid ceramic thermal insulation tile face coat, the present invention relates to the preparation method of ceramic insulation watt face coat.The invention solves the problems that Rigid Porous ceramic insulation watt is hygroscopic, non-oxidizability and the low technical problem of heat emissivity coefficient.Method: one, prepare raw material powder;Two, compound is prepared;Three, spray-on coating;Four, sintering.The coating microstrueture using the present invention to prepare has the Gradient Features of gradual change, and the coating of porous matrix side is cellular, and face coat is smooth compact shape.The existence of Porous transition layer can coordinate the expansion not matching properties of coating and matrix.The present invention is used for preparing rigid ceramic thermal insulation tile face coat.

Description

一种刚性陶瓷隔热瓦表面涂层的制备方法A preparation method for the surface coating of rigid ceramic heat-insulating tiles

技术领域technical field

本发明涉及陶瓷隔热瓦表面涂层的制备方法。The invention relates to a method for preparing a surface coating of a ceramic heat-insulating tile.

背景技术Background technique

临近空间高超声速飞行器需要在有氧和高温环境下飞行数千秒,相比于穿越近空间区域的高速飞行器(仅几十秒),其在氧化和高温环境下服役时间特别长(大两个数量级)。大气对飞行器的阻尼功的一部分最终表现为传向飞行器表面的气动加热,从而导致表面温度的急剧升高。长时间的气动加热使得头部和翼缘部分的表面温度超过2000℃,同时为保持高的升阻比和良好的气动外形,这些部位外表面不允许产生明显烧蚀。此外,随着飞行器的飞行速度向更高马赫数迈进,给飞行器表面热防护提出了更为严苛的要求。由于高辐射率涂层可以大幅提高跨大气层飞行器表面向外辐射热量的能力,能够以散热的方式降低飞行器表面温度,因此为解决跨大气层飞行器表面热防护提供了一条新的途径。陶瓷隔热瓦是美国最早在航天飞机迎风面使用的热防护材料,是一种纤维型刚性隔热材料,其主要成分为石英纤维、硼硅酸铝纤维或氧化铝纤维。经高温烧结后,纤维之间相互“搭接”形成多孔结构(孔率80-95%),赋予陶瓷隔热瓦良好的隔热性能和力学性能。与陶瓷隔热瓦相匹配的高辐射涂层技术也取得了明显进步。由于高摩擦、高温、易氧化等特殊的使用环境,这类涂层多数由耐高温的陶瓷相材料组成,对少数含有有机成分的涂层,则一般应用在温度相对较低的尾翼内侧和上表面处。根据制备工艺的不同,在陶瓷纤维隔热瓦表面制备保护涂层的主要方法有喷涂法、刷涂法和化学气相沉积法等。RCG(Reaction CuredGlass)是美国最早在哥伦比亚号航天飞机表面隔热瓦上使用的一种刚性陶瓷表面高发射率涂层,发射率在0.9-0.93之间。涂层具有耐热冲击,热膨胀系数低,防水,化学稳定性好等特点,最高可在1100℃下使用,高温下可保持良好的力学性能。但是,由于有机粘合剂甲基纤维素的存在,烧结后容易在涂层中形成挥发不均匀的现象,导致涂层变脆。TUFI(Toughened Unipiece Fibrous Insulation)涂层是在第二代刚性隔热瓦耐火纤维复合材料FRCI绝热瓦和氧化铝增强陶瓷瓦AETB上涂装的。用空气喷涂法将玻璃粘接剂和高辐射剂MoSi2的混合物涂至多孔衬底上,提高了瓦顶致密度,其抵抗破坏能力比反应固化涂层RCG提高几倍,并且具有良好的耐久性。Near-space hypersonic vehicles need to fly for thousands of seconds in an aerobic and high-temperature environment. Compared with high-speed vehicles that pass through the near-space region (only tens of seconds), their service time in an oxidative and high-temperature environment is particularly long (two Magnitude). Part of the damping work done by the atmosphere to the aircraft is finally expressed as aerodynamic heating to the surface of the aircraft, resulting in a sharp increase in the surface temperature. Long-term aerodynamic heating makes the surface temperature of the head and flange parts exceed 2000°C. At the same time, in order to maintain a high lift-to-drag ratio and a good aerodynamic shape, the outer surface of these parts is not allowed to produce obvious ablation. In addition, as the flight speed of the aircraft moves towards a higher Mach number, more stringent requirements are put forward for the thermal protection of the aircraft surface. Since the high-emissivity coating can greatly improve the ability of the surface of the transatmospheric vehicle to radiate heat outward, and can reduce the surface temperature of the vehicle through heat dissipation, it provides a new way to solve the thermal protection of the surface of the transatmospheric vehicle. Ceramic insulation tile is the earliest thermal protection material used in the United States on the windward side of the space shuttle. It is a fiber-type rigid insulation material, and its main components are quartz fiber, aluminum borosilicate fiber or alumina fiber. After high-temperature sintering, the fibers "overlap" each other to form a porous structure (80-95% porosity), which endows the ceramic tile with good thermal insulation and mechanical properties. Significant progress has also been made in the technology of high-radiation coatings that match ceramic insulation tiles. Due to the special use environment such as high friction, high temperature, and easy oxidation, most of these coatings are composed of high-temperature resistant ceramic phase materials. For a small number of coatings containing organic components, they are generally applied on the inner and upper sides of the tail with relatively low temperature. at the surface. According to different preparation processes, the main methods for preparing protective coatings on the surface of ceramic fiber insulation tiles include spraying, brushing and chemical vapor deposition. RCG (Reaction Cured Glass) is the first high-emissivity coating on the rigid ceramic surface used in the United States on the surface insulation tile of the Columbia space shuttle. The emissivity is between 0.9-0.93. The coating has the characteristics of thermal shock resistance, low thermal expansion coefficient, waterproof, and good chemical stability. It can be used at a maximum temperature of 1100 ° C, and can maintain good mechanical properties at high temperatures. However, due to the presence of the organic binder methyl cellulose, it is easy to form uneven volatilization in the coating after sintering, resulting in the coating becoming brittle. TUFI (Toughened Unipiece Fibrous Insulation) coating is applied on the second-generation rigid insulation tile refractory fiber composite material FRCI insulation tile and alumina reinforced ceramic tile AETB. The mixture of glass adhesive and high-radiation agent MoSi 2 is applied to the porous substrate by air spraying method, which improves the density of the tile roof, and its damage resistance is several times higher than that of the reaction-cured coating RCG, and has good durability sex.

