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CN102560411A - Preparation method of anti-ablative coating on surface of titanium alloy - Google Patents

Preparation method of anti-ablative coating on surface of titanium alloy Download PDF

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Publication number
CN102560411A
CN102560411A CN2012100063020A CN201210006302A CN102560411A CN 102560411 A CN102560411 A CN 102560411A CN 2012100063020 A CN2012100063020 A CN 2012100063020A CN 201210006302 A CN201210006302 A CN 201210006302A CN 102560411 A CN102560411 A CN 102560411A
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titanium alloy
chemical reaction
coating
flow rate
preparation
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魏建忠
马捷
李辉
张永志
范爱玲
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Beijing University of Technology
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Beijing University of Technology
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Abstract

一种钛合金表面抗烧蚀涂层的制备方法,本发明属于材料腐蚀与防护领域。利用化学反应WF6+3H2→W+6HF,在钛合金表面得到难熔金属钨涂层。钛合金表面抗烧蚀涂层的制备方法,其特征在于:化学反应温度420~480℃,H2流量为3.2~3.8L/min,WF6流量为5.2~5.8g/min,升温速度为8~12℃/min,降温速度为10~15℃/min,化学反应时间为25~35min。通过对化学反应温度、气体流量以及升温和降温速度等参数的控制,可得到抗烧蚀性能良好的钨涂层,该涂层在1000℃的恒温炉中检验,效果明显。

Figure 201210006302

A method for preparing an anti-ablation coating on the surface of a titanium alloy belongs to the field of material corrosion and protection. Using the chemical reaction WF 6 +3H 2 →W+6HF, the refractory metal tungsten coating is obtained on the surface of the titanium alloy. The preparation method of the anti-ablation coating on the surface of titanium alloy is characterized in that: the chemical reaction temperature is 420-480°C, the flow rate of H2 is 3.2-3.8L/min, the flow rate of WF6 is 5.2-5.8g/min, and the heating rate is 8 ~12℃/min, the cooling rate is 10~15℃/min, and the chemical reaction time is 25~35min. By controlling the chemical reaction temperature, gas flow rate, heating and cooling speed and other parameters, a tungsten coating with good ablation resistance can be obtained. The coating is tested in a constant temperature furnace at 1000 ° C, and the effect is obvious.

Figure 201210006302

Description

一种钛合金表面抗烧蚀涂层的制备方法A kind of preparation method of anti-ablation coating on titanium alloy surface

技术领域 technical field

本发明属于金属材料腐蚀与防护领域,特别为钛合金提供了一种抗烧蚀的难熔金属钨防护涂层的制备方法。The invention belongs to the field of metal material corrosion and protection, and in particular provides a preparation method of an ablation-resistant refractory metal tungsten protective coating for titanium alloys.

背景技术 Background technique

钛是上世纪五十年代发展起来的一种结构金属,钛合金具有比强度高、韧性和抗蚀性好等特点而被广泛应用于航空航天、军工、建筑、汽车等工业中。然而,高温下抗氧化和耐蚀性很不理想,易烧蚀。表面处理可有效提高钛合金的性能。传统的表面改性处理如渗碳、渗硼和渗氮,存在着处理周期长、工件易变性等缺点;热喷涂技术制备的涂层存在着组织结构疏松、与基体结合较弱等不足;激光束、电子束表面改性因设备复杂、成本高而较少使用。难熔金属钨具有很高的熔点(3410℃),耐磨耐腐蚀性极强,高温下化学性质稳定。本专利利用气体的化学反应,在钛合金基体表面得到难熔金属钨涂层,该涂层在高温下具有很强的抗烧蚀性能。Titanium is a structural metal developed in the 1950s. Titanium alloys have the characteristics of high specific strength, toughness and corrosion resistance, and are widely used in aerospace, military, construction, automobile and other industries. However, the oxidation resistance and corrosion resistance at high temperature are not ideal, and it is easy to ablate. Surface treatment can effectively improve the performance of titanium alloys. Traditional surface modification treatments such as carburizing, boronizing and nitriding have disadvantages such as long treatment cycle and workpiece variability; coatings prepared by thermal spraying technology have shortcomings such as loose structure and weak bonding with the substrate; laser Beam and electron beam surface modification are rarely used due to complex equipment and high cost. The refractory metal tungsten has a very high melting point (3410°C), has strong wear resistance and corrosion resistance, and has stable chemical properties at high temperatures. This patent uses the chemical reaction of the gas to obtain a refractory metal tungsten coating on the surface of the titanium alloy substrate. The coating has strong anti-ablation performance at high temperatures.

