CN105177493B - A kind of surface of hot working die arc-plasma auxiliary low pressure nitriding method - Google Patents
A kind of surface of hot working die arc-plasma auxiliary low pressure nitriding method Download PDFInfo
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Abstract
本发明公开了一种热作模具表面电弧等离子体辅助低压渗氮方法。首先利用电弧增强辉光放电产生的Ar+对热作模具表面进行离子刻蚀,去除材料表面的氧化物。而后炉内连续通入一定流量高纯N2、高纯H2、以及高纯Ar,保持炉内温度(300‑600℃)和气压(0.2‑1.0 Pa)恒定,工件转平台接脉冲电源负极,进行等离子渗氮。2h渗氮渗层深度在15‑40μm,渗氮层中化合物层厚度0‑3μm,硬度1000‑1300 HV0.1,脆性等级小于1级,疏松级别小于1级。此外,通过氩离子有效、实时地轰击活化工件表面,以达到增加氮原子扩散通道,加速渗氮过程,最终得到高强度高韧性的渗氮表层。The invention discloses a low-pressure nitriding method assisted by electric arc plasma on the surface of a hot work mold. Firstly, Ar + generated by arc-enhanced glow discharge is used to perform ion etching on the surface of the hot-working mold to remove oxides on the surface of the material. Then a certain flow of high-purity N 2 , high-purity H 2 , and high-purity Ar is continuously fed into the furnace to keep the temperature (300-600°C) and air pressure (0.2-1.0 Pa) constant in the furnace, and the workpiece transfer platform is connected to the negative pole of the pulse power supply , for plasma nitriding. The depth of the 2h nitriding layer is 15-40μm, the thickness of the compound layer in the nitriding layer is 0-3μm, the hardness is 1000-1300 HV 0.1 , the brittleness level is less than 1 level, and the porosity level is less than 1 level. In addition, the surface of the workpiece is effectively and real-time bombarded by argon ions to increase the diffusion channels of nitrogen atoms, accelerate the nitriding process, and finally obtain a high-strength and high-toughness nitriding surface layer.
Description
技术领域technical field
本发明属于材料表面改性领域,具体涉及一种热作模具表面电弧等离子体辅助低压渗氮方法,适用于硬质合金刀具、模具、金属零部件的表面强化。The invention belongs to the field of material surface modification, and in particular relates to a low-pressure nitriding method assisted by electric arc plasma on the surface of a hot work mold, which is suitable for surface strengthening of hard alloy cutters, molds and metal parts.
背景技术Background technique
等离子渗氮是一种重要的化学热处理技术,具有处理温度低、速度快、无污染、工艺可控性好等优点,可显著提高金属材料的表面硬度和耐磨性能。渗氮方法通常分为气体渗氮、液体渗氮、固体渗氮和离子渗氮等。其中离子渗氮因其效率高、污染小、易控制、工件变形小等优点得到了广泛应用。Plasma nitriding is an important chemical heat treatment technology, which has the advantages of low treatment temperature, fast speed, no pollution, good process controllability, etc., and can significantly improve the surface hardness and wear resistance of metal materials. Nitriding methods are usually divided into gas nitriding, liquid nitriding, solid nitriding and ion nitriding. Among them, ion nitriding has been widely used because of its high efficiency, low pollution, easy control, and small deformation of workpieces.
目前,常用的离子渗氮技术有直流离子渗氮、脉冲直流离子渗氮、活性屏离子渗氮、空心阴极等离子渗氮、离子注入渗氮等等。At present, the commonly used ion nitriding technologies include direct current ion nitriding, pulse direct current ion nitriding, active screen ion nitriding, hollow cathode plasma nitriding, ion implantation nitriding and so on.
在直流离子渗氮过程中,工件置于真空容器中并和直流高压电的负极相连,阳极则接在真空室外壳上,工件就在直流辉光放电产生的低温等离子体中进行渗氮处理。工件作为放电系统的阴极,离子渗氮处理过程中不可避免地存在一些难以解决的问题,如 M.OIzon-Dionysio 研究了直流离子渗氮的“边角效应”,指出造成工件边角部位的表面形貌及组织结构与其他部位有所差异,导致表面硬度的不均匀。此外,还存在表面打弧、空心阴极效应等缺点。In the DC ion nitriding process, the workpiece is placed in a vacuum container and connected to the negative electrode of the DC high voltage, and the anode is connected to the outer shell of the vacuum chamber, and the workpiece is nitrided in the low-temperature plasma generated by the DC glow discharge. . The workpiece is used as the cathode of the discharge system, and there are inevitably some difficult problems in the ion nitriding process. For example, M.OIzon-Dionysio studied the "corner effect" of DC ion nitriding and pointed out that the surface of the corners of the workpiece caused The morphology and organizational structure are different from other parts, resulting in uneven surface hardness. In addition, there are disadvantages such as surface arcing and hollow cathode effect.
为了快速息弧和提高渗氮工件的质量,脉冲电源的开发和应用是近30年来离子化学热处理技术发展的最大亮点。采用脉冲电源进行离子化学热处理具有灭弧容易、空心阴极效应小、无功损耗低、便于工艺参数独立控制等特点,特别是对一些形状特殊的零件,或是需经特别工艺处理,脉冲电源的优势更为明显。在低压等离子弧源中进行离子渗氮处理,可使温度降低100℃以上。In order to quickly quench the arc and improve the quality of nitriding workpieces, the development and application of pulse power supply is the biggest highlight in the development of ion chemical heat treatment technology in the past 30 years. The use of pulse power supply for ion chemical heat treatment has the characteristics of easy arc extinguishing, small hollow cathode effect, low reactive power loss, and easy independent control of process parameters, especially for some parts with special shapes, or need special process treatment, pulse power supply The advantages are more obvious. Ion nitriding treatment in a low-pressure plasma arc source can reduce the temperature by more than 100°C.