发明内容Contents of the invention

本发明要解决刚性多孔陶瓷隔热瓦易吸水,抗氧化性和热辐射系数低的技术问题,而提供一种刚性陶瓷隔热瓦表面涂层的制备方法。The invention aims to solve the technical problems that the rigid porous ceramic heat-insulating tile is easy to absorb water, has low oxidation resistance and low thermal radiation coefficient, and provides a method for preparing the surface coating of the rigid ceramic heat-insulating tile.

一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:A method for preparing a surface coating of a rigid ceramic heat-insulating tile, specifically carried out according to the following steps:

一、将硼硅玻璃粉和熔融SiO2粉均匀混合,得到原料粉1,按质量份数原料粉1中硼硅玻璃粉40~60份、熔融SiO2粉为40~60份;1. Mix borosilicate glass powder and molten SiO2 powder evenly to obtain raw material powder 1. In raw material powder 1, 40-60 parts of borosilicate glass powder and fused SiO2 powder are 40-60 parts in parts by mass;

将硼硅玻璃粉、熔融SiO2粉、MoSi2粉和SiB4粉均匀混合,得到原料粉2,按质量份数原料粉2中硼硅玻璃粉为30~40份、熔融SiO2粉为30~40份、MoSi2粉为10~20份、SiB4粉为10~20份;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder and SiB4 powder uniformly to obtain raw material powder 2. In raw material powder 2 , borosilicate glass powder is 30-40 parts by mass, and fused SiO2 powder is 30 parts ~40 parts, MoSi 2 powder is 10~20 parts, SiB 4 powder is 10~20 parts;

将硼硅玻璃粉、熔融SiO2粉、MoSi2粉、SiB4粉和ZrB2粉均匀混合,得到原料粉3,按质量份数原料粉3中硼硅玻璃粉为20~30份、熔融SiO2粉为20~30份、MoSi2粉为10~20份、SiB4粉为10~20份、ZrB2粉为10~15份;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder, SiB4 powder and ZrB2 powder evenly to obtain raw material powder 3 , in parts by mass, borosilicate glass powder in raw material powder 3 is 20-30 parts, fused SiO 2 powder is 20-30 parts, MoSi 2 powder is 10-20 parts, SiB 4 powder is 10-20 parts, ZrB 2 powder is 10-15 parts;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料1;按质量份数原料粉1为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~300份;2. Put the raw material powder 1, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 10-30 minutes to obtain the mixture 1; the raw material powder 1 is 100 parts by mass, The binder is 1-5 parts, the sintering agent is 0.5-1 part, and the dispersant is 150-300 parts;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料2;按质量份数原料粉2为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Evenly mix the raw material powder 2, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill tank, and ball mill for 10-30 minutes to obtain the mixture 2; the raw material powder 2 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料3;按质量份数原料粉3为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill tank, and ball mill for 10 to 30 minutes to obtain the mixture 3; the raw material powder 3 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant;

其中粘结剂为正硅酸乙酯,烧结剂为碳化硼;The binder is ethyl orthosilicate, and the sintering agent is boron carbide;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂三~四层;再喷涂混合料2,喷涂至少三层;再喷涂混合料3,喷涂至少三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray three to four layers; then spray the mixture 2, and spray at least three layers ; Spray the mixture 3 again, spray at least three layers, and obtain a uniform and smooth coating on the surface of the ceramic heat insulating tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,然后放入马弗炉中,进行涂层烧结,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层。4. Put the ceramic heat insulating tile processed in step 3 into a constant temperature and humidity box for drying, then put it into a muffle furnace for coating sintering, and then cool with the furnace to obtain the surface coating of the rigid ceramic heat insulating tile.

所述正硅酸乙酯和碳化硼为化学分析纯,质量纯度为99%。The tetraethyl orthosilicate and boron carbide are chemically analytically pure, with a mass purity of 99%.

本发明通过优化涂层配方和控制涂层烧结温度,在多孔陶瓷瓦表面构建与基底材料具有相近热膨胀系数的复合陶瓷涂层,该功能涂层能够满足高超声速飞行器再入时严苛的工况条件,具备把气动热向外辐射的能力。By optimizing the coating formula and controlling the sintering temperature of the coating, the present invention builds a composite ceramic coating with a thermal expansion coefficient similar to that of the base material on the surface of the porous ceramic tile. This functional coating can meet the harsh working conditions of hypersonic vehicle re-entry Conditions, with the ability to radiate aerodynamic heat to the outside.

本发明的有益效果是:采用本发明制备的涂层微观结构具有渐变的梯度特征,多孔基体侧的涂层呈多孔状,表面涂层呈光滑致密状。多孔过渡层的存在能够协调涂层与基体的膨胀不匹配特性。本发明涂层具有较低的热膨胀系数0.8~3.0×10-6K-1,涂层中的高辐射剂发挥高辐射的作用,制备态涂层的辐射系数不小于0.90。根据基体状态和工况条件的实验需要,调节三种混合料浆的配比,获得与基体匹配的最优涂层。The beneficial effects of the invention are: the microstructure of the coating prepared by the invention has a gradually changing gradient feature, the coating on the side of the porous substrate is porous, and the surface coating is smooth and compact. The existence of the porous transition layer can coordinate the expansion mismatch characteristics of the coating and the substrate. The coating of the invention has a relatively low coefficient of thermal expansion of 0.8 to 3.0×10 -6 K -1 , the high radiation agent in the coating plays a role of high radiation, and the radiation coefficient of the prepared coating is not less than 0.90. According to the experimental needs of the substrate state and working conditions, adjust the ratio of the three mixed slurries to obtain the optimal coating that matches the substrate.

本发明用于制备刚性陶瓷隔热瓦表面涂层。The invention is used for preparing the surface coating of rigid ceramic heat-insulating tiles.

附图说明Description of drawings

图1为实施例一~四制备的刚性陶瓷隔热瓦表面涂层的热膨胀系数曲线图,其中1代表陶瓷瓦未处理表面、2代表实施例一、3代表实施例二、4代表实施例三、5代表实施例四;Fig. 1 is the thermal expansion coefficient curve diagram of the surface coating of the rigid ceramic heat-insulating tile prepared in Examples 1-4, wherein 1 represents the untreated surface of the ceramic tile, 2 represents Embodiment 1, 3 represents Embodiment 2, and 4 represents Embodiment 3 , 5 represent embodiment four;

图2为实施例一制备的刚性陶瓷隔热瓦表面涂层的截面电子扫描图;Fig. 2 is the cross-sectional electronic scanning diagram of the surface coating of the rigid ceramic heat-insulating tile prepared in embodiment one;

图3为实施例二制备的刚性陶瓷隔热瓦表面涂层在不同热震循环后的辐射系数曲线图。Fig. 3 is a curve diagram of the emissivity of the surface coating of the rigid ceramic heat-insulating tile prepared in Example 2 after different thermal shock cycles.