发明内容 Contents of the invention

本发明选用气体间的化学反应,在钛合金基体上生成8~12微米厚的难熔金属钨涂层。化学反应方程式为:WF6+3H2→W+6HF。The invention adopts the chemical reaction between gases to form a refractory metal tungsten coating with a thickness of 8-12 microns on the titanium alloy substrate. The chemical reaction equation is: WF 6 +3H 2 →W+6HF.

所用设备有:温度控制柜(要求控温精度高);加热炉(内设置工件摆放装置,且有畅通的气体流通管道);尾气吸收装置(采用氢氧化钠水溶液对尾气进行喷淋吸收,可达到环保要求)。The equipment used includes: temperature control cabinet (requires high temperature control accuracy); heating furnace (with a workpiece placement device inside and a smooth gas circulation pipe); tail gas absorption device (using sodium hydroxide aqueous solution to spray and absorb the tail gas, meet environmental protection requirements).

工艺流程:Process flow:

(1)工件表面预处理。(1) Pretreatment of workpiece surface.

使用碱水洗去工件表面污物,并用水冲洗干净,之后分别用丙酮和酒精进行超声波清洗,得到洁净表面。Use alkaline water to wash away the dirt on the surface of the workpiece, rinse it with water, and then use acetone and alcohol to perform ultrasonic cleaning respectively to obtain a clean surface.

(2)工件入炉。(2) The workpiece is put into the furnace.

(3)通高纯Ar排净装置内空气,并检查装置的气密性。(3) Exhaust the air in the device through high-purity Ar, and check the airtightness of the device.

(4)停止通Ar,开始通H2,加热。(4) Stop flowing Ar, start flowing H 2 , and heat.

(5)化学反应。(5) Chemical reaction.

到达设定温度后,通WF6,进行气体化学反应,同时打开尾气吸收装置,吸收反应副产物HF。根据不同要求,可在钛合金表面得到不同厚度的涂层。After reaching the set temperature, pass WF 6 to carry out the gas chemical reaction, and at the same time open the tail gas absorption device to absorb the reaction by-product HF. According to different requirements, different thickness coatings can be obtained on the surface of titanium alloy.

化学反应温度420~480℃,H2流量为3.2~3.8L/min,WF6流量为5.2~5.8g/min,升温速度为8~12℃/min,降温速度为10~15℃/min,化学反应时间为25~35min。The chemical reaction temperature is 420-480°C, the flow rate of H 2 is 3.2-3.8L/min, the flow rate of WF 6 is 5.2-5.8g/min, the heating rate is 8-12°C/min, and the cooling rate is 10-15°C/min. The chemical reaction time is 25-35 minutes.

(6)降温。(6) cooling.

反应结束,关闭WF6气体,继续通H2直到室温。出炉,检测。After the reaction is over, turn off the WF 6 gas, and continue to pass H 2 until room temperature. Baked, tested.

本专利技术的主要特点Main features of this patented technology

(1)本专利操作简单,整个过程自动控制,易实现工业批量生产;(1) The operation of this patent is simple, the whole process is automatically controlled, and it is easy to realize industrial mass production;

(2)本专利采用常压下的化学反应,设备简单,投入少,见效快。(2) This patent adopts the chemical reaction under normal pressure, and equipment is simple, and input is few, and quick effect is obtained.

