CN104630693A - Combined treatment method of surface of austenitic stainless steel - Google Patents
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Abstract
Description
技术领域 technical field
本发明涉及一种奥氏体不锈钢表面的复合处理方法,属于金属材料表面改性技术领域。 The invention relates to a composite treatment method for the surface of austenitic stainless steel, which belongs to the technical field of surface modification of metal materials.
背景技术 Background technique
奥氏体不锈钢因具有良好的综合力学性能和工艺性能,且在氧化性和还原性介质中均表现出较好的耐蚀性,从而在工业、民用、国防等领域中得到了广泛的应用。目前,奥氏体不锈钢亦是不锈钢中种类最多、使用量最大的一种钢材,其生产量和使用量约占不锈钢总产量及使用量的一半以上。但是,受表面硬度低、摩擦系数大、耐磨性差等缺点的制约,奥氏体不锈钢一般不能用于制作滑动摩擦配副零部件,其更广泛地使用受到限制。基于摩擦磨损始发生于材料表面,已有研究表明,借助表面技术可有效提高奥氏体不锈钢的耐磨性。选用合适的表面处理技术对于拓展奥氏体不锈钢作为摩擦材料的应用具有显著意义。 Austenitic stainless steel has been widely used in industry, civil, national defense and other fields due to its good comprehensive mechanical properties and process properties, and good corrosion resistance in both oxidizing and reducing media. At present, austenitic stainless steel is also a kind of steel with the largest variety and the largest amount of use among stainless steels, and its production and use account for more than half of the total output and use of stainless steel. However, due to the disadvantages of low surface hardness, high friction coefficient, and poor wear resistance, austenitic stainless steel cannot generally be used to make sliding friction parts, and its wider use is limited. Based on the fact that friction and wear begin on the surface of the material, studies have shown that the wear resistance of austenitic stainless steel can be effectively improved by means of surface technology. The selection of appropriate surface treatment technology is of great significance for expanding the application of austenitic stainless steel as friction material.
发明内容 Contents of the invention
本发明旨在提供一种奥氏体不锈钢表面的复合处理方法,所得的奥氏体不锈钢具有优异的脂润滑摩擦学性能。 The invention aims to provide a composite treatment method for the surface of austenitic stainless steel, and the obtained austenitic stainless steel has excellent grease lubrication tribological properties.
本发明提供的一种奥氏体不锈钢表面的复合处理方法,首先对奥氏体不锈钢进行电化学处理,然后采用离子氮化技术制备氮化改性层。 The present invention provides a composite treatment method for the surface of austenitic stainless steel. Firstly, the austenitic stainless steel is electrochemically treated, and then the nitriding modified layer is prepared by ion nitriding technology.
上述处理方法,包括以下步骤: The above processing method includes the following steps:
(1)对奥氏体不锈钢工件预处理:将奥氏体不锈钢工件表面除油后使用SiC水砂纸进行逐级打磨、清洗、干燥备用; (1) Pretreatment of austenitic stainless steel workpieces: after degreasing the surface of austenitic stainless steel workpieces, use SiC water sandpaper to perform step-by-step grinding, cleaning, and drying for later use;