卢森堡工程师 Georges 发明了活性屏离子渗氮技术,解决了直流离子渗氮存在的问题。活性屏离子渗氮处理技术,是将阴极电位施加在一个所谓的活性屏(金属屏)上,而不施加在被处理的工件上,故完全可避免工件表面打弧、空心阴极效应和边缘效应等问题。1987年美国威斯康辛大学 Conrad 教授提出了等离子源离子注入技术,随后 Collins 教授等提出等离子体浸没离子注入技术,实质上是在等离子源离子注入技术的基础上增加温度辅助作用,使注入的氮元素向表层深处扩散,以增大硬化层深度。 Luxembourg engineer Georges invented active screen ion nitriding technology, which solved the problems of direct current ion nitriding. Active screen ion nitriding treatment technology is to apply the cathode potential on a so-called active screen (metal screen) instead of on the workpiece to be processed, so it can completely avoid arcing on the surface of the workpiece, hollow cathode effect and edge effect And other issues. In 1987, Professor Conrad of the University of Wisconsin in the United States proposed the plasma source ion implantation technology, and then Professor Collins et al. proposed the plasma immersion ion implantation technology, which essentially added temperature assistance on the basis of the plasma source ion implantation technology, so that the implanted nitrogen element could Diffusion deep into the surface to increase the depth of the hardened layer.
上述方案在一定程度上发展了渗氮工艺,但离子渗氮的渗层浅,对结构复杂的金属零部件难以保证渗层均匀一致,且设备复杂、初期投资大,其大范围的推广应用受到限制。The above scheme has developed the nitriding process to a certain extent, but the ionized nitriding layer is shallow, and it is difficult to ensure a uniform layer for metal parts with complex structures, and the equipment is complicated and the initial investment is large. limit.
等离子源辅助渗氮技术是将等离子体的产生与工件独立,在更低气压下进行,在炉内单独配制的一个等离子体发生器,离化含氮气体进行渗氮。Zerwiec总结分析各种离子源辅助渗氮技术后,指出离子源辅助渗氮技术,氮离子大部分通过注入方式进入材料表面,入射离子逐渐损失能量,最后停留在材料中,并引起材料表面成分、结构和性能发生变化,获得优异性能。Plasma source assisted nitriding technology is to separate the generation of plasma from the workpiece at a lower pressure. A plasma generator is separately prepared in the furnace to ionize nitrogen-containing gas for nitriding. After summarizing and analyzing various ion source-assisted nitriding technologies, Zerwiec pointed out that in the ion source-assisted nitriding technology, most of the nitrogen ions enter the surface of the material through implantation, and the incident ions gradually lose energy, and finally stay in the material, causing the surface composition of the material, The structure and performance change, and excellent performance is obtained.
发明内容:Invention content:
针对目前渗氮工艺的不足,为控制渗氮层中化合物的厚度,以及改善化合物层的疏松性,本发明提供一种热作模具表面电弧等离子体辅助低压渗氮方法,采用低压、脉冲以及渗氮气氛中通入Ar-H2-N2相结合来制备具有高强度和高韧性渗氮层。Aiming at the deficiencies of the current nitriding process, in order to control the thickness of the compound in the nitriding layer and improve the porosity of the compound layer, the present invention provides a low-pressure nitriding method assisted by arc plasma on the surface of a hot work mold, which adopts low pressure, pulse and nitriding Nitriding layers with high strength and toughness are prepared by passing Ar-H 2 -N 2 into nitrogen atmosphere.
本发明的目的通过以下技术方案实现:The object of the present invention is achieved through the following technical solutions:
一种热作模具表面电弧等离子体辅助低压渗氮方法,包括以下步骤:A method of arc plasma assisted low pressure nitriding on the surface of a hot work mold, comprising the following steps:
1)工件为不同前处理状态的 4Cr5MoSiV1 热作模具钢,经超声波清洗、吹干,置于低压渗氮装置中,依次开启机械泵、分子涡轮泵抽真空至本底真空,加热至 300-600℃,去除真空室内残留物;1) The workpiece is 4Cr5MoSiV1 hot-working die steel in different pre-treatment states. After ultrasonic cleaning and drying, it is placed in a low-pressure nitriding device, and the mechanical pump and molecular turbo pump are turned on in turn to evacuate to the background vacuum, and heated to 300-600 ℃, remove the residue in the vacuum chamber;
2)保持反应炉内温度 300-500℃,反应炉内气压为2.0×10-2 -4.0×10-3 Pa,工件转平台接脉冲电源负极,电弧靶引弧,通氩气,反应炉内气压保持 0.2-1.0Pa,对工件表面进行离子刻蚀 30-60min;2) Keep the temperature in the reaction furnace at 300-500°C, the air pressure in the reaction furnace is 2.0×10 -2 -4.0×10 -3 Pa, the workpiece transfer platform is connected to the negative pole of the pulse power supply, the arc target is ignited, and the argon gas is passed through the reaction furnace. Keep the air pressure at 0.2-1.0Pa, and perform ion etching on the surface of the workpiece for 30-60min;
3)向反应炉内连续通入高纯 N2、高纯 H2 和惰性气体 Ar,保持反应炉内温度和气压恒定,工件转平台接脉冲电源负极,电弧靶电流 80-85A保持恒定,进行 60-120min 等离子渗氮;3) Continuously feed high-purity N 2 , high-purity H 2 and inert gas Ar into the reaction furnace to keep the temperature and air pressure in the reaction furnace constant. 60-120min plasma nitriding;
4)随后开启炉体循环冷却水系统冷却 60-120min,工件在低真空状态下随炉冷却至室温,开启真空炉并取出工件。4) Then turn on the circulating cooling water system of the furnace body to cool for 60-120 minutes, the workpiece is cooled to room temperature with the furnace in a low vacuum state, turn on the vacuum furnace and take out the workpiece.