(3)本专利适应各种形状、尺寸的钛合金,应用性广;(3) This patent is suitable for titanium alloys of various shapes and sizes, and has wide applicability;

(4)本专利所得涂层的成分为100%存钨,对钛合金的高温防护作用效果明显。(4) The composition of the coating obtained in this patent is 100% tungsten, which has an obvious high-temperature protection effect on titanium alloys.

附图说明: Description of drawings:

图1:带有钨涂层的钛合金金相显微照片。Figure 1: Metallographic micrograph of titanium alloy with tungsten coating.

具体实施方式: Detailed ways:

将钛合金基体进行表面预处理后,进行化学反应的工艺参数及效果如下:After the surface pretreatment of the titanium alloy substrate, the process parameters and effects of the chemical reaction are as follows:

Figure BDA0000129878730000021
Figure BDA0000129878730000021

Figure BDA0000129878730000031
Figure BDA0000129878730000031

通过设置合适的化学反应参数,在钛合金基体上形成8~10微米的难熔金属致密钨涂层,能够对钛合金起到很好的防护作用,抗烧蚀温度提高了400℃以上。工艺参数设定为:化学反应温度420~480℃,H2流量为3.2~3.8L/min,WF6流量为5.2~5.8g/min,升温速度为8~12℃/min,降温速度为10~15℃/min,反应时间25~35min。By setting appropriate chemical reaction parameters, a refractory metal dense tungsten coating of 8 to 10 microns is formed on the titanium alloy substrate, which can protect the titanium alloy very well, and the ablation resistance temperature is increased by more than 400°C. The process parameters are set as follows: chemical reaction temperature 420-480°C, H 2 flow rate 3.2-3.8L/min, WF 6 flow rate 5.2-5.8g/min, heating rate 8-12°C/min, cooling rate 10 ~15°C/min, reaction time 25~35min.

Claims (1)

1. the preparation method of the anti-ablative coating of titanium alloy surface is characterized in that: 420~480 ℃ of chemical reaction temperature, H 2Flow is 3.2~3.8L/min, WF 6Flow is 5.2~5.8g/min, and heat-up rate is 8~12 ℃/min, and cooling rate is 10~15 ℃/min, and chemical time is 25~35min.
CN2012100063020A 2012-01-10 2012-01-10 Preparation method of anti-ablative coating on surface of titanium alloy Pending CN102560411A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103352222A (en) * 2013-06-24 2013-10-16 核工业西南物理研究院 Preparation method of carbon-based tungsten coating for tokamak device
CN109825814A (en) * 2019-04-10 2019-05-31 北京工业大学 A method of strong adhesive force tungsten layer is prepared in titanium alloy surface

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1305023A (en) * 2000-10-19 2001-07-25 太原理工大学 Plasma surface-alloying process for titanium alloy
CN1342215A (en) * 1999-02-11 2002-03-27 哈迪德有限公司 Tungsten carbide coatings and method for producing the same
CN1962935A (en) * 2006-12-08 2007-05-16 北京工业大学 Process for preparing high-purity compact profile tungsten products

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1342215A (en) * 1999-02-11 2002-03-27 哈迪德有限公司 Tungsten carbide coatings and method for producing the same
CN1305023A (en) * 2000-10-19 2001-07-25 太原理工大学 Plasma surface-alloying process for titanium alloy
CN1962935A (en) * 2006-12-08 2007-05-16 北京工业大学 Process for preparing high-purity compact profile tungsten products

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103352222A (en) * 2013-06-24 2013-10-16 核工业西南物理研究院 Preparation method of carbon-based tungsten coating for tokamak device
CN103352222B (en) * 2013-06-24 2016-03-02 核工业西南物理研究院 A kind of preparation method of the carbon-base tungsten coating for tokamak device
CN109825814A (en) * 2019-04-10 2019-05-31 北京工业大学 A method of strong adhesive force tungsten layer is prepared in titanium alloy surface

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