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CN100392145C - Method for preparing aluminum-copper-iron quasicrystal coating by vacuum evaporation - Google Patents

Method for preparing aluminum-copper-iron quasicrystal coating by vacuum evaporation Download PDF

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CN100392145C
CN100392145C CNB2005101117780A CN200510111778A CN100392145C CN 100392145 C CN100392145 C CN 100392145C CN B2005101117780 A CNB2005101117780 A CN B2005101117780A CN 200510111778 A CN200510111778 A CN 200510111778A CN 100392145 C CN100392145 C CN 100392145C
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coating
copper
vacuum evaporation
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ferrum
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CN1789480A (en
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周细应
冷培榆
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Shanghai University of Engineering Science
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Abstract

本发明涉及材料表面工程技术领域,具体地说是一种真空蒸镀制备铝-铜-铁准晶涂层的方法,该制备工艺步骤为:称取质量百分比为65%Al、20%Cu和15%Fe的铝-铜-铁准晶粉末;镀前准备;抽真空达到2×10-3~5×10-3Pa;调节工艺参数;真空蒸镀;缓冷取出;成品。本发明与现有技术相比,涂层制备只需控制准晶粉末的成分配比,涂层的附着性能好,金属离子轰击表面会产生注入效应,有利于提高涂层附着力,镀层组织均匀、致密,有利于该涂层的推广应用,准晶粉末经过真空蒸镀后,在试样表面仍然形成铝-铜-铁准晶涂层,获得的准晶涂层硬度高,摩擦系数低,具有良好的耐磨及抗高温氧化性能。

Figure 200510111778

The invention relates to the technical field of material surface engineering, in particular to a method for preparing an aluminum-copper-iron quasicrystal coating by vacuum evaporation. The preparation process steps are: weighing 65% Al, 20% Cu and 15% Fe aluminum-copper-iron quasicrystalline powder; preparation before plating; vacuuming to 2×10 -3 ~5×10 -3 Pa; adjustment of process parameters; vacuum evaporation; slow cooling and removal; finished product. Compared with the prior art, the present invention only needs to control the composition ratio of the quasi-crystalline powder for the preparation of the coating, and the adhesion of the coating is good. The metal ion bombarding the surface will produce an injection effect, which is beneficial to improve the adhesion of the coating, and the structure of the coating is uniform. , dense, which is conducive to the popularization and application of the coating. After the quasicrystalline powder is vacuum evaporated, an aluminum-copper-iron quasicrystalline coating is still formed on the surface of the sample. The obtained quasicrystalline coating has high hardness and low friction coefficient. It has good wear resistance and high temperature oxidation resistance.

Figure 200510111778

Description

真空蒸镀制备铝-铜-铁准晶涂层的方法 Method for preparing aluminum-copper-iron quasicrystal coating by vacuum evaporation

[技术领域] [technical field]

本发明涉及材料表面工程技术领域,具体地说是一种真空蒸镀制备铝-铜-铁准晶涂层的方法。The invention relates to the technical field of material surface engineering, in particular to a method for preparing an aluminum-copper-iron quasicrystal coating by vacuum evaporation.

[背景技术] [Background technique]

准晶材料是八十年代中后期迅速发展起来的,具有许多优良的性能的新型材料,如硬度高、表面能低、摩擦系数极低,耐热耐蚀性能优良以及光电磁性能优异等性能。因此,准晶材料的这种类似陶瓷材料的特性吸引了涂层技术工作者的广泛注意。由于准晶材料具有脆性大的特点,极大的限制了准晶材料的潜在应用领域。于是,准晶材料的工程应用研究目前主要集中在表面涂层和复合材料两个方面。Quasicrystalline materials were developed rapidly in the middle and late 1980s. They are new materials with many excellent properties, such as high hardness, low surface energy, extremely low coefficient of friction, excellent heat resistance and corrosion resistance, and excellent optical and electromagnetic properties. Therefore, the ceramic-like properties of quasi-crystalline materials have attracted extensive attention of coating technology workers. Due to the high brittleness of quasicrystal materials, the potential application fields of quasicrystal materials are greatly limited. Therefore, the engineering application research of quasicrystalline materials is currently mainly concentrated in two aspects of surface coating and composite materials.