进一步地,步骤1)所述的不同前处理状态的 H13 热作模具钢分别为喷砂态、砂轮研磨态、砂纸磨光态(1000#)、机械抛光态。Further, the H13 hot work die steels in different pretreatment states described in step 1) are sandblasting state, grinding wheel grinding state, sandpaper polishing state (1000#), and mechanical polishing state.
进一步地,步骤1)所述的加热采用红外电加热管加热,装置腔室内的实际温度由热电偶测量。Further, the heating described in step 1) is heated by an infrared electric heating tube, and the actual temperature in the chamber of the device is measured by a thermocouple.
进一步地,步骤2)与步骤3)所述的工件转平台接脉冲电源,负偏压均为 300-500V,采用双极脉冲,脉冲频率 10-20kHz,占空比 0.8-1.0。Further, the workpiece transfer platform described in step 2) and step 3) is connected to the pulse power supply, the negative bias voltage is 300-500V, bipolar pulse is used, the pulse frequency is 10-20kHz, and the duty cycle is 0.8-1.0.
进一步地,步骤2)所述的电弧靶电流为 80-85A。Further, the arc target current in step 2) is 80-85A.
进一步地,步骤2)所述的氩气流量为 180-200 mL/min。Further, the flow rate of argon in step 2) is 180-200 mL/min.
进一步地,步骤2)所述的离子刻蚀是指电弧增强辉光放电技术;所述电弧增强辉光放电技术,电弧增强辉光放电技术,是通过弧光放电产生高密度电子,电子与通入氩气碰撞,电离出 Ar+,对工件表面进行刻蚀。所述电弧靶采用 Ti靶。Further, the ion etching in step 2) refers to the arc-enhanced glow discharge technology; the arc-enhanced glow discharge technology, the arc-enhanced glow discharge technology, is to generate high-density electrons through arc discharge, and the electrons and access Argon collides, ionizes Ar + , and etches the surface of the workpiece. The arc target adopts Ti target.
进一步地,步骤3)所述的 N2 流量为 25-50mL/min,H2 流量为 25-50mL/min,Ar流量为 80-120 mL/min。Further, the N 2 flow rate in step 3) is 25-50 mL/min, the H 2 flow rate is 25-50 mL/min, and the Ar flow rate is 80-120 mL/min.
进一步地,步骤3)所述的温度 300-500℃,气压 0.2-1.0Pa。Further, the temperature in step 3) is 300-500°C, and the air pressure is 0.2-1.0Pa.
进一步地,所述反应炉为实验采用Metaplas-Domino mini型设备。Further, the reaction furnace adopts Metaplas-Domino mini equipment for the experiment.
更进一步地,实现本发明目的的技术方案按照以下步骤:Furthermore, the technical solution for realizing the object of the present invention follows the steps below:
(1)选取不同前处理状态的H13钢工件,用丙酮溶液超声清洗20 min,取出后用吹风机吹干,置于电弧等离子体辅助渗氮装置中进行渗氮处理。(1) H13 steel workpieces in different pre-treatment states were selected, ultrasonically cleaned with acetone solution for 20 min, taken out, dried with a hair dryer, and placed in an arc plasma assisted nitriding device for nitriding treatment.
(2)保持炉内温度 500℃,真空室内气压为 4.0×10-3Pa,工件转平台接脉冲电源,电弧靶引弧,通氩气,炉内气压保持 0.2-1.0 Pa,对工件表面进行离子刻蚀 60min。(2) Keep the temperature in the furnace at 500°C, the air pressure in the vacuum chamber is 4.0×10 -3 Pa, the workpiece transfer platform is connected to the pulse power supply, the arc target arc is ignited, and the argon gas is supplied, and the pressure in the furnace is kept at 0.2-1.0 Pa. Ion etching for 60min.
(3)向炉内连续通入一定流量高纯 N2,高纯 H2,以及惰性气体 Ar,保持炉内温度和气压恒定,工件转平台接脉冲电源,电弧靶电流保持恒定,进行120min等离子渗氮。(3) Continuously feed a certain flow of high-purity N 2 , high-purity H 2 , and inert gas Ar into the furnace to keep the temperature and air pressure in the furnace constant. The workpiece transfer platform is connected to a pulse power supply, and the current of the arc target is kept constant for 120 minutes. Nitriding.
(4)随后开启炉体循环冷却水系统冷却 60min,工件在低真空状态下随炉冷却至室温,开启真空炉并取出工件。(4) Then turn on the circulating cooling water system of the furnace body to cool for 60 minutes. The workpiece is cooled to room temperature with the furnace in a low vacuum state, and the vacuum furnace is turned on and the workpiece is taken out.
步骤1所述的不同前处理状态的H13热作模具钢分别为喷砂态、砂轮研磨态、砂纸磨光态(1000#)、机械抛光态。The H13 hot work die steels in different pretreatment states described in step 1 are sandblasting state, grinding wheel grinding state, sandpaper polishing state (1000#), and mechanical polishing state.