(2)将预处理好的奥氏体不锈钢工件留出工作面,其余部分使用环氧树脂密封、干燥后、将其作为工作电极、用饱和甘汞电极作为参比电极、铂片作为辅助电极置于浓度为10~25 wt. %的NaCl溶液中,在20~30 ℃下分别进行开路电位和动电位极化曲线测试,开路电位测试时间为10~20 min,极化曲线测试取相对于开路电位-0.25 V为起始电压、+2.0 V为终止电压,扫描速率为1mV/s; (2) Leave the pretreated austenitic stainless steel workpiece on the working surface, seal the rest with epoxy resin, dry it, use it as the working electrode, use the saturated calomel electrode as the reference electrode, and the platinum sheet as the auxiliary electrode Placed in a NaCl solution with a concentration of 10-25 wt. %, the open-circuit potential and potentiodynamic polarization curve tests were carried out at 20-30 °C, the open-circuit potential test time was 10-20 min, and the polarization curve test was taken relative to Open circuit potential -0.25 V is the initial voltage, +2.0 V is the final voltage, and the scan rate is 1mV/s;
(3)将步骤(2)处理好的奥氏体不锈钢放入辉光离子渗金属炉内的工件台上,并通过工件台与脉冲电源的阴极连接,成为工件极,炉壳与脉冲电源的阳极连接,并接地; (3) Put the austenitic stainless steel processed in step (2) on the workpiece table in the glow ion metallization furnace, and connect the cathode of the pulse power supply through the workpiece table to become the workpiece pole, the furnace shell and the pulse power supply. Anode connection, and ground;
(4)把辉光离子渗金属炉炉腔内部抽成真空度为0.1 Pa,通入流量为30 sccm~35 sccm的氨气到炉腔,使炉腔内气压维持在35 Pa~45 Pa,启动脉冲电源,在阳极与阴极间施加直流偏压,当工件极温度升至350 ℃~450 ℃时,对奥氏体不锈钢进行离子轰击清洗20 min~40 min; (4) Evacuate the interior of the glow ion metal infiltration furnace cavity to a vacuum of 0.1 Pa, and feed ammonia gas with a flow rate of 30 sccm to 35 sccm into the furnace cavity to maintain the pressure in the furnace cavity at 35 Pa to 45 Pa. Start the pulse power supply, apply a DC bias voltage between the anode and the cathode, and when the temperature of the workpiece rises to 350 ℃ ~ 450 ℃, perform ion bombardment cleaning on the austenitic stainless steel for 20 minutes to 40 minutes;
(5)将工件极电压调至–600 V~–500 V,工件极电流调至30 A~40 A,工件极温度维持在500 ℃~550 ℃,保温8 h~10 h,关闭脉冲电源,使奥氏体不锈钢缓冷到室温。 (5) Adjust the workpiece pole voltage to -600 V ~ -500 V, the workpiece pole current to 30 A ~ 40 A, maintain the workpiece pole temperature at 500 ℃ ~ 550 ℃, keep warm for 8 h ~ 10 h, turn off the pulse power supply, Allow the austenitic stainless steel to cool slowly to room temperature.
上述方案中,所述步骤(2)中NaCl溶液的质量浓度优选为15~20%。 In the above scheme, the mass concentration of the NaCl solution in the step (2) is preferably 15-20%.
上述方案中,所述步骤(5)中,工件极电压优选为–550 V,工件极电流优选为35A,工件极温度优选525 ℃~535 ℃。 In the above scheme, in the step (5), the workpiece pole voltage is preferably -550 V, the workpiece pole current is preferably 35A, and the workpiece pole temperature is preferably 525°C to 535°C.
本发明属于金属材料表面改性技术领域,利用奥氏体不锈钢对Cl-点蚀敏感性高的特点,先对316不锈钢进行电化学处理获得表面织构,再采用离子氮化技术制备氮化改性层。 The invention belongs to the technical field of surface modification of metal materials. Utilizing the characteristics of austenitic stainless steel with high sensitivity to Cl - pitting corrosion, first electrochemically treat 316 stainless steel to obtain surface texture, and then use ion nitriding technology to prepare nitriding modified sex layer.
本发明的有益效果: Beneficial effects of the present invention:
本发明将电化学处理与离子氮化技术相结合,对奥氏体不锈钢进行复合处理,充分发挥了表面织构化和离子氮化的优势,提高了奥氏体不锈钢的摩擦学性能,降低了摩擦系数,减少了磨损失重。 The present invention combines electrochemical treatment with ion nitriding technology, and performs composite treatment on austenitic stainless steel, fully exerts the advantages of surface texture and ion nitriding, improves the tribological performance of austenitic stainless steel, reduces the Coefficient of friction, reducing wear and weight loss.