具体实施方式detailed description

本发明技术方案不局限于以下所列举的具体实施方式,还包括各具体实施方式之间的任意组合。The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.

具体实施方式一:本实施方式一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:Embodiment 1: In this embodiment, a method for preparing a surface coating of a rigid ceramic heat-insulating tile is specifically carried out in accordance with the following steps:

一、将硼硅玻璃粉和熔融SiO2粉均匀混合,得到原料粉1,按质量份数原料粉1中硼硅玻璃粉40~60份、熔融SiO2粉为40~60份;1. Mix borosilicate glass powder and molten SiO2 powder evenly to obtain raw material powder 1. In raw material powder 1, 40-60 parts of borosilicate glass powder and fused SiO2 powder are 40-60 parts in parts by mass;

将硼硅玻璃粉、熔融SiO2粉、MoSi2粉和SiB4粉均匀混合,得到原料粉2,按质量份数原料粉2中硼硅玻璃粉为30~40份、熔融SiO2粉为30~40份、MoSi2粉为10~20份、SiB4粉为10~20份;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder and SiB4 powder uniformly to obtain raw material powder 2. In raw material powder 2 , borosilicate glass powder is 30-40 parts by mass, and fused SiO2 powder is 30 parts ~40 parts, MoSi 2 powder is 10~20 parts, SiB 4 powder is 10~20 parts;

将硼硅玻璃粉、熔融SiO2粉、MoSi2粉、SiB4粉和ZrB2粉均匀混合,得到原料粉3,按质量份数原料粉3中硼硅玻璃粉为20~30份、熔融SiO2粉为20~30份、MoSi2粉为10~20份、SiB4粉为10~20份、ZrB2粉为10~15份;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder, SiB4 powder and ZrB2 powder evenly to obtain raw material powder 3 , in parts by mass, borosilicate glass powder in raw material powder 3 is 20-30 parts, fused SiO 2 powder is 20-30 parts, MoSi 2 powder is 10-20 parts, SiB 4 powder is 10-20 parts, ZrB 2 powder is 10-15 parts;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料1;按质量份数原料粉1为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~300份;2. Put the raw material powder 1, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 10-30 minutes to obtain the mixture 1; the raw material powder 1 is 100 parts by mass, The binder is 1-5 parts, the sintering agent is 0.5-1 part, and the dispersant is 150-300 parts;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料2;按质量份数原料粉2为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Evenly mix the raw material powder 2, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill tank, and ball mill for 10-30 minutes to obtain the mixture 2; the raw material powder 2 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料3;按质量份数原料粉3为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill tank, and ball mill for 10 to 30 minutes to obtain the mixture 3; the raw material powder 3 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant;

其中粘结剂为正硅酸乙酯,烧结剂为碳化硼;The binder is ethyl orthosilicate, and the sintering agent is boron carbide;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂三~四层;再喷涂混合料2,喷涂至少三层;再喷涂混合料3,喷涂至少三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray three to four layers; then spray the mixture 2, and spray at least three layers ; Spray the mixture 3 again, spray at least three layers, and obtain a uniform and smooth coating on the surface of the ceramic heat insulating tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,然后放入马弗炉中,进行涂层烧结,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层。4. Put the ceramic heat insulating tile processed in step 3 into a constant temperature and humidity box for drying, then put it into a muffle furnace for coating sintering, and then cool with the furnace to obtain the surface coating of the rigid ceramic heat insulating tile.

具体实施方式二:本实施方式与具体实施方式一不同的是:步骤一中硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为10~20%。其它与具体实施方式一相同。Embodiment 2: This embodiment differs from Embodiment 1 in that in Step 1, borosilicate glass powder is synthesized by melting silicon oxide and boron oxide at a high temperature of 1100° C., wherein the weight content of boron oxide is 10-20%. Others are the same as in the first embodiment.

具体实施方式三:本实施方式与具体实施方式一不同的是:步骤一中硼硅玻璃粉平均粒径为2~10μm;熔融SiO2粉中SiO2质量含量大于98%,平均粒径为2~10μm;MoSi2粉的平均粒径为1~4μm;SiB4粉的平均粒径为10~50μm;ZrB2粉的平均粒径为20~50μm。其它与具体实施方式一相同。Specific embodiment three: the difference between this embodiment and specific embodiment one is: the average particle diameter of borosilicate glass powder in step one is 2~10 μ m; SiO2 mass content is greater than 98% in the molten SiO2 powder, and average particle diameter is 2 ~10μm; the average particle size of MoSi 2 powder is 1~4μm; the average particle size of SiB 4 powder is 10~50μm; the average particle size of ZrB 2 powder is 20~50μm. Others are the same as in the first embodiment.

具体实施方式四:本实施方式与具体实施方式一不同的是:步骤二中球料重量比均为(3~4)∶1。其它与具体实施方式一相同。Embodiment 4: The difference between this embodiment and Embodiment 1 is that the weight ratio of balls to materials in step 2 is (3-4):1. Others are the same as in the first embodiment.

具体实施方式五:本实施方式与具体实施方式一不同的是:步骤二中分散剂为纯净水。其它与具体实施方式一相同。Embodiment 5: The difference between this embodiment and Embodiment 1 is that the dispersant in step 2 is pure water. Others are the same as in the first embodiment.

具体实施方式六:本实施方式与具体实施方式一不同的是:步骤三中所述空气喷涂法的工艺参数为:空气压力0.1~0.3MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面5~10厘米。其它与具体实施方式一相同。Embodiment 6: This embodiment differs from Embodiment 1 in that the process parameters of the air spraying method described in step 3 are: air pressure 0.1 to 0.3 MPa, the nozzle is perpendicular to the surface to be sprayed, and the distance from the spray gun mouth to the sprayed surface is 5 ~10 cm. Others are the same as in the first embodiment.