步骤2中的等离子刻蚀是电弧增强辉光放电技术,刻蚀过程中工件转平台接脉冲电源。而碰撞出的 Ar+刻蚀工件表面,去除表面的氧化物。The plasma etching in step 2 is an arc-enhanced glow discharge technology, and the workpiece is transferred to the platform and connected to a pulse power supply during the etching process. The collided Ar + etches the surface of the workpiece and removes the oxide on the surface.
步骤2中氩气流量为 190 mL/min。The argon flow rate in step 2 was 190 mL/min.
步骤2与步骤3中工件转台接脉冲电源,负偏压为 300V,脉冲频率 20kHz,占空比0.8。电弧靶采用Ti靶,电弧靶电流为 80-85A,靶前面附有挡板,蒸发的Ti离子(或原子)沉积在挡板上,从而碰撞产生Ar+。In step 2 and step 3, the workpiece turntable is connected to the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty ratio is 0.8. The arc target adopts Ti target, the current of the arc target is 80-85A, and a baffle is attached in front of the target, and the evaporated Ti ions (or atoms) are deposited on the baffle, thereby colliding to generate Ar + .
步骤3中渗氮过程中N2流量为 50mL/min,H2流量为 25 mL/min,Ar 流量为 120mL/min。渗氮过程中通入 Ar,通过控制 Ar的流量控制炉内气压保持在 1.0Pa。During the nitriding process in step 3, the N 2 flow rate is 50 mL/min, the H 2 flow rate is 25 mL/min, and the Ar flow rate is 120 mL/min. During the nitriding process, Ar is introduced, and the pressure in the furnace is controlled at 1.0 Pa by controlling the flow rate of Ar.
步骤3中渗氮温度和气压保持恒定,气压为1.0Pa,温度为 500℃。In step 3, the nitriding temperature and air pressure are kept constant, the air pressure is 1.0 Pa, and the temperature is 500°C.
步骤3中渗氮过程中通有惰性气体氩气,降低了气氛中的氮浓度,抑制化合物层的产生,降低硬度梯度;此外,通过氩离子有效地轰击活化工件表面,以达到增加氮原子扩散通道,加速渗氮过程,最终得到高强度高韧性的表层。渗氮层中化合物层厚度小于0-3μm,硬度1000-1300 HV0.1,脆性等级小于1级,疏松级别小于1级。In step 3, the inert gas argon is passed through the nitriding process, which reduces the nitrogen concentration in the atmosphere, suppresses the generation of the compound layer, and reduces the hardness gradient; in addition, the surface of the workpiece is effectively bombarded and activated by argon ions to achieve the increase of nitrogen atoms The diffusion channel accelerates the nitriding process, and finally obtains a high-strength and high-toughness surface layer. The thickness of the compound layer in the nitriding layer is less than 0-3μm, the hardness is 1000-1300 HV 0.1 , the brittleness level is less than 1 level, and the porosity level is less than 1 level.
步骤3中电弧等离子体辅助渗氮工艺将传统的辉光放电改为辉光放电与弧光放电的结合,渗氮工作气压为 1.0Pa,低压增加了氮的自由程,利于氮的扩散;基体接入脉冲电源,脉冲频率高达 20kHz,灭弧速度快,弧光点能量小,对零件表面不产生任何电弧损伤,并且可以有效的抑制“空心阴极效应”。In step 3, the arc plasma assisted nitriding process changes the traditional glow discharge into a combination of glow discharge and arc discharge. The working pressure of nitriding is 1.0Pa. Input pulse power supply, the pulse frequency is as high as 20kHz, the arc extinguishing speed is fast, the energy of the arc point is small, no arc damage is caused to the surface of the parts, and the "hollow cathode effect" can be effectively suppressed.
所述的反应炉为实验采用 Metaplas-Domino mini 型设备。Described reaction furnace adopts Metaplas-Domino mini type equipment for experiment.
本发明等离子辅助渗氮技术原理为:The principle of plasma assisted nitriding technology of the present invention is:
等离子源辅助渗氮技术是将等离子体的产生与工件独立,在更低气压下进行,在炉内单独配制的一个等离子体发生器,离化含氮气体进行渗氮,氮大部分通过注入方式进入材料表面,入射离子逐渐损失能量,最后停留在材料中,并引起材料表面成分、结构和性能发生变化,获得优异性能。Plasma source-assisted nitriding technology is to separate the generation of plasma from the workpiece and carry out at lower pressure. A plasma generator is separately prepared in the furnace to ionize nitrogen-containing gas for nitriding. Most of the nitrogen is injected. Entering the surface of the material, the incident ions gradually lose energy, and finally stay in the material, causing changes in the surface composition, structure and properties of the material, and obtaining excellent performance.
与现有技术相比, 本发明具有的有益效果如下:Compared with the prior art, the present invention has the following beneficial effects:
(1)本发明电弧等离子体辅助低压渗氮技术能够改善传统离子渗氮的不足,弧光放电具有较高的等离子密度,所需辉光能量小,避免对工件表面造成的损伤。当渗氮压力很低时,单位体积内分子数量很少,铁离子自由程较长,工件表面形成及沉积的铁氮化物 FeN几率就低,同时,较高动能的离子轰击表面引起新形成的化合物层被溅射。(1) The arc plasma-assisted low-pressure nitriding technology of the present invention can improve the shortcomings of traditional ion nitriding. The arc discharge has a higher plasma density, requires less glow energy, and avoids damage to the workpiece surface. When the nitriding pressure is very low, the number of molecules per unit volume is small, the free path of iron ions is longer, and the probability of forming and depositing iron nitride FeN on the surface of the workpiece is low. At the same time, ions with higher kinetic energy bombard the surface to cause new formation. The compound layer is sputtered.