从总体发展与研究成果来看,准晶涂层的形成一般被认为有两个过程:第一步是固态扩散过程;第二步是准晶相的纯化过程。准晶涂层的制备方法主要分为两大类:物理气相沉积(PVD)和热喷涂方法。物理气相沉积法包括真空蒸镀、溅射沉积、激光熔融合成、离子束混合等。From the perspective of overall development and research results, the formation of quasicrystalline coatings is generally considered to have two processes: the first step is the solid-state diffusion process; the second step is the purification process of the quasicrystalline phase. The preparation methods of quasicrystalline coatings are mainly divided into two categories: physical vapor deposition (PVD) and thermal spraying methods. Physical vapor deposition methods include vacuum evaporation, sputtering deposition, laser fusion synthesis, ion beam mixing, etc.

真空蒸镀就是在真空中使金属或化合物升华为气态,然后在基体表面沉积,经退火后得到准晶涂层。目前采用的真空蒸镀法的缺点是涂层成分与母材有较大差异。Vacuum evaporation is to sublimate metal or compound into gaseous state in vacuum, then deposit on the surface of substrate, and obtain quasi-crystalline coating after annealing. The disadvantage of the vacuum evaporation method currently used is that the composition of the coating is quite different from that of the base material.

[发明内容] [Content of the invention]

本发明的目的是克服现有技术的不足,采用真空镀膜机,以难熔金属钼作为加热的蒸发器皿,将铝-铜-铁准晶粉末直接作为待镀合金并在真空中蒸发形成涂层,通过一系列的工艺参数调整来获得准晶涂层的一种真空蒸镀制备铝-铜-铁准晶涂层的方法。The purpose of the present invention is to overcome the deficiencies of the prior art, adopt a vacuum coating machine, use refractory metal molybdenum as a heating evaporation vessel, use aluminum-copper-iron quasicrystal powder directly as the alloy to be plated and evaporate in a vacuum to form a coating , a method for preparing aluminum-copper-iron quasicrystal coatings by vacuum evaporation to obtain quasicrystal coatings through a series of process parameter adjustments.

为实现上述目的,设计一种真空蒸镀制备铝-铜-铁准晶涂层的方法,该制备工艺步骤为:(1)称取质量百分比为65%Al、20%Cu和15%Fe的铝-铜-铁准晶粉末;(2)镀前准备;(3)抽真空达到2×10-3~5×10-3Pa;(4)调节工艺参数;(5)真空蒸镀;(6)缓冷取出;(7)成品。所述的镀前准备为试样砂纸打磨、抛光以及超声波清洗。所述的调节工艺参数为调节蒸镀距离为13厘米、蒸发电流为340安培、蒸发电压为5伏。所述的真空蒸镀是以难熔金属钼作为加热的蒸发器皿,将准晶粉末直接作为待镀合金并在真空中蒸发形成涂层。该方法制备的铝-铜-铁准晶涂层可应用于机械、汽车、石化、电力、化工、航空领域。In order to achieve the above object, design a kind of method that vacuum evaporation prepares aluminum-copper-iron quasicrystal coating, and this preparation process step is: (1) take by weight 65%Al, 20%Cu and 15%Fe Aluminum-copper-iron quasicrystal powder; (2) Preparation before plating; (3) Vacuuming to 2×10 -3 ~ 5×10 -3 Pa; (4) Adjusting process parameters; (5) Vacuum evaporation; ( 6) slowly cooling and taking out; (7) finished product. The preparation before plating includes sanding, polishing and ultrasonic cleaning of the sample. The adjustment process parameters include adjusting the evaporation distance to 13 cm, the evaporation current to 340 amperes, and the evaporation voltage to 5 volts. The vacuum evaporation uses refractory metal molybdenum as a heated evaporation vessel, and the quasicrystal powder is directly used as an alloy to be plated and evaporated in a vacuum to form a coating. The aluminum-copper-iron quasi-crystal coating prepared by the method can be applied to the fields of machinery, automobile, petrochemical, electric power, chemical industry and aviation.