附图说明 Description of drawings
图1为未处理奥氏体不锈钢和实施例1处理后的奥氏体不锈钢与GCr15对磨的摩擦系数图; Fig. 1 is the friction coefficient figure of untreated austenitic stainless steel and the austenitic stainless steel and GCr15 after the treatment of embodiment 1;
图2为未处理奥氏体不锈钢和实施例1处理后的奥氏体不锈钢与Si3N4对磨的摩擦系数图; Fig. 2 is the coefficient of friction figure of untreated austenitic stainless steel and austenitic stainless steel treated in embodiment 1 and Si 3 N 4 against grinding;
图3为未处理奥氏体不锈钢和实施例1处理后的奥氏体不锈钢与GCr15对磨的磨损失重图; Fig. 3 is untreated austenitic stainless steel and the austenitic stainless steel and GCr15 after the treatment of embodiment 1 wear loss weight diagram;
图4为未处理奥氏体不锈钢和实施例1处理后的奥氏体不锈钢与Si3N4对磨的磨损失重图; Fig. 4 is untreated austenitic stainless steel and embodiment 1 treated austenitic stainless steel and Si 3 N 4 wear loss weight diagram for grinding;
图5为未处理奥氏体不锈钢和实施例2处理后的奥氏体不锈钢与GCr15对磨的摩擦系数图; Fig. 5 is the coefficient of friction figure of untreated austenitic stainless steel and the austenitic stainless steel and GCr15 after the treatment of embodiment 2;
图6为未处理奥氏体不锈钢和实施例2处理后的奥氏体不锈钢与Si3N4对磨的摩擦系数图; Fig. 6 is the coefficient of friction figure of untreated austenitic stainless steel and austenitic stainless steel treated in embodiment 2 and Si 3 N 4 against grinding;
图7为未处理奥氏体不锈钢和实施例2处理后的奥氏体不锈钢与GCr15对磨的磨损失重图; Fig. 7 is untreated austenitic stainless steel and embodiment 2 processed austenitic stainless steel and GCr15 to the wear loss figure of grinding;
图8为未处理奥氏体不锈钢和实施例2处理后的奥氏体不锈钢与Si3N4对磨的磨损失重图; Fig. 8 is untreated austenitic stainless steel and the austenitic stainless steel after the treatment of embodiment 2 and Si 3 N 4 wear loss weight diagram of grinding;
图1中1—未处理奥氏体不锈钢与GCr15对磨的的摩擦系数图;2—实施例1处理后的奥氏体不锈钢与GCr15对磨的摩擦系数图; Among Fig. 1 1—the friction coefficient figure of untreated austenitic stainless steel and GCr15 grinding; 2—the friction coefficient figure of the austenitic stainless steel and GCr15 grinding of the processed austenitic stainless steel after embodiment 1;
图2中3—未处理奥氏体不锈钢与Si3N4对磨的摩擦系数图;4—实施例1处理后的奥氏体不锈钢与Si3N4对磨的摩擦系数图; Among Fig. 2, 3—the friction coefficient diagram of untreated austenitic stainless steel and Si 3 N 4 grinding; 4—the friction coefficient diagram of austenitic stainless steel and Si 3 N 4 grinding after the treatment of embodiment 1;
图3中5—未处理奥氏体不锈钢与GCr15对磨的磨损失重图;6—实施例1处理后的奥氏体不锈钢与GCr15对磨的磨损失重图; Among Fig. 3, 5—untreated austenitic stainless steel and GCr15 wear loss weight map; 6—austenitic stainless steel and GCr15 wear loss weight map after the treatment of embodiment 1;
图4中7—未处理奥氏体不锈钢与Si3N4对磨的磨损失重图;8—实施例1处理后的奥氏体不锈钢与Si3N4对磨的磨损失重图; Among Fig. 4, 7—untreated austenitic stainless steel and Si 3 N 4 pair grinding wear loss diagram; 8—austenitic stainless steel after embodiment 1 treatment and Si 3 N 4 Wear loss weight diagram of pair grinding;
图5中9—未处理奥氏体不锈钢与GCr15对磨的的摩擦系数图;10—实施例2处理后的奥氏体不锈钢与GCr15对磨的摩擦系数图; Among Fig. 5, 9—the friction coefficient figure of untreated austenitic stainless steel and GCr15 grinding; 10—the friction coefficient figure of the austenitic stainless steel and GCr15 grinding of the processed austenitic stainless steel after embodiment 2;
图6中11—未处理奥氏体不锈钢与Si3N4对磨的摩擦系数图;12—实施例2处理后的奥氏体不锈钢与Si3N4对磨的摩擦系数图; Among Fig. 6, 11—the friction coefficient diagram of untreated austenitic stainless steel and Si 3 N 4 grinding; 12—the friction coefficient diagram of austenitic stainless steel and Si 3 N 4 grinding after the treatment of Example 2;
图7中13—未处理奥氏体不锈钢与GCr15对磨的磨损失重图;14—实施例2处理后的奥氏体不锈钢与GCr15对磨的磨损失重图; Among Fig. 7, 13—untreated austenitic stainless steel and GCr15 wear loss weight map; 14—embodiment 2 treated austenitic stainless steel and GCr15 wear loss weight map;
图8中15—未处理奥氏体不锈钢与Si3N4对磨的磨损失重图;16—实施例2处理后的奥氏体不锈钢与Si3N4对磨的磨损失重图; Among Fig. 8, 15—untreated austenitic stainless steel and Si 3 N 4 pair grinding wear loss weight map; 16—austenitic stainless steel and Si 3 N 4 pair grinding wear loss weight map after processing in Example 2;
图1、图2、图5、图6中μ—摩擦系数;T—摩擦时间;图3、图4、图7、图8中G—磨损失重。 In Fig. 1, Fig. 2, Fig. 5, and Fig. 6, μ—friction coefficient; T—friction time; in Fig. 3, Fig. 4, Fig. 7, and Fig. 8, G—wear weight loss.