(2)工件转平台接入脉冲电源,采用双极脉冲,频率高达 20kHz,灭弧速度快,对零件表面不产生任何电弧损伤,并且可以有效的抑制“空心阴极效应”。(2) The workpiece transfer platform is connected to the pulse power supply, using bipolar pulses, the frequency is as high as 20kHz, the arc extinguishing speed is fast, no arc damage is caused to the surface of the parts, and the "hollow cathode effect" can be effectively suppressed.
(3)通过氩离子有效地轰击活化工件表面,以达到增加氮原子扩散通道,加速渗氮过程,避免化合物层的形成,同时提高工件的热疲劳性能。(3) The surface of the workpiece is effectively bombarded and activated by argon ions to increase the diffusion channels of nitrogen atoms, accelerate the nitriding process, avoid the formation of compound layers, and improve the thermal fatigue performance of the workpiece.
附图说明Description of drawings
图1为真空腔室工作示意图;Fig. 1 is the working schematic diagram of vacuum chamber;
图2为喷砂态H13钢电弧等离子体辅助渗氮处理后截面硬度梯度曲线图;Fig. 2 is the cross-sectional hardness gradient curve of H13 steel in the sandblasted state after arc plasma assisted nitriding treatment;
图3为喷砂态H13钢横截面渗氮层金相照片;Fig. 3 is the metallographic photograph of the nitrided layer of the H13 steel cross-section in the blasted state;
图4为砂轮研磨态H13钢电弧等离子体辅助渗氮处理后截面硬度梯度曲线图;Fig. 4 is a cross-sectional hardness gradient curve of H13 steel in the grinding state of grinding wheel after arc plasma assisted nitriding treatment;
图5为砂轮研磨态H13钢横截面渗氮层金相照片;Fig. 5 is the metallographic photograph of the nitriding layer of the H13 steel cross-section in the grinding state of the grinding wheel;
图6为砂纸磨光态(1000#)H13钢电弧等离子体辅助渗氮处理后截面硬度梯度曲线图;Fig. 6 is the hardness gradient curve of the cross section of H13 steel in the state of sandpaper grinding (1000#) after arc plasma assisted nitriding treatment;
图7为砂纸磨光态(1000#)H13钢横截面渗氮层金相照片;Figure 7 is a metallographic photo of the nitrided layer of the H13 steel cross-section in the state of sandpaper grinding (1000#);
图8为机械抛光态H13钢电弧等离子体辅助渗氮处理后截面硬度梯度曲线图;Fig. 8 is a curve diagram of the cross-section hardness gradient of mechanically polished H13 steel after arc plasma assisted nitriding treatment;
图9为机械抛光态H13钢横截面渗氮层金相照片。Fig. 9 is a metallographic photo of the nitrided layer of the H13 steel cross-section in the mechanically polished state.
具体实施方式:detailed description:
下面结合具体的实施例对本发明作进一步的说明,但并不局限于此。The present invention will be further described below in conjunction with specific examples, but is not limited thereto.
实施例1 —工件表面喷砂Embodiment 1—workpiece surface blasting
(1)工件为经过喷砂处理的H13钢,喷砂粒度80目,粗糙度Ra 1.4μm,用丙酮溶液超声清洗工件20分钟,取出后用吹风机吹干,置于电弧等离子体辅助渗氮装置中进行渗氮处理,依次开启机械泵、分子涡轮泵抽真空至本底真空,加热至 600℃,去除真空室内残留物。(1) The workpiece is H13 steel that has been sandblasted, with a sandblasting particle size of 80 mesh and a roughness Ra of 1.4 μm. The workpiece is ultrasonically cleaned with acetone solution for 20 minutes, taken out and dried with a hair dryer, and placed in an arc plasma assisted nitriding device Carry out nitriding treatment in the vacuum chamber, turn on the mechanical pump and the molecular turbo pump in turn to evacuate to the background vacuum, heat to 600°C, and remove the residue in the vacuum chamber.
(2)保持炉内温度保持 500℃,真空室内气压为 4.0×10-3Pa,工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20kHz,占空比 0.8。电弧靶引弧,电弧靶采用Ti靶,靶电流为 85A,靶前面附有挡板,蒸发的Ti离子沉积在挡板上,从而碰撞产生Ar+,刻蚀工件表面,去除表面的氧化物。通氩气,氩气流量为 190 mL/min,炉内气压保持 1.0 Pa,对工件表面进行离子刻蚀 60min。(2) Keep the temperature in the furnace at 500°C, the air pressure in the vacuum chamber is 4.0×10 -3 Pa, the workpiece transfer platform is connected to the negative electrode of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target is used to start the arc. The arc target uses a Ti target. The target current is 85A. There is a baffle in front of the target. The evaporated Ti ions are deposited on the baffle, thereby colliding to generate Ar + , etching the surface of the workpiece, and removing the oxide on the surface. The argon flow rate is 190 mL/min, the pressure in the furnace is kept at 1.0 Pa, and the surface of the workpiece is ion-etched for 60 min.
(3)向炉内连续通入定流量高纯度N2,高纯度H2,以及惰性气体 Ar,N2流量为 50mL/min,H2流量为 25 mL/min,Ar流量为 120 mL/min。工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20kHz,占空比 0.8。电弧靶电流为 85A,保持气压 1.0Pa,温度 500℃,进行 120min等离子渗氮。(3) Continuously feed constant flow of high-purity N 2 , high-purity H 2 , and inert gas Ar into the furnace. The flow rate of N 2 is 50 mL/min, the flow rate of H 2 is 25 mL/min, and the flow rate of Ar is 120 mL/min. The workpiece transfer platform is connected to the negative pole of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target current is 85A, the air pressure is kept at 1.0Pa, the temperature is 500°C, and plasma nitriding is carried out for 120min.