具体实施方式七:本实施方式与具体实施方式一不同的是:步骤四中干燥时控制干燥温度为70~90℃,湿度为40~50%。其它与具体实施方式一相同。Embodiment 7: This embodiment is different from Embodiment 1 in that: in step 4, during drying, the drying temperature is controlled to be 70-90° C., and the humidity is 40-50%. Others are the same as in the first embodiment.

具体实施方式八:本实施方式与具体实施方式七不同的是:步骤四中干燥时控制干燥温度为80℃。其它与具体实施方式七相同。Embodiment 8: This embodiment is different from Embodiment 7 in that: in step 4, the drying temperature is controlled to be 80° C. during drying. Others are the same as in the seventh embodiment.

具体实施方式九:本实施方式与具体实施方式一不同的是:步骤四所述涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为900~1100℃条件下保温0.5h~1h,控制升温速率为5℃/min。其它与具体实施方式一相同。Embodiment 9: The difference between this embodiment and Embodiment 1 is that the coating sintering process described in step 4 is: heat preservation at a temperature of 200°C for 0.5h, and then heat preservation at a temperature of 900-1100°C for 0.5 h~1h, control the heating rate to 5°C/min. Others are the same as in the first embodiment.

采用以下实施例验证本发明的有益效果:Adopt the following examples to verify the beneficial effects of the present invention:

实施例一:Embodiment one:

本实施例一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:In this embodiment, a method for preparing the surface coating of a rigid ceramic heat-insulating tile is specifically carried out in accordance with the following steps:

一、将50g硼硅玻璃粉和50g熔融SiO2粉均匀混合,得到原料粉1;1. Uniformly mix 50g of borosilicate glass powder and 50g of fused SiO2 powder to obtain raw material powder 1;

将40g硼硅玻璃粉、40g熔融SiO2粉、10g MoSi2粉和10g SiB4粉均匀混合,得到原料粉2;40g borosilicate glass powder, 40g fused SiO powder, 10g MoSi powder and 10g SiB powder were evenly mixed to obtain raw material powder 2 ;

将30g硼硅玻璃粉、30g熔融SiO2粉、15g MoSi2粉、15g SiB4粉和10g ZrB2粉均匀混合,得到原料粉3;30g of borosilicate glass powder, 30g of fused SiO2 powder, 15g of MoSi2 powder, 15g of SiB4 powder and 10g of ZrB2 powder were uniformly mixed to obtain raw material powder 3 ;

步骤一中硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为10%;In step 1, borosilicate glass powder is synthesized by melting silicon oxide and boron oxide at a high temperature of 1100°C, wherein the weight content of boron oxide is 10%;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料1;原料粉1为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1g、分散剂为纯净水200g;2. Evenly mix the raw material powder 1, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 1; the raw material powder 1 is 100g, and the binder is orthosilicic acid Ethyl ester 5g, sintering agent is boron carbide 1g, dispersant is purified water 200g;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料2;原料粉2为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.6g、分散剂为纯净水200g;Put the raw material powder 2, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 20 minutes to obtain the mixture 2; the raw material powder 2 is 100g, and the binder is ethyl orthosilicate 5g, the sintering agent is boron carbide 1.6g, the dispersant is 200g of purified water;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料3;原料粉3为100g、粘结剂为正硅酸乙酯3g、烧结剂为碳化硼0.6g、分散剂为纯净水200g;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 3; the raw material powder 3 is 100g, and the binder is tetraethyl orthosilicate 3g, the sintering agent is 0.6g of boron carbide, and the dispersant is 200g of purified water;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂三层;再喷涂混合料2,喷涂三层;再喷涂混合料3,喷涂三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray three layers; then spray the mixture 2, spray three layers; and then spray Mixture 3, spray three layers to obtain a uniform and smooth coating on the surface of the ceramic heat insulation tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,控制干燥温度为80℃,湿度为40%,然后放入马弗炉中,进行涂层烧结,涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为1000℃条件下保温1h,控制升温速率为5℃/min,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层;4. Put the ceramic heat-insulating tiles processed in step 3 into a constant temperature and humidity box for drying. Control the drying temperature at 80°C and humidity at 40%, and then put them into a muffle furnace for coating sintering and coating sintering The process is: heat preservation at 200°C for 0.5h, then heat preservation at 1000°C for 1h, control the heating rate at 5°C/min, and then cool with the furnace to obtain the surface coating of rigid ceramic heat-insulating tiles;

步骤三中所述空气喷涂法的工艺参数为:空气压力0.2MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面8厘米。The process parameters of the air spraying method described in step 3 are: air pressure 0.2 MPa, nozzle perpendicular to the surface to be sprayed, and distance from the nozzle of the spray gun to the surface to be sprayed is 8 cm.

实施例二:Embodiment two:

本实施例一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:In this embodiment, a method for preparing the surface coating of a rigid ceramic heat-insulating tile is specifically carried out in accordance with the following steps:

一、将60g硼硅玻璃粉和40g熔融SiO2粉均匀混合,得到原料粉1;1. Uniformly mix 60g of borosilicate glass powder and 40g of fused SiO2 powder to obtain raw material powder 1;

将40g硼硅玻璃粉、30g熔融SiO2粉、15g MoSi2粉和15g SiB4粉均匀混合,得到原料粉2;40g borosilicate glass powder, 30g fused SiO powder, 15g MoSi powder and 15g SiB powder were evenly mixed to obtain raw material powder 2 ;

将40g硼硅玻璃粉、20g熔融SiO2粉、15g MoSi2粉、15g SiB4粉和10g ZrB2粉均匀混合,得到原料粉3;40g of borosilicate glass powder, 20g of molten SiO2 powder, 15g of MoSi2 powder, 15g of SiB4 powder and 10g of ZrB2 powder were uniformly mixed to obtain raw material powder 3 ;