具体实施方式 Detailed ways
下面通过附图和实施例来进一步说明本发明,但不局限于以下实施例。 The present invention is further illustrated below by means of the accompanying drawings and examples, but is not limited to the following examples.
现以316奥氏体不锈钢为例,对本发明进行实施: Now taking 316 austenitic stainless steel as an example, the present invention is implemented:
实施例1: Example 1:
本实施例中复合表面处理方法,具体包括以下步骤: Composite surface treatment method in the present embodiment specifically comprises the following steps:
(1)对奥氏体不锈钢工件预处理:将奥氏体不锈钢工件表面除油后使用SiC水砂纸进行逐级打磨、清洗、干燥备用; (1) Pretreatment of austenitic stainless steel workpieces: after degreasing the surface of austenitic stainless steel workpieces, use SiC water sandpaper to perform step-by-step grinding, cleaning, and drying for later use;
(2)将预处理好的奥氏体不锈钢工件留出工作面,其余部分使用环氧树脂密封、干燥后、将其作为工作电极、用饱和甘汞电极作为参比电极、铂片作为辅助电极置于浓度为15 wt. %的NaCl溶液中,在25 ℃下分别进行开路电位和动电位极化曲线测试,开路电位测试时间为15 min,极化曲线测试取相对于开路电位-0.25 V为起始电压、+2.0 V为终止电压,扫描速率为1mV/s; (2) Leave the pretreated austenitic stainless steel workpiece on the working surface, seal the rest with epoxy resin, dry it, use it as the working electrode, use the saturated calomel electrode as the reference electrode, and the platinum sheet as the auxiliary electrode Placed in a NaCl solution with a concentration of 15 wt.%, the open circuit potential and potentiodynamic polarization curve tests were carried out at 25 °C. The open circuit potential test time was 15 min, and the polarization curve test was taken relative to the open circuit potential -0.25 V as The initial voltage, +2.0 V is the end voltage, and the scan rate is 1mV/s;
(3)将步骤(2)处理好的奥氏体不锈钢放入辉光离子渗金属炉内的工件台上,并通过工件台与脉冲电源的阴极连接,成为工件极,炉壳与脉冲电源的阳极连接,并接地; (3) Put the austenitic stainless steel processed in step (2) on the workpiece table in the glow ion metallization furnace, and connect the cathode of the pulse power supply through the workpiece table to become the workpiece pole, the furnace shell and the pulse power supply. Anode connection, and ground;
(4)把辉光离子渗金属炉炉腔1内部抽成真空度为1×10–1 Pa,通入流量为30 sccm~35 sccm的氨气到炉腔,使炉腔内气压维持在40 Pa,启动脉冲电源,在阳极与阴极间施加直流偏压,当工件极温度升至350 ℃~450 ℃时,对奥氏体不锈钢进行离子轰击清洗30 min; (4) Evacuate the chamber 1 of the glow ion metal infiltration furnace to a vacuum degree of 1× 10-1 Pa, and feed ammonia gas with a flow rate of 30 sccm to 35 sccm into the furnace chamber to maintain the pressure in the furnace chamber at 40 Pa, start the pulse power supply, apply a DC bias voltage between the anode and the cathode, and when the temperature of the workpiece rises to 350 ℃ ~ 450 ℃, perform ion bombardment cleaning on the austenitic stainless steel for 30 minutes;
(5)将工件极电压调至–550 V,工件极电流调至35 A,工件极温度维持在525 ℃,保温9 h,关闭脉冲电源,使奥氏体不锈钢缓冷到室温。 (5) Adjust the workpiece pole voltage to –550 V, the workpiece pole current to 35 A, maintain the workpiece pole temperature at 525 °C, keep warm for 9 h, turn off the pulse power supply, and slowly cool the austenitic stainless steel to room temperature.