(4)随后开启炉体冷却水循环系统冷却 60min,工件在 1.0×10-7Pa真空下随炉冷却至室温,开启真空炉并取出工件, 图1为真空腔室工作示意图。(4) Then turn on the cooling water circulation system of the furnace body to cool for 60 minutes. The workpiece is cooled to room temperature with the furnace under a vacuum of 1.0×10 -7 Pa. Then turn on the vacuum furnace and take out the workpiece. Figure 1 is a schematic diagram of the vacuum chamber.
喷砂态的H13钢,经上述 500℃电弧等离子体辅助渗氮后硬度梯度曲线见图2,其表层硬度为1192.0 HV0.2,2h渗氮渗层深度在 15-20 μm之间,渗氮层中扩散层中没有出现呈脉状分布的渗氮物,氮化物级别为1级,见图3。The H13 steel in the sandblasted state has a hardness gradient curve after the above-mentioned 500°C arc plasma assisted nitriding is shown in Figure 2. The surface hardness is 1192.0 HV 0.2 , and the depth of the nitriding layer is between 15-20 μm in 2 hours. There is no vein-like distribution of nitride in the middle diffusion layer, and the nitride level is level 1, as shown in Figure 3.
机械研磨态的H13钢,原始粗糙度为1.4μm,渗氮后粗糙度依然为1.4μm,经喷砂后表面产生较大的晶格畸变,位错密度增加,Ar+对表面的轰击效果不明显,金相显微镜(500×)下化合物层厚度约为 3μm。压痕测试表明表层脆性良好,压痕四周没有明显裂纹,脆性等级为1级。The mechanically ground H13 steel has an original roughness of 1.4 μm, and the roughness after nitriding is still 1.4 μm. After sandblasting, the surface has a large lattice distortion, the dislocation density increases, and the bombardment effect of Ar + on the surface is not good. Obviously, the thickness of the compound layer under the metallographic microscope (500×) is about 3 μm. The indentation test shows that the brittleness of the surface layer is good, there are no obvious cracks around the indentation, and the brittleness grade is level 1.
实施例2 —工件表面砂轮研磨Embodiment 2—workpiece surface grinding wheel grinding
(1)工件为砂轮研磨态的H13钢,粗糙度 Ra 0.8μm,用丙酮溶液超声清洗工件20分钟,取出后用吹风机吹干,置于电弧等离子体辅助渗氮装置中进行渗氮处理,依次开启机械泵、分子涡轮泵抽真空至本底真空,加热至 600℃,去除真空室内残留物。(1) The workpiece is H13 steel in the grinding state of the grinding wheel, with a roughness Ra of 0.8 μm. The workpiece is ultrasonically cleaned with acetone solution for 20 minutes. After taking it out, it is dried with a hair dryer, and placed in an arc plasma assisted nitriding device for nitriding treatment. Turn on the mechanical pump and the molecular turbo pump to evacuate to the background vacuum, heat to 600°C, and remove the residue in the vacuum chamber.
(2)保持炉内温度保持 500℃,真空室内气压为 4.0×10-3Pa,工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20kHz,占空比 0.8。电弧靶引弧,电弧靶采用Ti靶,靶电流为 85A,靶前面附有挡板,蒸发的Ti离子沉积在挡板上,从而碰撞产生Ar+,刻蚀工件表面,去除表面的氧化物。通氩气,氩气流量为 190 mL/min,炉内气压保持 1.0Pa,对工件表面进行离子刻蚀 60min。(2) Keep the temperature in the furnace at 500°C, the air pressure in the vacuum chamber is 4.0×10 -3 Pa, the workpiece transfer platform is connected to the negative electrode of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target is used to strike the arc. The arc target uses a Ti target. The target current is 85A. There is a baffle in front of the target. The evaporated Ti ions are deposited on the baffle, thereby colliding to generate Ar + , etching the surface of the workpiece, and removing the oxide on the surface. The argon flow rate is 190 mL/min, the pressure in the furnace is kept at 1.0 Pa, and the surface of the workpiece is ion-etched for 60 min.
(3)向炉内连续通入定流量高纯度 N2,高纯度 H2,以及惰性气体 Ar,N2流量为 50mL/min,H2流量 为25 mL/min,Ar流量为 120 mL/min。工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20 kHz,占空比0.8。电弧靶电流为 85A,保持气压 1.0Pa,温度 500℃,进行 120min等离子渗氮。(3) Continuously feed constant flow of high-purity N 2 , high-purity H 2 , and inert gas Ar into the furnace. The flow rate of N 2 is 50 mL/min, the flow rate of H 2 is 25 mL/min, and the flow rate of Ar is 120 mL/min. The workpiece transfer platform is connected to the negative pole of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20 kHz, and the duty cycle is 0.8. The arc target current is 85A, the air pressure is kept at 1.0Pa, the temperature is 500°C, and plasma nitriding is carried out for 120min.
(4)随后开启炉体冷却水循环系统冷却 60min,工件在 1.0×10-7Pa真空状态下随炉冷却至室温,开启真空炉并取出工件。(4) Then turn on the cooling water circulation system of the furnace body to cool for 60 minutes, the workpiece is cooled to room temperature with the furnace under a vacuum state of 1.0×10 -7 Pa, turn on the vacuum furnace and take out the workpiece.
