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CN106588125A - Production method of C/C composite material gradient anti-oxidation coating - Google Patents

Production method of C/C composite material gradient anti-oxidation coating Download PDF

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CN106588125A
CN106588125A CN201611215625.5A CN201611215625A CN106588125A CN 106588125 A CN106588125 A CN 106588125A CN 201611215625 A CN201611215625 A CN 201611215625A CN 106588125 A CN106588125 A CN 106588125A
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国礼杰
尹孝辉
李申申
高银银
张向忠
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Anhui University of Technology AHUT
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/665—Local sintering, e.g. laser sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
    • C04B2235/9684—Oxidation resistance

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Abstract

本发明公开一种C/C复合材料梯度抗氧化涂层的制备方法，属于C/C复合材料抗氧化涂层制备技术。该方法首先将C/C复合材料进行表面粗化处理，然后配制所需SiC陶瓷粉和混合粉，混合粉由SiC陶瓷粉及ZrB2组成，将SiC陶瓷粉及混合粉先后分层涂覆在C/C复合材料表面得到SiC陶瓷粉涂层及混合粉涂层，烘干后备用；将烘干后的C/C复合材料采用激光熔覆进行表面熔覆，制得C/C复合材料梯度抗氧化涂层。本发明方法能够获得结合优良、抗氧化能力优异的涂层；本发明方法得到的C/C复合材料抗氧化涂层，可以扩大C/C复合材料的使用温度，满足实际应用的需要，从而扩大了C/C复合材料的应用范围。

The invention discloses a preparation method of a gradient anti-oxidation coating of a C/C composite material, which belongs to the preparation technology of an anti-oxidation coating of a C/C composite material. In this method, the surface of the C/C composite material is first roughened, and then the required SiC ceramic powder and mixed powder are prepared. The mixed powder is composed of SiC ceramic powder and ZrB 2 . The surface of the C/C composite material is coated with SiC ceramic powder and mixed powder coating, which is dried and used for later use; the surface of the dried C/C composite material is clad by laser cladding to obtain a C/C composite material gradient Antioxidant coating. The method of the present invention can obtain a coating with excellent bonding and excellent oxidation resistance; the C/C composite anti-oxidation coating obtained by the method of the present invention can expand the service temperature of the C/C composite to meet the needs of practical applications, thereby expanding The scope of application of C/C composite materials.

Description

一种C/C复合材料梯度抗氧化涂层的制备方法A kind of preparation method of gradient anti-oxidation coating of C/C composite material

技术领域：Technical field:

本发明属于C/C复合材料抗氧化涂层制备技术，具体涉及一种C/C复合材料梯度抗氧化涂层的制备方法。The invention belongs to the preparation technology of C/C composite material anti-oxidation coating, in particular to a preparation method of C/C composite material gradient anti-oxidation coating.

背景技术：Background technique:

C/C复合材料是目前极少数可在2000℃以上保持较高力学性能的材料之一，它具有低密度、高比强、高比模、低热膨胀系数、耐热冲击、耐烧蚀等一系列优异性能，尤其是这种材料的强度随温度的升高不降反升的独特性能，使其作为航空航天等高技术领域热结构件使用具有其它材料难以比拟的优势。由于C/C复合材料抗氧化性能差，极大的限制了其在氧化环境下的使用。高温抗氧化研究一直是热结构C/C复合材料研究领域的热点和难点。近年来，通过国内外研究学者的共同努力，C/C复合材料抗氧化涂层研究取得了一定进展，但仍存在许多问题。ZrB2-SiC复相陶瓷作为一种超高温陶瓷材料具有高熔点、高硬度、优良的抗热冲击和较低的氧化速率，在高温结构材料领域有重要的应用前景和价值。制备梯度ZrB2-SiC复相陶瓷涂层可以很大程度上解决C/C复合材料抗氧化涂层存在的上述问题。C/C composite material is currently one of the very few materials that can maintain high mechanical properties above 2000 °C. It has low density, high specific strength, high specific modulus, low thermal expansion coefficient, thermal shock resistance, and ablation resistance. A series of excellent properties, especially the unique property that the strength of this material does not decrease but increases with the increase of temperature, makes it have advantages that other materials cannot match when used as thermal structural parts in high-tech fields such as aerospace. Due to the poor oxidation resistance of C/C composites, its use in oxidizing environments is greatly limited. Research on high temperature oxidation resistance has always been a hot and difficult point in the research field of thermal structural C/C composites. In recent years, through the joint efforts of researchers at home and abroad, some progress has been made in the research of anti-oxidation coatings for C/C composites, but there are still many problems. As an ultra-high temperature ceramic material, ZrB 2 -SiC composite ceramic has high melting point, high hardness, excellent thermal shock resistance and low oxidation rate, and has important application prospects and value in the field of high temperature structural materials. The preparation of gradient ZrB 2 -SiC multiphase ceramic coating can largely solve the above-mentioned problems in the anti-oxidation coating of C/C composite materials.

