CN103060764A - Method of plating ZnO film on surface of metal material - Google Patents
Method of plating ZnO film on surface of metal material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000007769 metal material Substances 0.000 title claims abstract description 30
- 238000007747 plating Methods 0.000 title claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000011787 zinc oxide Substances 0.000 claims abstract description 49
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 25
- 239000010409 thin film Substances 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 238000004544 sputter deposition Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000005498 polishing Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000010408 film Substances 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 2
- 239000013077 target material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 28
- 230000008569 process Effects 0.000 abstract description 8
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- 239000000203 mixture Substances 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 22
- 238000000576 coating method Methods 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 7
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- 238000005516 engineering process Methods 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
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- 230000001050 lubricating effect Effects 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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Abstract
本发明在金属材料表面镀ZnO薄膜的方法，涉及材料表面改性领域。所述方法：将金属材料进行表面抛光处理和清洗，放入磁控溅射炉内，氧化锌置于靶位，金属材料与氧化锌的极间距为3-5cm；将磁控溅射炉抽真空至真空度为1.0×10-4Pa-5.0×10-4Pa，充入氩气至压强为1-10Pa，清洗和活化金属材料；充入氧气和氩气的混合气体至压强为20-35Pa，溅射功率50-80W，磁控溅射炉内的温度至320-380°C，保温；关闭电源，将磁控溅射炉内抽真空，冷却至室温出炉。该方法工艺简单，生产成本低；ZnO薄膜在磨损过程中具有明显的发光特性，且摩擦系数低、耐磨性好。
The invention relates to a method for plating a ZnO thin film on the surface of a metal material and relates to the field of material surface modification. The method is as follows: the metal material is subjected to surface polishing treatment and cleaning, put into a magnetron sputtering furnace, zinc oxide is placed at the target position, and the pole distance between the metal material and zinc oxide is 3-5cm; the magnetron sputtering furnace is pumped Vacuum to a vacuum degree of 1.0×10 -4 Pa-5.0×10 -4 Pa, fill in argon to a pressure of 1-10Pa, clean and activate metal materials; fill in a mixture of oxygen and argon to a pressure of 20- 35Pa, sputtering power 50-80W, the temperature in the magnetron sputtering furnace reaches 320-380°C, keep warm; turn off the power, vacuumize the magnetron sputtering furnace, cool to room temperature and leave the furnace. The method has the advantages of simple process and low production cost; the ZnO thin film has obvious luminous characteristics in the wear process, and has low friction coefficient and good wear resistance.
Description
技术领域 technical field
本发明涉及材料表面改性领域，具体涉及在金属材料表面镀ZnO的方法。 The invention relates to the field of material surface modification, in particular to a method for plating ZnO on the surface of metal materials.
背景技术 Background technique
摩擦和磨损是空间机械系统寿命受限的原因之一，如人造卫星的天线驱动系统、太阳能电池帆板机构、光学仪器的驱动机构等。极端的外部条件使得一些难于观察和预测的材料表面磨损状况变化很大，一旦部件超过承受极限而又无法得到及时反馈，将危害整个系统的运行，带来无法估量的损失。为了确保空间机械系统的安全运行，延长航空航天设备的在役寿命，并最大限度的降低损失，对空间机械系统的摩擦过程进行实时监测、定位和预警是必然的要求。 Friction and wear are one of the reasons for the limited life of space mechanical systems, such as the antenna drive system of artificial satellites, the solar cell sail mechanism, and the drive mechanism of optical instruments. Extreme external conditions make some material surface wear conditions that are difficult to observe and predict vary greatly. Once a component exceeds the tolerance limit and cannot get timely feedback, it will jeopardize the operation of the entire system and cause incalculable losses. In order to ensure the safe operation of the space mechanical system, prolong the service life of aerospace equipment, and minimize losses, real-time monitoring, positioning and early warning of the friction process of the space mechanical system are inevitable requirements.