砂轮研磨态的H13钢,经上述500oC电弧等离子体辅助渗氮后硬度梯度曲线见图4,其表层硬度为 1314.8 HV0.2,表面研磨态增加扩散通道,2h渗氮渗层深度增加,在 30-35 μm之间,渗氮层中扩散层中没有出现呈脉状分布的渗氮物,氮化物级别为1级,见图5。The hardness gradient curve of H13 steel in grinding wheel grinding state is shown in Fig. 4 after the above 500 o C arc plasma assisted nitriding. Between 30-35 μm, there is no vein-like distribution of nitride in the diffusion layer in the nitrided layer, and the nitride level is level 1, as shown in Figure 5.
砂轮研磨态的H13钢,原始粗糙度为 0.80μm,渗氮过程中由于Ar+的轰击,渗氮后粗糙度为 0.90μm,金相显微镜(500×)下化合物层厚度约为2μm。压痕测试表明表层脆性良好,压痕四周没有明显裂纹,脆性等级为1级。The H13 steel in the state of grinding wheel grinding has an original roughness of 0.80 μm. Due to the bombardment of Ar + during the nitriding process, the roughness after nitriding is 0.90 μm, and the thickness of the compound layer under the metallographic microscope (500×) is about 2 μm. The indentation test shows that the brittleness of the surface layer is good, and there are no obvious cracks around the indentation, and the brittleness grade is level 1.
实施例3 —工件表面砂纸研磨Embodiment 3—workpiece surface sandpaper grinding
(1)工件为砂纸磨光态(1000#)H13钢,粗糙度Ra 0.35μm,用丙酮溶液超声清洗工件20分钟,取出后用吹风机吹干,置于电弧等离子体辅助渗氮装置中进行渗氮处理,依次开启机械泵、分子涡轮泵抽真空至本底真空,加热至 600℃,去除真空室内残留物。(1) The workpiece is sandpaper-polished (1000#) H13 steel, with a roughness of Ra 0.35 μm. The workpiece is ultrasonically cleaned with acetone solution for 20 minutes. After taking it out, it is dried with a hair dryer and placed in an arc plasma assisted nitriding device for nitriding For nitrogen treatment, turn on the mechanical pump and molecular turbo pump in turn to evacuate to the background vacuum, heat to 600°C, and remove the residue in the vacuum chamber.
(2)保持炉内温度保持 500℃,真空室内气压为 4.0×10-3Pa,工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20kHz,占空比 0.8。电弧靶引弧,电弧靶采用 Ti 靶,靶电流为 85A,靶前面附有挡板,蒸发的Ti离子沉积在挡板上,从而碰撞产生 Ar+,刻蚀工件表面,去除表面的氧化物。通氩气,氩气流量为190 mL/min,炉内气压保持 1.0Pa,对工件表面进行离子刻蚀 60min。(2) Keep the temperature in the furnace at 500°C, the air pressure in the vacuum chamber is 4.0×10 -3 Pa, the workpiece transfer platform is connected to the negative electrode of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target is used to start the arc. The arc target uses a Ti target. The target current is 85A. There is a baffle in front of the target. The evaporated Ti ions are deposited on the baffle, thereby colliding to generate Ar + , etching the surface of the workpiece, and removing the oxide on the surface. The argon flow rate is 190 mL/min, the pressure in the furnace is kept at 1.0 Pa, and ion etching is performed on the surface of the workpiece for 60 min.
(3)向炉内连续通入定流量高纯度 N2,高纯度 H2,以及惰性气体 Ar,N2流量为 50mL/min,H2流量为 25 mL/min,Ar流量为 120 mL/min。工件转平台接脉冲电源负极,负偏压为 300V,脉冲频率 20kHz,占空比 0.8。电弧靶电流为 85A,保持气压 1.0Pa,温度 500℃,进行 120min等离子渗氮。(3) Continuously feed constant flow of high-purity N 2 , high-purity H 2 , and inert gas Ar into the furnace. The flow rate of N 2 is 50 mL/min, the flow rate of H 2 is 25 mL/min, and the flow rate of Ar is 120 mL/min. The workpiece transfer platform is connected to the negative pole of the pulse power supply, the negative bias voltage is 300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target current is 85A, the air pressure is kept at 1.0Pa, the temperature is 500°C, and plasma nitriding is carried out for 120min.
(4)随后开启炉体冷却水循环系统冷却 60min,工件 1.0×10-7Pa真空状态下随炉冷却至室温,开启真空炉并取出工件。(4) Then turn on the cooling water circulation system of the furnace body to cool for 60 minutes, the workpiece is cooled to room temperature with the furnace under a vacuum state of 1.0×10 -7 Pa, and the vacuum furnace is turned on and the workpiece is taken out.
砂纸磨光态(1000#)H13钢,经上述 500℃电弧等离子体辅助渗氮后硬度梯度曲线见图6,表面研磨态增加扩散通道,2h渗氮渗层深度增加,在 30-35μm之间,其表层硬度为1312.4HV0.2 渗氮层中扩散层中没有出现呈脉状分布的渗氮物,氮化物级别为1级,见图7。The hardness gradient curve of H13 steel in the sandpaper ground state (1000#) after the above-mentioned 500°C arc plasma assisted nitriding is shown in Figure 6. The surface ground state increases the diffusion channel, and the depth of the nitriding layer increases after 2 hours, between 30-35 μm , the surface hardness is 1312.4HV 0.2 In the nitrided layer, there is no vein-like distribution of nitrides in the diffusion layer, and the nitride level is level 1, as shown in Figure 7.