发明内容：Invention content:

本发明目的在于提供一种C/C复合材料梯度抗氧化涂层的制备方法，本发明方法能够获得性能优异的抗氧化涂层。The purpose of the present invention is to provide a preparation method of a C/C composite material gradient anti-oxidation coating, and the method of the invention can obtain an anti-oxidation coating with excellent performance.

本发明所提供的一种C/C复合材料梯度抗氧化涂层的制备方法，该方法具体步骤如下：A kind of preparation method of gradient anti-oxidation coating of C/C composite material provided by the present invention, the concrete steps of this method are as follows:

(1)将C/C复合材料进行表面粗化处理；(1) roughening the surface of the C/C composite material;

(2)配制所需SiC陶瓷粉和混合粉，所述混合粉由SiC陶瓷粉及ZrB2组成，将所述SiC陶瓷粉及所述混合粉先后分层涂覆在所述C/C复合材料表面得到SiC陶瓷粉涂层及混合粉涂层，烘干后备用；(2) prepare required SiC ceramic powder and mixed powder, described mixed powder is made up of SiC ceramic powder and ZrB , described SiC ceramic powder and described mixed powder are successively coated on described C/C composite material The surface is coated with SiC ceramic powder coating and mixed powder coating, and it is used after drying;

(3)将烘干后的所述C/C复合材料采用激光熔覆进行表面熔覆，制得所述C/C复合材料梯度抗氧化涂层。(3) Surface cladding of the dried C/C composite material by laser cladding to obtain a gradient anti-oxidation coating of the C/C composite material.

所述SiC陶瓷粉与所述ZrB2的质量比为：1:(1-1:5)。The mass ratio of the SiC ceramic powder to the ZrB 2 is: 1:(1-1:5).

所述SiC陶瓷粉涂层及混合粉涂层的层厚均为1mm。The layer thicknesses of the SiC ceramic powder coating and the mixed powder coating are both 1mm.

所述激光熔覆的具体工艺参数为：激光功率2.4kW，光斑直径4mm，扫描速度300mm/min，搭接率30-80％。The specific process parameters of the laser cladding are: laser power 2.4kW, spot diameter 4mm, scanning speed 300mm/min, lap rate 30-80%.

采用本发明获得的涂层与C/C复合材料属于冶金结合，界面结合强度高，涂层为以SiC为中间层的梯度涂层，缓解了C/C复合材料与ZrB2抗氧化层间的内应力，涂层与基体间没有裂纹、气孔等缺陷，解决涂层与C/C复合材料基体的热膨胀匹配性问题，提高了C/C复合材料抗氧化温度。The coating obtained by the present invention and the C/C composite material belong to metallurgical bonding, and the interface bonding strength is high. The coating is a gradient coating with SiC as the intermediate layer, which alleviates the gap between the C/C composite material and the ZrB2 anti - oxidation layer. Internal stress, there are no defects such as cracks and pores between the coating and the substrate, which solves the problem of thermal expansion matching between the coating and the C/C composite substrate, and improves the oxidation resistance temperature of the C/C composite.