目前，智能摩擦涂层的研究主要集中在摩擦涂层的自修复、环境自适应性。美军已研究成功一种用于武器表面保护的智能涂层系统，该涂层能够找到既具有自修复特性、又能够改变颜色并感知结构损伤或环境变化的材料，可明显提高武器的战斗力和生存能力。然而，这类涂层只是随着环境改变，通过成分变化改善材料表面摩擦性能，并不能为材料表面后期的磨损提供安全预警信号。 At present, the research on intelligent friction coatings mainly focuses on the self-healing and environmental adaptability of friction coatings. The U.S. military has successfully researched an intelligent coating system for weapon surface protection. This coating can find materials that not only have self-healing properties, but also can change color and sense structural damage or environmental changes, which can significantly improve the combat effectiveness and survival of weapons. ability. However, this type of coating only improves the frictional properties of the material surface through compositional changes as the environment changes, and cannot provide a safety early warning signal for the later wear of the material surface.
国内在摩擦过程中通过发光材料诱导发光的预警机制用来监测航空航天机械系统的磨损状况涂层的研究并不多，国外在具有光传感器预警功能的摩擦智能涂层的研究方面也刚刚起步。如美国空军理工学院与加利福尼亚大学合作开发了一种真空电弧-磁控溅射-脉冲激光沉积混合技术在钢表面制备了一种具有光传感器功能的多层摩擦涂层，涂层制备工艺复杂，组分多变，将影响对光信号的判断。 In China, there are not many researches on coatings used to monitor the wear condition of aerospace mechanical systems through early warning mechanisms induced by luminescent materials during the friction process, and foreign research on friction smart coatings with optical sensor early warning functions has just started. For example, the U.S. Air Force Institute of Technology and the University of California have jointly developed a vacuum arc-magnetron sputtering-pulse laser deposition hybrid technology to prepare a multilayer friction coating with optical sensor function on the steel surface. The coating preparation process is complicated. The composition is changeable, which will affect the judgment of the optical signal.
发明内容 Contents of the invention
本发明的目的是提供在金属材料表面镀ZnO薄膜的方法，该方法采用磁控溅射单一技术在金属材料表面镀ZnO薄膜，工艺简单，生产成本低，非常便于工业化生产；金属材料表面的ZnO薄膜在磨损过程中不仅具有明显的发光特性，且摩擦系数低、耐磨性好，通过诱导发光特性的改变实现对金属材料表面磨损情况进行实时监控。 The purpose of the present invention is to provide the method for coating ZnO thin film on the metal material surface, this method adopts magnetron sputtering single technology to plate ZnO thin film on the metal material surface, and technique is simple, and production cost is low, is very convenient to suitability for industrialized production; ZnO on the metal material surface The thin film not only has obvious luminescence characteristics during the wear process, but also has a low friction coefficient and good wear resistance. Real-time monitoring of the wear of the metal material surface can be realized by inducing the change of the luminescence characteristics.
本发明的目的采用如下技术方案实现。 The object of the present invention adopts following technical scheme to realize.
一种在金属材料表面镀ZnO薄膜的方法，包括如下步骤： A method for plating a ZnO thin film on a metal material surface, comprising the steps of:
(1) 将金属材料进行表面抛光处理和清洗； (1) Surface polishing and cleaning of metal materials;
（2）将清洗后的金属材料放入磁控溅射炉内，利用氧化锌靶材在金属材料表面沉积ZnO薄膜。 (2) Put the cleaned metal material into a magnetron sputtering furnace, and use a zinc oxide target to deposit a ZnO film on the surface of the metal material.
步骤（2）利用氧化锌靶材在金属材料表面沉积ZnO薄膜的具体方法为：将氧化锌置于靶位，金属材料与氧化锌的极间距为3-5 cm；将磁控溅射炉抽真空至真空度为1.0×10-4Pa-5.0×10-4Pa，充入氩气至压强为1-10 Pa，对金属材料表面进行清洗和活化；充入氧气和氩气的混合气体至压强为20-35Pa，控制溅射功率50-80W，调节磁控溅射炉内的温度至320-380°C，保温1-5小时；关闭电源，将磁控溅射炉内抽真空至真空度为1.0×10-4Pa-5.0×10-4Pa后，冷却至室温出炉。 Step (2) The specific method of depositing ZnO thin film on the surface of the metal material by using the zinc oxide target material is as follows: place the zinc oxide on the target position, and the pole distance between the metal material and the zinc oxide is 3-5 cm; pump the magnetron sputtering furnace Vacuum to a vacuum degree of 1.0×10 -4 Pa-5.0×10 -4 Pa, fill in argon to a pressure of 1-10 Pa, clean and activate the surface of metal materials; fill in a mixed gas of oxygen and argon to The pressure is 20-35Pa, control the sputtering power to 50-80W, adjust the temperature in the magnetron sputtering furnace to 320-380°C, keep it warm for 1-5 hours; turn off the power, and evacuate the magnetron sputtering furnace to vacuum After the temperature is 1.0×10 -4 Pa-5.0×10 -4 Pa, it is cooled to room temperature and released from the oven.