步骤一中硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为15%;In step 1, borosilicate glass powder is synthesized by melting silicon oxide and boron oxide at a high temperature of 1100°C, wherein the weight content of boron oxide is 15%;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料1;原料粉1为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.2g、分散剂为纯净水300g;2. Evenly mix the raw material powder 1, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 1; the raw material powder 1 is 100g, and the binder is orthosilicic acid Ethyl ester 5g, sintering agent is boron carbide 1.2g, dispersant is pure water 300g;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料2;原料粉2为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.6g、分散剂为纯净水220g;Put the raw material powder 2, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 20 minutes to obtain the mixture 2; the raw material powder 2 is 100g, and the binder is ethyl orthosilicate 5g, sintering agent is boron carbide 1.6g, dispersant is pure water 220g;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料3;原料粉3为100g、粘结剂为正硅酸乙酯3g、烧结剂为碳化硼0.6g、分散剂为纯净水220g;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 3; the raw material powder 3 is 100g, and the binder is tetraethyl orthosilicate 3g, the sintering agent is 0.6g of boron carbide, and the dispersant is 220g of purified water;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂四层;再喷涂混合料2,喷涂四层;再喷涂混合料3,喷涂四层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray four layers; then spray the mixture 2, spray four layers; and then spray Mixture 3, spray four layers to obtain a uniform and smooth coating on the surface of the ceramic heat insulation tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,控制干燥温度为90℃,湿度为40%,然后放入马弗炉中,进行涂层烧结,涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为1000℃条件下保温1h,控制升温速率为5℃/min,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层;4. Put the ceramic heat-insulating tiles processed in step 3 into a constant temperature and humidity box for drying. The drying temperature is controlled at 90°C and the humidity is 40%, and then put into a muffle furnace for coating sintering and coating sintering The process is: heat preservation at 200°C for 0.5h, then heat preservation at 1000°C for 1h, control the heating rate at 5°C/min, and then cool with the furnace to obtain the surface coating of rigid ceramic heat-insulating tiles;

步骤三中所述空气喷涂法的工艺参数为:空气压力0.2MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面8厘米。The process parameters of the air spraying method described in step 3 are: air pressure 0.2 MPa, nozzle perpendicular to the surface to be sprayed, and distance from the nozzle of the spray gun to the surface to be sprayed is 8 cm.

实施例三:Embodiment three:

本实施例一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:In this embodiment, a method for preparing the surface coating of a rigid ceramic heat-insulating tile is specifically carried out in accordance with the following steps:

一、将40g硼硅玻璃粉和60g熔融SiO2粉均匀混合,得到原料粉1;1. Evenly mix 40g of borosilicate glass powder and 60g of molten SiO2 powder to obtain raw material powder 1;

将40g硼硅玻璃粉、30g熔融SiO2粉、20g MoSi2粉和10g SiB4粉均匀混合,得到原料粉2;40g borosilicate glass powder, 30g fused SiO powder, 20g MoSi powder and 10g SiB powder were evenly mixed to obtain raw material powder 2 ;

将40g硼硅玻璃粉、20g熔融SiO2粉、10g MoSi2粉、15g SiB4粉和15g ZrB2粉均匀混合,得到原料粉3;40g of borosilicate glass powder, 20g of molten SiO2 powder, 10g of MoSi2 powder, 15g of SiB4 powder and 15g of ZrB2 powder were uniformly mixed to obtain raw material powder 3 ;

步骤一中硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为20%;In step 1, borosilicate glass powder is synthesized by melting silicon oxide and boron oxide at a high temperature of 1100°C, wherein the weight content of boron oxide is 20%;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料1;原料粉1为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.2g、分散剂为纯净水250g;2. Evenly mix the raw material powder 1, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 1; the raw material powder 1 is 100g, and the binder is orthosilicic acid Ethyl ester 5g, sintering agent is boron carbide 1.2g, dispersant is purified water 250g;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料2;原料粉2为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.6g、分散剂为纯净水220g;Put the raw material powder 2, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 20 minutes to obtain the mixture 2; the raw material powder 2 is 100g, and the binder is ethyl orthosilicate 5g, sintering agent is boron carbide 1.6g, dispersant is pure water 220g;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料3;原料粉3为100g、粘结剂为正硅酸乙酯3g、烧结剂为碳化硼0.6g、分散剂为纯净水220g;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 3; the raw material powder 3 is 100g, and the binder is tetraethyl orthosilicate 3g, the sintering agent is 0.6g of boron carbide, and the dispersant is 220g of purified water;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂四层;再喷涂混合料2,喷涂四层;再喷涂混合料3,喷涂三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray four layers; then spray the mixture 2, spray four layers; and then spray Mixture 3, spray three layers to obtain a uniform and smooth coating on the surface of the ceramic heat insulation tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,控制干燥温度为90℃,湿度为50%,然后放入马弗炉中,进行涂层烧结,涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为1000℃条件下保温1h,控制升温速率为5℃/min,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层;4. Put the ceramic heat-insulating tiles processed in step 3 into a constant temperature and humidity box for drying. The drying temperature is controlled at 90°C and the humidity is 50%, and then put into a muffle furnace for coating sintering and coating sintering The process is: heat preservation at 200°C for 0.5h, then heat preservation at 1000°C for 1h, control the heating rate at 5°C/min, and then cool with the furnace to obtain the surface coating of rigid ceramic heat-insulating tiles;

步骤三中所述空气喷涂法的工艺参数为:空气压力0.2MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面8厘米。The process parameters of the air spraying method described in step 3 are: air pressure 0.2 MPa, nozzle perpendicular to the surface to be sprayed, and distance from the nozzle of the spray gun to the surface to be sprayed is 8 cm.

实施例四:Embodiment four:

本实施例一种刚性陶瓷隔热瓦表面涂层的制备方法,具体是按照以下步骤进行的:In this embodiment, a method for preparing the surface coating of a rigid ceramic heat-insulating tile is specifically carried out in accordance with the following steps:

一、将55g硼硅玻璃粉和45g熔融SiO2粉均匀混合,得到原料粉1;1. Uniformly mix 55g of borosilicate glass powder and 45g of fused SiO2 powder to obtain raw material powder 1;

将30g硼硅玻璃粉、40g熔融SiO2粉、20g MoSi2粉和10g SiB4粉均匀混合,得到原料粉2;30g borosilicate glass powder, 40g fused SiO powder, 20g MoSi powder and 10g SiB powder were evenly mixed to obtain raw material powder 2 ;

将30g硼硅玻璃粉、30g熔融SiO2粉、10g MoSi2粉、15g SiB4粉和15g ZrB2粉均匀混合,得到原料粉3;30g of borosilicate glass powder, 30g of molten SiO2 powder, 10g of MoSi2 powder, 15g of SiB4 powder and 15g of ZrB2 powder were uniformly mixed to obtain raw material powder 3 ;

步骤一中硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为20%;In step 1, borosilicate glass powder is synthesized by melting silicon oxide and boron oxide at a high temperature of 1100°C, wherein the weight content of boron oxide is 20%;

二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料1;原料粉1为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.2g、分散剂为纯净水250g;2. Evenly mix the raw material powder 1, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 1; the raw material powder 1 is 100g, and the binder is orthosilicic acid Ethyl ester 5g, sintering agent is boron carbide 1.2g, dispersant is purified water 250g;