本发明同现有技术相比,涂层制备只需控制准晶粉末的成分配比,涂层的附着性能较好,各种金属离子轰击表面会产生注入效应,有利于提高涂层附着力,镀层组织均匀、致密,有利于该涂层的推广应用,准晶粉末经过真空蒸镀后,在试样表面仍然形成铝-铜-铁准晶涂层,获得的准晶涂层硬度高,摩擦系数低,具有良好的耐磨及抗高温氧化性能。Compared with the prior art, the present invention only needs to control the composition ratio of the quasi-crystal powder in the preparation of the coating, and the adhesion performance of the coating is better, and various metal ions bombard the surface to produce an injection effect, which is beneficial to improve the adhesion of the coating. The coating structure is uniform and dense, which is conducive to the popularization and application of the coating. After the quasicrystalline powder is vacuum evaporated, an aluminum-copper-iron quasicrystalline coating is still formed on the surface of the sample. The obtained quasicrystalline coating has high hardness and friction resistance. Low coefficient, good wear resistance and high temperature oxidation resistance.

[附图说明] [Description of drawings]

图1为本发明的工艺流程图。Fig. 1 is a process flow diagram of the present invention.

参见附图1,1为称取质量百分比为65%Al、20%Cu和15%Fe的准晶粉末;2为镀前准备;3为抽真空达到2×10-3~5×10-3Pa;4为调节工艺参数;5为真空蒸镀;6为缓冷取出;7为成品See attached drawing 1, 1 is quasi-crystalline powder weighing 65% Al, 20% Cu and 15% Fe by mass percentage; 2 is preparation before plating; 3 is vacuuming to reach 2×10 -3 ~ 5×10 -3 Pa; 4 is for adjusting process parameters; 5 is for vacuum evaporation; 6 is for slow cooling and removal; 7 is for finished product

[具体实施方式] [Detailed ways]

下面对本发明作进一步的说明,本发明对本专业技术领域的人来说还是比较清楚的。The present invention will be further described below, and the present invention is relatively clear to those skilled in the art.

称取质量百分比为65%Al、20%Cu和15%Fe的铝-铜-铁准晶粉末50g。Weigh 50 g of aluminum-copper-iron quasicrystal powder with mass percent of 65% Al, 20% Cu and 15% Fe.

镀前准备:将待镀试样先用砂纸磨平,然后再将此试样抛光,最后进行超声波清洗。Preparation before plating: smooth the sample to be plated with sandpaper, then polish the sample, and finally perform ultrasonic cleaning.

将上述试样放入真空镀膜机真空蒸镀室试样放置的位置中,并将称取的50g铝-铜-铁准晶粉末放入难熔金属钼作为加热的蒸发器皿中,然后密封真空蒸镀室,对真空蒸镀室抽真空达到2×10-3~5×10-3Pa后,通过调节各项工艺参数使蒸镀距离至13厘米、蒸发电流至340安培和蒸发电压至5伏,开始真空蒸镀,蒸镀20分钟后缓冷取出试样,即可获得该准晶涂层。采用该工艺制备的铝-铜-铁准晶涂层的硬度可以达到7.6GPa以上,弹性模量达到219.5Gpa。该涂层在10%硝酸溶液中的耐蚀性提高将近10倍。在400℃恒温氧化1小时,涂层的氧化增重仅为无涂层的五分之一,说明其抗氧化性能相比提高了5倍。Put the above sample into the position where the sample is placed in the vacuum evaporation chamber of the vacuum coating machine, and put the weighed 50g aluminum-copper-iron quasicrystal powder into the evaporation vessel heated by refractory metal molybdenum, and then seal the vacuum Evaporation chamber, after vacuuming the vacuum evaporation chamber to 2×10 -3 ~ 5×10 -3 Pa, adjust various process parameters to make the evaporation distance to 13 cm, the evaporation current to 340 amperes and the evaporation voltage to 5 V, start vacuum evaporation, after evaporation for 20 minutes, slowly cool and take out the sample to obtain the quasicrystalline coating. The hardness of the aluminum-copper-iron quasicrystal coating prepared by this process can reach more than 7.6GPa, and the elastic modulus can reach 219.5GPa. The corrosion resistance of the coating in 10% nitric acid solution is nearly 10 times higher. Oxidation at a constant temperature of 400 ° C for 1 hour, the oxidation weight gain of the coating is only one-fifth of that of the non-coating, indicating that its oxidation resistance is 5 times higher than that of the non-coating.