所述混合气体中氧气和氩气压强比为1：1-3。 The pressure ratio of oxygen and argon in the mixed gas is 1:1-3.
步骤（1）中所述清洗的方法为超声清洗。 The cleaning method described in step (1) is ultrasonic cleaning.
超声清洗的溶剂为丙酮。 The solvent for ultrasonic cleaning is acetone.
有益效果： Beneficial effect:
（1）本发明采用磁控溅射技术实现了在金属材料表面镀具有发光特性的金属氧化物ZnO，方法上比国内外同类涂层采用真空电弧-磁控溅射-脉冲激光沉积混合技术简单，产业化成本低。 (1) The present invention uses magnetron sputtering technology to realize the metal oxide ZnO coating with luminescent properties on the surface of metal materials. The method is simpler than that of similar coatings at home and abroad using vacuum arc-magnetron sputtering-pulse laser deposition hybrid technology , low industrialization cost.
（2） 本发明ZnO薄膜的摩擦系数在0.13-0.14之间且稳定、寿命较长、耐磨性好。采用350nm紫外激光对ZnO薄膜磨损过程进行激发，光谱特性显示，可见光区范围变窄，在530nm处绿光稍微减弱，且在650-750nm处红光区峰值增加，便于对磨损状况进行视觉观察；ZnO薄膜在磨损过程中具有明显的发光特性，通过光学信号的反馈对材料表面结构性能的失效问题进行准确预测。 (2) The friction coefficient of the ZnO thin film of the present invention is between 0.13-0.14 and is stable, has a long life and good wear resistance. Using 350nm ultraviolet laser to excite the wear process of ZnO thin film, the spectral characteristics show that the range of visible light region is narrowed, the green light is slightly weakened at 530nm, and the peak value of red light region is increased at 650-750nm, which is convenient for visual observation of the wear condition; The ZnO thin film has obvious luminescence characteristics during the wear process, and the failure problem of the surface structure performance of the material can be accurately predicted through the feedback of the optical signal.
the
附图说明 Description of drawings
图1为材料3的表面形貌。 Figure 1 shows the surface morphology of material 3.
图2为基体和材料3摩擦系数随时间的变化曲线，其中1-基体，2-材料3。 Figure 2 is the curve of the friction coefficient of the substrate and material 3 versus time, where 1-substrate, 2-material 3.
图3（a）材料3进行摩擦磨损试验后的表面形貌；图3 (b)基体进行摩擦磨损试验后的表面形貌。 Fig. 3 (a) Surface morphology of material 3 after friction and wear test; Fig. 3 (b) Surface morphology of substrate after friction and wear test.
图4材料3在350nm波长激励下磨损前后的发光特性，其中1-磨损前，2-磨损后。 Figure 4. The luminescent properties of material 3 before and after wear under the excitation of 350nm wavelength, where 1-before wear, 2-after wear.
具体实施方式 Detailed ways
本发明是在铝片表面采用磁控溅射设计一种润滑耐磨发光薄膜，通过350nm激光激发实现对摩擦部件在磨损过程中的监控。 The invention adopts magnetron sputtering to design a lubricating and wear-resistant luminescent film on the surface of an aluminum sheet, and realizes monitoring of friction parts in the wear process through 350nm laser excitation.