将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料2;原料粉2为100g、粘结剂为正硅酸乙酯5g、烧结剂为碳化硼1.6g、分散剂为纯净水220g;Put the raw material powder 2, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 20 minutes to obtain the mixture 2; the raw material powder 2 is 100g, and the binder is ethyl orthosilicate 5g, sintering agent is boron carbide 1.6g, dispersant is pure water 220g;

将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨20min,得到混合料3;原料粉3为100g、粘结剂为正硅酸乙酯3g、烧结剂为碳化硼0.8g、分散剂为纯净水220g;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill jar, and mill for 20 minutes to obtain the mixture 3; the raw material powder 3 is 100g, and the binder is tetraethyl orthosilicate 3g, the sintering agent is 0.8g of boron carbide, and the dispersant is 220g of purified water;

三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂三层;再喷涂混合料2,喷涂四层;再喷涂混合料3,喷涂三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat-insulating tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat-insulating tile, spray three layers; then spray the mixture 2, spray four layers; and then spray Mixture 3, spray three layers to obtain a uniform and smooth coating on the surface of the ceramic heat insulation tile;

四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,控制干燥温度为90℃,湿度为40%,然后放入马弗炉中,进行涂层烧结,涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为1000℃条件下保温1h,控制升温速率为5℃/min,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层;4. Put the ceramic heat-insulating tiles processed in step 3 into a constant temperature and humidity box for drying. The drying temperature is controlled at 90°C and the humidity is 40%, and then put into a muffle furnace for coating sintering and coating sintering The process is: heat preservation at 200°C for 0.5h, then heat preservation at 1000°C for 1h, control the heating rate at 5°C/min, and then cool with the furnace to obtain the surface coating of rigid ceramic heat-insulating tiles;

步骤三中所述空气喷涂法的工艺参数为:空气压力0.2MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面8厘米。The process parameters of the air spraying method described in step 3 are: air pressure 0.2 MPa, nozzle perpendicular to the surface to be sprayed, and distance from the nozzle of the spray gun to the surface to be sprayed is 8 cm.

实施例一~四制备的刚性陶瓷隔热瓦表面涂层的热膨胀系数曲线图如图1所示,其中1代表陶瓷隔热瓦的未处理表面、2代表实施例一、3代表实施例二、4代表实施例三、5代表实施例四。The thermal expansion coefficient curves of the surface coatings of rigid ceramic heat-insulating tiles prepared in Examples 1-4 are shown in Figure 1, where 1 represents the untreated surface of ceramic heat-insulating tiles, 2 represents Embodiment 1, and 3 represents Embodiment 2. 4 represents embodiment three, and 5 represents embodiment four.

实施例一制备的刚性陶瓷隔热瓦表面涂层的截面电子扫描图如图2所示。The cross-sectional electronic scanning diagram of the surface coating of the rigid ceramic heat-insulating tile prepared in Example 1 is shown in FIG. 2 .

实施例二制备的刚性陶瓷隔热瓦表面涂层在不同热震循环后的辐射系数曲线图如图3所示。The emissivity curves of the surface coating of the rigid ceramic heat-insulating tile prepared in Example 2 after different thermal shock cycles are shown in FIG. 3 .

由附图可知,采用低成本的大气喷涂法能够在刚性陶瓷隔热瓦表面获得热膨胀系数低、抗热震性能好且具有多孔微观结构特征的高辐射涂层。It can be seen from the drawings that a high-radiation coating with low thermal expansion coefficient, good thermal shock resistance and porous microstructure can be obtained on the surface of rigid ceramic heat-insulating tiles by using the low-cost atmospheric spraying method.

Claims (8)