实施例2: Example 2:
本实施方式与实施例1不同的是步骤(2)中NaCl溶液的浓度为20 wt. %,步骤(5)中工件极温度维持在535 ℃,其它步骤及参数与实施例1相同。 The difference between this embodiment and Example 1 is that the concentration of the NaCl solution in step (2) is 20 wt.%, the temperature of the workpiece pole in step (5) is maintained at 535 ° C, and other steps and parameters are the same as in Example 1.
将实施例1和实施例2得到的处理后的奥氏体不锈钢进行摩擦学性能测试。 The treated austenitic stainless steel obtained in Example 1 and Example 2 was subjected to a tribological performance test.
在进行摩擦磨损测试时,所有试样表面均涂覆一层润滑脂。本发明为了发挥表面织构化和离子氮化的优势:表面织构可以贮存润滑脂,氮化处理可提高表面耐磨性,二者具有“相辅相成”的效果;所以在进行摩擦磨损测试时,所有试样表面均涂覆一层润滑脂。 During the friction and wear test, the surfaces of all samples were coated with a layer of grease. In order to give full play to the advantages of surface texturing and ion nitriding, the present invention: the surface texture can store grease, and the nitriding treatment can improve the surface wear resistance, and the two have the effect of "complementing each other"; so when performing friction and wear tests, All specimen surfaces were coated with a layer of grease.
在上述工艺条件下,处理奥氏体不锈钢获得摩擦学性能优异的,测试数据见表1。 Under the above process conditions, the austenitic stainless steel has excellent tribological properties. The test data are shown in Table 1.
表1 Table 1
由表1所提供的测试结果可见:与未处理不锈钢相比,316不锈钢经过复合表面处理后,磨损实验结果表明,奥氏体不锈钢经复合处理后,摩擦系数和磨损失重量均显著低于未处理不锈钢。由上述结果可知,复合表面处理后奥氏体不锈钢获得了优异的摩擦学性能。 From the test results provided in Table 1, it can be seen that compared with untreated stainless steel, after 316 stainless steel has undergone composite surface treatment, the wear test results show that the friction coefficient and wear loss weight of austenitic stainless steel after composite treatment are significantly lower than those of untreated stainless steel. Handle stainless steel. From the above results, it can be seen that the austenitic stainless steel obtained excellent tribological properties after composite surface treatment.
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CN105755427B (en) * | 2016-04-20 | 2018-06-26 | 深圳市八六三新材料技术有限责任公司 | A kind of austenitic stainless steel and its compound plasma intensifying method |
CN105908182A (en) * | 2016-06-01 | 2016-08-31 | 太原理工大学 | Preparation method of austenite stainless steel surface nickel-titanium alloy coating |
CN106011852A (en) * | 2016-06-01 | 2016-10-12 | 太原理工大学 | Preparation method of high-entropy alloy coating on surface of austenitic stainless steel |
CN105908182B (en) * | 2016-06-01 | 2019-02-22 | 太原理工大学 | A kind of preparation method of nickel-titanium alloy coating on the surface of austenitic stainless steel |
CN106011852B (en) * | 2016-06-01 | 2019-03-01 | 太原理工大学 | A kind of preparation method of austenite stainless steel surface high entropy alloy coating |
CN106884136A (en) * | 2017-01-17 | 2017-06-23 | 清华大学 | A kind of metal material surface nitriding deposits the wear-resisting modified layer preparation method of duplex anti-friction |
CN106884136B (en) * | 2017-01-17 | 2019-08-16 | 清华大学 | A kind of metal material surface nitriding deposition wear-resisting modified layer preparation method of duplex anti-friction |
CN107761044A (en) * | 2017-11-22 | 2018-03-06 | 烟台大学 | A kind of corrosion resistant surface modifying method of austenitic stainless steel marine environment and use equipment |
CN110117766A (en) * | 2018-02-05 | 2019-08-13 | 尤尼罗库株式会社 | The manufacturing method of sealing component and metal block based on this |
CN110117766B (en) * | 2018-02-05 | 2021-07-02 | 尤尼罗库株式会社 | Method for manufacturing sealing component and metal block based on same |
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