实施例1 Example 1
在铝片表面镀ZnO薄膜的方法，包括如下步骤： The method for plating ZnO thin film on the surface of aluminum sheet comprises the following steps:
(1) 将铝片进行表面抛光处理，用丙酮进行超声清洗； (1) Polish the aluminum sheet and ultrasonically clean it with acetone;
（2）将超声清洗后的铝片放入磁控溅射炉内，利用氧化锌靶材在铝片表面沉积ZnO薄膜，具体方法如下：将氧化锌置于靶位，铝片与氧化锌的极间距为3 cm；将磁控溅射炉抽真空至真空度为1.0×10-4Pa，充入氩气至压强为5 Pa，对铝片表面进行清洗和活化；充入氧气和氩气的混合气体至压强为25Pa，所述混合气体中氧气和氩气压强比为1：1，溅射功率50W。调节磁控溅射炉内的温度至320°C，保温1小时；关闭电源，将磁控溅射炉内抽真空至真空度为1.0×10-4Pa，冷却至室温出炉，得到表面镀有ZnO薄膜的铝片，称为材料1。
(2) Put the ultrasonically cleaned aluminum sheet into a magnetron sputtering furnace, and use a zinc oxide target to deposit a ZnO film on the surface of the aluminum sheet. The specific method is as follows: place the zinc oxide at the target position, and The pole spacing is 3 cm; the magnetron sputtering furnace is evacuated to a vacuum degree of 1.0×10 -4 Pa, filled with argon to a pressure of 5 Pa, and the surface of the aluminum sheet is cleaned and activated; filled with oxygen and argon The pressure of the mixed gas is 25Pa, the pressure ratio of oxygen and argon in the mixed gas is 1:1, and the sputtering power is 50W. Adjust the temperature in the magnetron sputtering furnace to 320°C and keep it warm for 1 hour; turn off the power, evacuate the magnetron sputtering furnace to a vacuum degree of 1.0×10 -4 Pa, cool to room temperature and leave the furnace to obtain a surface coated with Aluminum flakes of ZnO thin film, referred to as
实施例2 Example 2
在铝片表面镀ZnO薄膜的方法，包括如下步骤： The method for plating ZnO thin film on the surface of aluminum sheet comprises the following steps:
(1) 将铝片进行表面抛光处理，用丙酮进行超声清洗； (1) Polish the aluminum sheet and ultrasonically clean it with acetone;
（2）将超声清洗后的铝片放入磁控溅射炉内，利用氧化锌靶材在铝片表面沉积ZnO薄膜，具体方法如下：将氧化锌置于靶位，铝片与氧化锌的极间距为5 cm；将磁控溅射炉抽真空至真空度为3.0×10-4Pa，充入氩气至压强为10 Pa，对铝片表面进行清洗和活化；充入氧气和氩气的混合气体至压强为30Pa，混合气体中氧气和氩气压强比为1：3，溅射功率60W，调节磁控溅射炉内的温度至380°C，保温5小时；关闭电源，将磁控溅射炉内抽真空至真空度为3.0×10-4Pa后，冷却至室温出炉，得到表面镀有ZnO薄膜的铝片，称为材料2。
(2) Put the ultrasonically cleaned aluminum sheet into a magnetron sputtering furnace, and use a zinc oxide target to deposit a ZnO film on the surface of the aluminum sheet. The specific method is as follows: place the zinc oxide at the target position, and The pole spacing is 5 cm; the magnetron sputtering furnace is evacuated to a vacuum degree of 3.0×10 -4 Pa, filled with argon to a pressure of 10 Pa, and the surface of the aluminum sheet is cleaned and activated; filled with oxygen and argon The pressure of the mixed gas is 30Pa, the pressure ratio of oxygen and argon in the mixed gas is 1:3, the sputtering power is 60W, the temperature in the magnetron sputtering furnace is adjusted to 380°C, and the temperature is kept for 5 hours; Vacuum the controlled sputtering furnace to a vacuum degree of 3.0×10 -4 Pa, cool to room temperature and release from the furnace to obtain an aluminum sheet coated with a ZnO film on the surface, which is called
实施例3 Example 3
在铝片表面镀ZnO薄膜的方法，包括如下步骤： The method for plating ZnO thin film on the surface of aluminum sheet comprises the following steps:
(1) 将铝片进行表面抛光处理，用丙酮进行超声清洗； (1) Polish the aluminum sheet and ultrasonically clean it with acetone;