1.一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于该方法具体是按照以下步骤进行的:1. A preparation method for the surface coating of rigid ceramic heat-insulating tiles, characterized in that the method is specifically carried out according to the following steps: 一、将硼硅玻璃粉和熔融SiO2粉均匀混合,得到原料粉1,按质量份数原料粉1中硼硅玻璃粉40~60份、熔融SiO2粉为40~60份;1. Mix borosilicate glass powder and molten SiO2 powder evenly to obtain raw material powder 1. In raw material powder 1, 40-60 parts of borosilicate glass powder and fused SiO2 powder are 40-60 parts in parts by mass; 将硼硅玻璃粉、熔融SiO2粉、MoSi2粉和SiB4粉均匀混合,得到原料粉2,按质量份数原料粉2中硼硅玻璃粉为30~40份、熔融SiO2粉为30~40份、MoSi2粉为10~20份、SiB4粉为10~20份;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder and SiB4 powder uniformly to obtain raw material powder 2. In raw material powder 2 , borosilicate glass powder is 30-40 parts by mass, and fused SiO2 powder is 30 parts ~40 parts, MoSi 2 powder is 10~20 parts, SiB 4 powder is 10~20 parts; 将硼硅玻璃粉、熔融SiO2粉、MoSi2粉、SiB4粉和ZrB2粉均匀混合,得到原料粉3,按质量份数原料粉3中硼硅玻璃粉为20~30份、熔融SiO2粉为20~30份、MoSi2粉为10~20份、SiB4粉为10~20份、ZrB2粉为10~15份;所述硼硅玻璃粉是通过氧化硅和氧化硼经高温1100℃熔融合成,其中氧化硼重量含量为10~20%;Mix borosilicate glass powder, fused SiO2 powder, MoSi2 powder, SiB4 powder and ZrB2 powder evenly to obtain raw material powder 3 , in parts by mass, borosilicate glass powder in raw material powder 3 is 20-30 parts, fused SiO 2 powder is 20-30 parts, MoSi 2 powder is 10-20 parts, SiB 4 powder is 10-20 parts, ZrB 2 powder is 10-15 parts; the borosilicate glass powder is made by silicon oxide and boron oxide at high temperature Fusion synthesis at 1100°C, wherein the weight content of boron oxide is 10-20%; 二、将步骤一得到的原料粉1、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料1;按质量份数原料粉1为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~300份;2. Put the raw material powder 1, binder, sintering agent and dispersant obtained in step 1 into a ball mill jar after uniform mixing, and ball mill for 10-30 minutes to obtain the mixture 1; the raw material powder 1 is 100 parts by mass, The binder is 1-5 parts, the sintering agent is 0.5-1 part, and the dispersant is 150-300 parts; 将步骤一得到的原料粉2、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料2;按质量份数原料粉2为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Evenly mix the raw material powder 2, binder, sintering agent and dispersant obtained in step 1, put them into a ball mill tank, and ball mill for 10-30 minutes to obtain the mixture 2; the raw material powder 2 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant; 将步骤一得到的原料粉3、粘结剂、烧结剂和分散剂均匀混合后放入球磨罐中,球磨10~30min,得到混合料3;按质量份数原料粉3为100份、粘结剂为1~5份、烧结剂为0.5~1份、分散剂为150~250份;Mix the raw material powder 3, binder, sintering agent and dispersant obtained in step 1 evenly, put them into a ball mill tank, and ball mill for 10 to 30 minutes to obtain the mixture 3; the raw material powder 3 is 100 parts by mass, and the bonding 1 to 5 parts of sintering agent, 0.5 to 1 part of sintering agent, and 150 to 250 parts of dispersant; 其中粘结剂为正硅酸乙酯,烧结剂为碳化硼;The binder is ethyl orthosilicate, and the sintering agent is boron carbide; 三、将陶瓷隔热瓦表面进行前处理,然后采用空气喷涂法将步骤二得到的混合料1均匀喷涂在陶瓷隔热瓦表面,喷涂三~四层;再喷涂混合料2,喷涂至少三层;再喷涂混合料3,喷涂至少三层,在陶瓷隔热瓦表面获得均匀平整的涂层;3. Pre-treat the surface of the ceramic heat insulation tile, and then use the air spray method to evenly spray the mixture 1 obtained in step 2 on the surface of the ceramic heat insulation tile, spray three to four layers; then spray the mixture 2, and spray at least three layers ; Spray the mixture 3 again, spray at least three layers, and obtain a uniform and smooth coating on the surface of the ceramic heat insulating tile; 四、将步骤三处理的陶瓷隔热瓦放入恒温恒湿箱中,进行干燥,然后放入马弗炉中,进行涂层烧结,再随炉冷却,获得刚性陶瓷隔热瓦表面涂层。4. Put the ceramic heat insulating tile processed in step 3 into a constant temperature and humidity box for drying, then put it into a muffle furnace for coating sintering, and then cool with the furnace to obtain the surface coating of the rigid ceramic heat insulating tile. 2.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤一中硼硅玻璃粉平均粒径为2~10μm;熔融SiO2粉中SiO2质量含量大于98%,平均粒径为2~10μm;MoSi2粉的平均粒径为1~4μm;SiB4粉的平均粒径为10~50μm;ZrB2粉的平均粒径为20~50μm。2. The preparation method of a surface coating of a rigid ceramic heat-insulating tile according to claim 1, wherein the average particle diameter of the borosilicate glass powder in step 1 is 2 to 10 μm; the SiO mass content in the molten SiO powder is More than 98%, the average particle size is 2-10 μm; the average particle size of MoSi 2 powder is 1-4 μm; the average particle size of SiB 4 powder is 10-50 μm; the average particle size of ZrB 2 powder is 20-50 μm. 3.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤二中球料重量比均为(3~4)∶1。3. The method for preparing a surface coating of a rigid ceramic heat-insulating tile according to claim 1, wherein the weight ratio of balls to materials in step 2 is (3-4):1. 4.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤二中分散剂为纯净水。4. The method for preparing a surface coating of a rigid ceramic heat-insulating tile according to claim 1, wherein the dispersant in step 2 is pure water. 5.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤三中所述空气喷涂法的工艺参数为:空气压力0.1~0.3MPa,喷嘴垂直于被喷涂表面,喷枪口距离喷涂表面5~10厘米。5. A method for preparing a surface coating of a rigid ceramic heat-insulating tile according to claim 1, characterized in that the process parameters of the air spraying method in step 3 are: air pressure 0.1-0.3 MPa, nozzle perpendicular to the Spray the surface, the nozzle of the spray gun is 5 to 10 cm away from the surface to be sprayed. 6.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤四中干燥时控制干燥温度为70~90℃,湿度为40~50%。6. A method for preparing a surface coating of a rigid ceramic heat-insulating tile according to claim 1, characterized in that the drying temperature is controlled to be 70-90°C and the humidity is 40-50% during drying in step 4. 7.根据权利要求6所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤四中干燥时控制干燥温度为80℃。7 . The method for preparing a surface coating of a rigid ceramic heat-insulating tile according to claim 6 , wherein the drying temperature is controlled to be 80° C. during drying in step 4. 7 . 8.根据权利要求1所述的一种刚性陶瓷隔热瓦表面涂层的制备方法,其特征在于步骤四所述涂层烧结工艺为:在温度为200℃条件下保温0.5h,然后在温度为900~1100℃条件下保温0.5h~1h,控制升温速率为5℃/min。8. The preparation method of a surface coating of a rigid ceramic heat-insulating tile according to claim 1, wherein the coating sintering process described in step 4 is as follows: heat preservation at a temperature of 200°C for 0.5h, and then at a temperature of Keep the temperature at 900-1100°C for 0.5h-1h, and control the heating rate at 5°C/min.
CN201510178042.9A 2015-04-15 2015-04-15 A preparation method for the surface coating of rigid ceramic heat-insulating tiles Active CN104860717B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510178042.9A CN104860717B (en) 2015-04-15 2015-04-15 A preparation method for the surface coating of rigid ceramic heat-insulating tiles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510178042.9A CN104860717B (en) 2015-04-15 2015-04-15 A preparation method for the surface coating of rigid ceramic heat-insulating tiles

Publications (2)

Publication Number Publication Date
CN104860717A CN104860717A (en) 2015-08-26
CN104860717B true CN104860717B (en) 2016-11-23

Family

ID=53906959

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510178042.9A Active CN104860717B (en) 2015-04-15 2015-04-15 A preparation method for the surface coating of rigid ceramic heat-insulating tiles

Country Status (1)