砂纸磨光态(1000#)H13钢,原始粗糙度为0.35μm,渗氮过程中由于Ar+的轰击,渗氮后粗糙度为0.65μm,金相显微镜(500×)下化合物层厚度约为1μm。压痕测试表明表层脆性良好,压痕四周没有明显裂纹,脆性等级为1级。Sandpaper polished state (1000#) H13 steel, the original roughness is 0.35μm, due to the bombardment of Ar + during the nitriding process, the roughness after nitriding is 0.65μm, the thickness of the compound layer under the metallographic microscope (500×) is about 1 μm. The indentation test shows that the brittleness of the surface layer is good, and there are no obvious cracks around the indentation, and the brittleness grade is level 1.
实施例4 —工件表面研磨抛光Embodiment 4—workpiece surface grinding and polishing
(1)工件为机械抛光态的H13钢,粗糙度Ra0.05μm,用丙酮溶液超声清洗工件20分钟,取出后用吹风机吹干,置于电弧等离子体辅助渗氮装置中进行渗氮处理,依次开启机械泵、分子涡轮泵抽真空至本底真空,加热至 600℃,去除真空室内残留物。(1) The workpiece is mechanically polished H13 steel with a roughness of Ra0.05μm. The workpiece is ultrasonically cleaned with acetone solution for 20 minutes. After taking it out, it is dried with a hair dryer and placed in an arc plasma assisted nitriding device for nitriding treatment. Turn on the mechanical pump and the molecular turbo pump to evacuate to the background vacuum, heat to 600°C, and remove the residue in the vacuum chamber.
(2)保持炉内温度保持 500℃,真空室内气压为 4.0×10-3Pa,工件转平台接脉冲电源负极,偏压为 -300V,脉冲频率 20kHz,占空比 0.8。电弧靶引弧,电弧靶采用的Ti靶,电弧靶电流为 85A,靶前面附有挡板,蒸发的Ti离子沉积在挡板上,从而碰撞产生 Ar+,刻蚀工件表面,去除表面的氧化物。通氩气,氩气流量为 190 mL/min,炉内气压保持 1.0Pa,对工件表面进行离子刻蚀 60min。(2) Keep the temperature in the furnace at 500°C, the air pressure in the vacuum chamber is 4.0×10 -3 Pa, the workpiece transfer platform is connected to the negative electrode of the pulse power supply, the bias voltage is -300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc is struck by the arc target. The arc target uses a Ti target. The current of the arc target is 85A. There is a baffle in front of the target. The evaporated Ti ions are deposited on the baffle, thereby colliding to generate Ar + , etching the surface of the workpiece, and removing the oxidation on the surface. thing. The argon flow rate is 190 mL/min, the pressure in the furnace is kept at 1.0 Pa, and ion etching is performed on the surface of the workpiece for 60 min.
(3)向炉内连续通入定流量高纯度N2,高纯度H2,以及惰性气体 Ar,N2流量为 50mL/min,H2流量为 25 mL/min,Ar流量为120 mL/min。工件转平台接脉冲电源负极,偏压为-300V,脉冲频率20kHz,占空比0.8。电弧靶电流为85A,保持气压1.0Pa,温度500 ℃,进行120min等离子渗氮。(3) Continuously feed constant flow of high-purity N 2 , high-purity H 2 , and inert gas Ar into the furnace. The flow rate of N 2 is 50 mL/min, the flow rate of H 2 is 25 mL/min, and the flow rate of Ar is 120 mL/min. The workpiece transfer platform is connected to the negative pole of the pulse power supply, the bias voltage is -300V, the pulse frequency is 20kHz, and the duty cycle is 0.8. The arc target current is 85A, the air pressure is kept at 1.0Pa, and the temperature is 500°C for 120min plasma nitriding.
(4) 随后开启炉体冷却水循环系统冷却60min,工件在1.0×10-7Pa真空状态下随炉冷却至室温,开启真空炉并取出工件。(4) Then turn on the cooling water circulation system of the furnace body to cool for 60 minutes, the workpiece is cooled to room temperature with the furnace under a vacuum state of 1.0×10 -7 Pa, turn on the vacuum furnace and take out the workpiece.
机械抛光态的H13钢,经上述500℃电弧等离子体辅助渗氮后硬度梯度曲线见图8,抛光态较研磨态渗速减小,2h渗氮渗层深度在15-20μm之间,其表层硬度为 1255.2 HV0.2渗氮层中扩散层中没有出现呈脉状分布的渗氮物,氮化物级别为1级,见图9。The mechanically polished H13 steel has a hardness gradient curve after arc plasma assisted nitriding at 500°C as shown in Figure 8. The penetration rate of the polished state is lower than that of the ground state. The hardness is 1255.2 HV 0.2 In the nitrided layer, there is no vein-like distribution of nitrides in the diffusion layer, and the nitride level is level 1, as shown in Figure 9.
机械抛光态的H13钢,原始粗糙度为0.05μm,渗氮过程中由于Ar+的轰击,渗氮后粗糙度为0.40μm,金相显微镜(500×)下化合物层厚度约为1μm。压痕测试表明表层脆性良好,压痕四周没有明显裂纹,脆性等级为1级。The mechanically polished H13 steel has an original roughness of 0.05 μm, and due to the bombardment of Ar + during the nitriding process, the roughness after nitriding is 0.40 μm, and the thickness of the compound layer under the metallographic microscope (500×) is about 1 μm. The indentation test shows that the brittleness of the surface layer is good, and there are no obvious cracks around the indentation, and the brittleness grade is level 1.
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