Claims (5)

1. a vacuum evaporation prepares the method for aluminium-copper-ferrum quasi-crystal coating, the preparation that it is characterized in that coating is with the evaporator boat of refractory metal molybdenum as heating, the aluminium-copper-ferrum quasi-crystal powder is directly formed coating as treating alloy plating and evaporating in a vacuum, and processing step is: (1) takes by weighing the aluminium-copper-ferrum quasi-crystal powder that mass percent is 65%Al, 20%Cu and 15%Fe; (2) prepare before the plating; (3) vacuumize and reach 2 * 10 -3~5 * 10 -3Pa; (4) vacuum evaporation; (5) slow cooling is taken out; (6) finished product.
2. a kind of vacuum evaporation as claimed in claim 1 prepares the method for aluminium-copper-ferrum quasi-crystal coating, it is characterized in that: be prepared as sample sand papering, polishing and ultrasonic cleaning before the described plating.
3. a kind of vacuum evaporation as claimed in claim 1 prepares the method for aluminium-copper-ferrum quasi-crystal coating, it is characterized in that: the technical parameter of described vacuum evaporation is that 13 centimetres, evaporation current are that 340 amperes, vaporization voltage are 5 volts for regulating the evaporation distance.
4. a kind of vacuum evaporation as claimed in claim 1 prepares the method for aluminium-copper-ferrum quasi-crystal coating, it is characterized in that: described vacuum evaporation is with the evaporator boat of refractory metal molybdenum as heating, and accurate crystalline flour end is directly formed coating as treating alloy plating and evaporating in a vacuum.
5. a kind of vacuum evaporation as claimed in claim 1 prepares the method for aluminium-copper-ferrum quasi-crystal coating, it is characterized in that: the aluminium-copper-ferrum quasi-crystal coating of this method preparation can be applicable to machinery, automobile, petrochemical industry, electric power, chemical industry, aviation field.
CNB2005101117780A 2005-12-21 2005-12-21 Method for preparing aluminum-copper-iron quasicrystal coating by vacuum evaporation Expired - Fee Related CN100392145C (en)

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TWI555855B (en) * 2015-12-18 2016-11-01 財團法人工業技術研究院 Hydrophobic alloy film and manufacturing method thereof
CN210227766U (en) * 2018-07-27 2020-04-03 佛山市顺德区美的电热电器制造有限公司 Frying pan
CN111139433A (en) * 2018-11-02 2020-05-12 佛山市顺德区美的电热电器制造有限公司 Pot, preparation method thereof and cooking utensil
CN113402171A (en) * 2021-06-10 2021-09-17 江西嘉逸陶瓷有限公司 Non-stick heat-resistant ceramic pot glaze and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1195177A (en) * 1996-12-20 1998-10-07 三菱伸铜株式会社 Zn steaming-plating film and metallized film capacitor
CN1430246A (en) * 2001-11-28 2003-07-16 东部电子株式会社 Forming method for forming film with copper diffusion preventing by alumium
WO2005051845A2 (en) * 2003-11-26 2005-06-09 Albemarle Netherlands B.V. Hydrothermal process for the preparation of quasi-crystalline boehmite
WO2005083139A1 (en) * 2004-02-16 2005-09-09 Saint Gobain Centre De Recherches Et D'etudes Europeen Metal coating for a kitchen utensil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1195177A (en) * 1996-12-20 1998-10-07 三菱伸铜株式会社 Zn steaming-plating film and metallized film capacitor
CN1430246A (en) * 2001-11-28 2003-07-16 东部电子株式会社 Forming method for forming film with copper diffusion preventing by alumium
WO2005051845A2 (en) * 2003-11-26 2005-06-09 Albemarle Netherlands B.V. Hydrothermal process for the preparation of quasi-crystalline boehmite
WO2005083139A1 (en) * 2004-02-16 2005-09-09 Saint Gobain Centre De Recherches Et D'etudes Europeen Metal coating for a kitchen utensil

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