Country Link
CN (1) CN104860717B (en)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105502946B (en) * 2015-09-30 2017-11-10 航天特种材料及工艺技术研究所 A kind of high emissivity glass glaze and the method that high emissivity coating is prepared by the glaze
CN105198480B (en) * 2015-10-29 2017-07-14 中原工学院 A kind of preparation method of molybdenum disilicide/silicon carbide compound porous ceramics
CN106083115B (en) * 2016-06-12 2019-07-02 山东工业陶瓷研究设计院有限公司 The thermal insulation tile coating and preparation method thereof of resistance to 1500 DEG C of high temperature
CN106380205B (en) * 2016-08-29 2019-09-27 天津大学 A kind of BAS based high-temp-resistant emission coating and preparation method
CN107603286B (en) * 2017-09-11 2019-08-09 山东工业陶瓷研究设计院有限公司 Rigid thermal insulation tile coating of 1500 DEG C of unburned heatproof and preparation method thereof
CN107556885B (en) * 2017-10-26 2019-11-08 中国科学院理化技术研究所 A kind of near-infrared radiation ceramic coating for ethylene cracking furnace and its preparation method and application
CN108658626B (en) * 2018-05-25 2020-10-09 莱芜亚赛陶瓷技术有限公司 MoSi2-SiO2-borosilicate high-temperature-resistant high-emissivity coating and preparation method and application thereof
CN110342916B (en) * 2019-08-20 2021-11-30 北京电子工程总体研究所 High-temperature-resistant and high-radiation-resistant powder, preparation thereof, coating slurry containing same, coating and application
CN113024280A (en) * 2021-02-26 2021-06-25 天津大学 Preparation method of double-layer silicon-oxygen-carbon composite ceramic coating for porous ceramic heat insulation matrix
CN113307659B (en) * 2021-06-10 2022-04-08 航天特种材料及工艺技术研究所 A kind of preparation method of forming high emissivity coating on insulating tile

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102137950A (en) * 2008-03-21 2011-07-27 株式会社Ihi Coating structure and surface treating method
CN101648817B (en) * 2009-08-28 2011-12-28 中材高新材料股份有限公司 High temperature resistance low-expansion high-radiation (reflecting) inorganic waterproof coating
CN103467074B (en) * 2013-08-19 2016-01-13 航天特种材料及工艺技术研究所 A kind of high-temperaure coating and preparation method thereof

Also Published As

Publication number Publication date
CN104860717A (en) 2015-08-26

Similar Documents

Publication Publication Date Title
CN104860717B (en) A preparation method for the surface coating of rigid ceramic heat-insulating tiles
CN106699209B (en) The preparation method of continuous alumina fiber enhancing alumina ceramic-base composites
US9126873B2 (en) Process for producing a self-healing layer on a part made of a C/C composite
CN107814591A (en) A kind of carbon material surface boride is modified the preparation method of silicon substrate antioxidant coating
CN104591782B (en) MoSi 2-BSG coated zirconia fiberboard integrated heat-insulating material and preparation method thereof
CN102303981A (en) Method for preparing ceramic-based composite material environment barrier coating by laser cladding
CN103724042B (en) A kind of lamination mixes the preparation method of solar heat protection sandwich
CN106966753B (en) A kind of preparation method of C/Al-Si-X anti-ablation composite material
CN104451525A (en) Thermal barrier coating with heat radiation performance and preparation method thereof
CN111747764A (en) Preparation method of silicon carbide fiber reinforced silicon carbide composites with in situ generation of ZrB2-ZrC
CN112142486A (en) Preparation method of ablation resistant silicon carbide fiber reinforced ceramic matrix composites
CN110240488A (en) A kind of high temperature resistant wave-permeable ceramic matric composite and preparation method thereof
CN102807394B (en) Method for preparing high temperature oxidation resisting coating on surface of carbon material
CN104862687B (en) A kind of preparation method of metal thermal protection struc ture face coat
CN110407597A (en) A kind of rare earth oxide modified silicon carbide ceramic matrix composite material and preparation method thereof
CN109400173A (en) A kind of boron nitride fiber enhancing nitride ceramic composites and preparation method thereof
CN112937048B (en) Ablation-resistant gradient-distribution heat-proof composite material with surface coated with high-temperature infrared stealth coating and preparation method thereof
CN107311684A (en) A kind of dissipation heat-resistant composite material and preparation method thereof
CN103738012A (en) Preparation method of ceramic matrix composite material with SiC/ZrC laminated distribution
CN107603286A (en) Rigid thermal insulation tile coating of unburned 1500 DEG C of heatproof and preparation method thereof
CN106966763B (en) Fibre-reinforced composite material surface coating and preparation method thereof under a kind of engine environmental
CN107353041A (en) SiC/SiC composite material surface coating systems and preparation method thereof
CN106882976A (en) A kind of preparation method of C/HfC-ZrC-SiC composites
CN109704816A (en) A kind of high temperature self-healing multiphase coating formed on base material and preparation method and application thereof
CN103724040B (en) Preparation method of SiC-ZrC segmented ceramic matrix composite spray pipe

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20210202

Address after: Building 1, Kechuang headquarters, Shenzhen (Harbin) Industrial Park, 288 Zhigu street, Songbei District, Harbin City, Heilongjiang Province

Patentee after: HEILONGJIANG DEMING TECHNOLOGY DEVELOPMENT Co.,Ltd.

Address before: 150001 No. 92 West straight street, Nangang District, Heilongjiang, Harbin

Patentee before: HARBIN INSTITUTE OF TECHNOLOGY

TR01 Transfer of patent right
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20220607

Address after: 241000 room 210, block a, robot and intelligent equipment technology business incubator, No. 69, Fuqiang Road, Jiujiang District, Wuhu City, Anhui Province

Patentee after: Wuhu Deming Thermal Insulation Technology Co.,Ltd.

Address before: Building 1, Kechuang headquarters, Shenzhen (Harbin) Industrial Park, 288 Zhigu street, Songbei District, Harbin City, Heilongjiang Province

Patentee before: HEILONGJIANG DEMING TECHNOLOGY DEVELOPMENT Co.,Ltd.

CP01 Change in the name or title of a patent holder
CP01 Change in the name or title of a patent holder

Address after: 241000 room 210, block a, robot and intelligent equipment technology business incubator, No. 69, Fuqiang Road, Jiujiang District, Wuhu City, Anhui Province

Patentee after: Wuhu Deming New Material Technology Development Co.,Ltd.

Address before: 241000 room 210, block a, robot and intelligent equipment technology business incubator, No. 69, Fuqiang Road, Jiujiang District, Wuhu City, Anhui Province

Patentee before: Wuhu Deming Thermal Insulation Technology Co.,Ltd.

PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Preparation method of surface coating for rigid ceramic insulation tiles

Granted publication date: 20161123

Pledgee: Agricultural Bank of China Co.,Ltd. Wuhu Economic and Technological Development Zone Branch

Pledgor: Wuhu Deming New Material Technology Development Co.,Ltd.

Registration number: Y2024980056115