（2）将超声清洗后的铝片放入磁控溅射炉内，利用氧化锌靶材在铝片表面沉积ZnO薄膜，具体方法如下：将氧化锌置于靶位，铝片与氧化锌的极间距为4cm；将磁控溅射炉抽真空至真空度为1.0×10-4Pa，充入氩气至压强为10 Pa，对铝片表面进行清洗和活化；充入氧气和氩气的混合气体至压强为35Pa，混合气体中氧气和氩气压强比为1：2，功率70W，调节磁控溅射炉内的温度至360°C，保温2小时；关闭电源，将磁控溅射炉内抽真空至真空度为5×10-4Pa后，冷却至室温出炉，得到表面镀有ZnO薄膜的铝片，称为材料3。 (2) Put the ultrasonically cleaned aluminum sheet into a magnetron sputtering furnace, and use a zinc oxide target to deposit a ZnO film on the surface of the aluminum sheet. The specific method is as follows: place the zinc oxide at the target position, and The pole spacing is 4cm; the magnetron sputtering furnace is evacuated to a vacuum degree of 1.0×10 -4 Pa, filled with argon to a pressure of 10 Pa, and the surface of the aluminum sheet is cleaned and activated; Mix the gas to a pressure of 35Pa, the pressure ratio of oxygen and argon in the mixed gas is 1:2, and the power is 70W. Adjust the temperature in the magnetron sputtering furnace to 360°C and keep it warm for 2 hours; After the furnace was evacuated to a vacuum degree of 5×10 -4 Pa, it was cooled to room temperature and released from the furnace to obtain an aluminum sheet coated with a ZnO film on the surface, which was called material 3.
用电镜分别观察材料1-3的表面形貌。其中材料3的表面形貌见图1。该图说明在铝片表面均镀上了具有明显ZnO锥形结构的薄膜，可产生光致发光现象。材料1和2的表面形貌与材料3相同。
The surface morphology of materials 1-3 were observed with electron microscope. The surface morphology of material 3 is shown in Figure 1. This figure shows that the surface of the aluminum sheet is coated with a thin film with an obvious ZnO cone structure, which can produce photoluminescence. The surface morphology of
将材料1-3分别在UMT-2型摩擦磨损试验机上进行摩擦磨损试验：在1N载荷下，GCr15钢球对摩条件下，测得平均摩擦系数为0.13、0.135和0.14。其中材料3和表面未镀有ZnO薄膜的铝片（简称为基体,下同）的摩擦系数随时间的变化曲线见图2。从图2中可以看出，铝片表面镀上ZnO薄膜后，摩擦系数减小，耐磨性能好，使用寿命延长。用电镜观察材料3及基体进行摩擦磨损试验后的表面形貌，结果见图3。从图3可以看出，材料3与基体相比，其磨痕浅，磨损量不明显。材料1和2的摩擦磨损实验结果同材料2.
Materials 1-3 were subjected to friction and wear tests on the UMT-2 friction and wear testing machine: under the load of 1N, the average friction coefficients were 0.13, 0.135 and 0.14 under the rubbing condition of GCr15 steel balls. Among them, the friction coefficient of material 3 and the aluminum sheet (referred to as the substrate, the same below) without ZnO film on the surface is shown in Figure 2. It can be seen from Figure 2 that after the ZnO film is coated on the surface of the aluminum sheet, the friction coefficient is reduced, the wear resistance is good, and the service life is prolonged. The surface morphology of material 3 and the substrate after the friction and wear test was observed with an electron microscope, and the results are shown in Figure 3. It can be seen from Fig. 3 that compared with the matrix, material 3 has shallow wear scars and the amount of wear is not obvious. The friction and wear test results of
对磨损前后的材料3采用350nm紫外激光（Labram HR800激光拉曼光谱仪）激发，得到了图4。从图4可以看出，ZnO薄膜随着磨损的进行，显示出不同的发光信号，可见光区绿光和红光仍然存在，但绿光有所减弱，便于对磨损状况进行视觉观察，从而实现对金属材料表面磨损情况的实时监控。材料1、2和3在350nm紫外激光下的发光性能相同。
Material 3 before and after wear was excited by a 350nm ultraviolet laser (Labram HR800 laser Raman spectrometer), and Figure 4 was obtained. It can be seen from Figure 4 that the ZnO thin film shows different luminescent signals as the wear progresses. The green light and red light in the visible light region still exist, but the green light is weakened, which is convenient for visual observation of the wear condition, so as to realize the Real-time monitoring of wear on the surface of metal materials.
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