附图说明：Description of drawings:

图1为ZrB2-SiC抗氧化涂层扫描电镜图；Figure 1 is a scanning electron microscope image of ZrB 2 -SiC anti-oxidation coating;

图2为ZrB2-SiC抗氧化涂层表面XRD图谱。Fig. 2 is the XRD spectrum of the ZrB 2 -SiC anti-oxidation coating surface.

具体实施方式：detailed description:

实施例1：一种C/C复合材料梯度抗氧化涂层的制备方法。首先，用400#砂纸将C/C复合材料试件进行表面粗化处理。然后用电子天平分别称量所需SiC陶瓷粉和质量比SiC:ZrB2＝1:1的混合粉末；将SiC陶瓷粉粉末和SiC+ZrB2混合粉末先后分层涂覆在C/C复合材料试件表面，层厚均为1mm,烘干后备用。将烘干后C/C复合材料试件采用激光熔覆技术进行表面熔覆，激光功率2.4kW，光斑直径4mm，扫描速度300mm/min，搭接率30％。Example 1: A method for preparing a C/C composite gradient anti-oxidation coating. First, the surface of the C/C composite specimen was roughened with 400# sandpaper. Then use an electronic balance to weigh the required SiC ceramic powder and the mixed powder with a mass ratio of SiC:ZrB 2 =1:1; layer-coat the SiC ceramic powder and SiC+ZrB 2 mixed powder on the C/C composite material The thickness of the surface of the test piece is 1mm, and it is used after drying. The surface of the dried C/C composite material specimen is clad by laser cladding technology, the laser power is 2.4kW, the spot diameter is 4mm, the scanning speed is 300mm/min, and the overlap rate is 30%.

实施例2：一种C/C复合材料梯度抗氧化涂层的制备方法。首先，用400#砂纸将C/C复合材料试件进行表面粗化处理。然后用电子天平分别称量所需SiC陶瓷粉和质量比SiC:ZrB2＝1:2的混合粉末；将SiC陶瓷粉粉末和SiC+ZrB2混合粉末先后分层涂覆在C/C复合材料试件表面，层厚均为1mm,烘干后备用。将烘干后C/C复合材料试件采用激光熔覆技术进行表面熔覆，激光功率2.4kW，光斑直径4mm，扫描速度300mm/min，搭接率50％。Example 2: A method for preparing a C/C composite gradient anti-oxidation coating. First, the surface of the C/C composite specimen was roughened with 400# sandpaper. Then use an electronic balance to weigh the required SiC ceramic powder and the mixed powder with a mass ratio of SiC:ZrB 2 =1:2; layer-coat the SiC ceramic powder and SiC+ZrB 2 mixed powder on the C/C composite material The thickness of the surface of the test piece is 1mm, and it is used after drying. The surface of the dried C/C composite material specimen is clad by laser cladding technology, the laser power is 2.4kW, the spot diameter is 4mm, the scanning speed is 300mm/min, and the overlap rate is 50%.

实施例3：一种C/C复合材料梯度抗氧化涂层的制备方法。首先，用400#砂纸将C/C复合材料试件进行表面粗化处理。然后用电子天平分别称量所需SiC陶瓷粉和质量比SiC:ZrB2＝1:5的混合粉末；将SiC陶瓷粉粉末和SiC+ZrB2混合粉末先后分层涂覆在C/C复合材料试件表面，层厚均为1mm,烘干后备用。将烘干后C/C复合材料试件采用激光熔覆技术进行表面熔覆，激光功率2.4kW，光斑直径4mm，扫描速度300mm/min，搭接率60％。Example 3: A method for preparing a C/C composite gradient anti-oxidation coating. First, the surface of the C/C composite specimen was roughened with 400# sandpaper. Then use an electronic balance to weigh the required SiC ceramic powder and the mixed powder with a mass ratio of SiC:ZrB 2 =1:5; layer-coat the SiC ceramic powder and SiC+ZrB 2 mixed powder on the C/C composite material The thickness of the surface of the test piece is 1mm, and it is used after drying. The surface of the dried C/C composite material specimen is clad by laser cladding technology, the laser power is 2.4kW, the spot diameter is 4mm, the scanning speed is 300mm/min, and the overlap rate is 60%.

图1为所获得的ZrB2-SiC抗氧化涂层具有不同于烧结陶瓷的非常规结构。由图可见界面生成连续的反应相，界面成型良好，没有气孔、裂纹和残余焊接线的存在。图2为ZrB2-SiC抗氧化涂层X射线衍射谱，涂层由ZrB2和SiC两相构成。Figure 1 shows that the obtained ZrB2-SiC anti-oxidation coating has an unconventional structure different from that of sintered ceramics. It can be seen from the figure that a continuous reaction phase is generated at the interface, the interface is well formed, and there are no pores, cracks and residual welding lines. Figure 2 is the X-ray diffraction spectrum of the ZrB 2 -SiC anti-oxidation coating, and the coating is composed of two phases of ZrB 2 and SiC.

由实施例1、实施例2和实施例3，激光熔覆制备C/C复合材料ZrB2-SiC梯度抗氧化涂层的方法可以在C/C复合材料基体表面获得结合优良，抗氧化能力优异的涂层。From Example 1, Example 2 and Example 3, the method of preparing C/C composite material ZrB 2 -SiC gradient anti-oxidation coating by laser cladding can obtain excellent bonding and excellent oxidation resistance on the surface of C/C composite material matrix coating.

Claims (4)

1. a kind of preparation method of C/C composites gradient ORC, it is characterised in that the method is comprised the following steps that：
(1) C/C composites are carried out into surface coarsening process；
(2) SiC ceramic powder and mixed powder needed for preparing, the mixed powder is by SiC ceramic powder and ZrB2Composition, by the SiC ceramic Powder and the mixed powder priority layered coated obtain SiC ceramic powder coating and mixing powder coating in the C/C composite material surfaces, It is standby after drying；
(3) by drying after the C/C composites surface cladding is carried out using laser melting coating, be obtained the C/C composites Gradient ORC.
2. a kind of preparation method of C/C composites gradient ORC according to claim 1, it is characterised in that institute SiC ceramic powder is stated with the ZrB2Mass ratio be：1:(1-1:5).
3. a kind of preparation method of C/C composites gradient ORC according to claim 1, it is characterised in that institute The thickness for stating SiC ceramic powder coating and mixing powder coating is 1mm.
4. a kind of preparation method of C/C composites gradient ORC according to claim 1, it is characterised in that institute The specific process parameter for stating laser melting coating is：Laser power 2.4kW, spot diameter 4mm, scanning speed 300mm/min, overlapping rate 30-80%.
CN201611215625.5A 2016-12-26 2016-12-26 Production method of C/C composite material gradient anti-oxidation coating Pending CN106588125A (en)

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Cited By (5)

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CN108218473A (en) * 2017-12-26 2018-06-29 宜兴市天宇世纪高新科技有限公司 The preparation method of low temperature antioxidant coating in a kind of carbon material surface
CN109735789A (en) * 2019-01-25 2019-05-10 航天材料及工艺研究所 A kind of multi-component Zr/Hf-based ultra-high melting point carbide anti-oxidation coating and preparation method thereof
CN110981548A (en) * 2019-12-27 2020-04-10 西北工业大学 Laser repairing method for crack of C/C composite ultrahigh-temperature ceramic coating
CN114907145A (en) * 2022-06-10 2022-08-16 辽宁奥亿达新材料有限公司 Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof
CN116479417A (en) * 2022-05-17 2023-07-25 中国人民解放军军事科学院国防科技创新研究院 Method for preparing ceramic matrix composite coating by adopting high-speed laser cladding process

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