CN102433536A - Preparation method of TIN ceramic membrane with high bonding strength on surface of low-carbon steel - Google Patents
Preparation method of TIN ceramic membrane with high bonding strength on surface of low-carbon steel Download PDFInfo
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- CN102433536A CN102433536A CN2011103978296A CN201110397829A CN102433536A CN 102433536 A CN102433536 A CN 102433536A CN 2011103978296 A CN2011103978296 A CN 2011103978296A CN 201110397829 A CN201110397829 A CN 201110397829A CN 102433536 A CN102433536 A CN 102433536A
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- 229910001209 Low-carbon steel Inorganic materials 0.000 title claims abstract description 27
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000012528 membrane Substances 0.000 title claims description 7
- 238000010894 electron beam technology Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000007733 ion plating Methods 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract 2
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 5
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 4
- 239000010962 carbon steel Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000002950 deficient Effects 0.000 claims 1
- 238000005238 degreasing Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000000428 dust Substances 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000001883 metal evaporation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
本发明属于表面处理技术领域，其特征是公开了高能束流复合方法制备TIN陶瓷膜技术。所说高能束流复合方法是指先用脉冲电子束进行表面清洗和轰击，然后利用多弧离子镀在低碳钢表面制备TIN陶瓷膜。该方法包括：打磨低碳钢表面，清除表面的油污、灰尘等杂质，对其强流脉冲电子束表面轰击处理；然后采用多弧离子镀技术在低碳钢表面制备TIN陶瓷膜。本发明能够在低碳钢表面制备出硬度高、耐磨性好，结合强度高，力学性能好的TIN陶瓷膜。The present invention belongs to the field of surface treatment technology, and is characterized in that a high-energy beam composite method is disclosed for preparing TIN ceramic film technology. The high-energy beam composite method refers to first using a pulsed electron beam to clean and bombard the surface, and then using multi-arc ion plating to prepare a TIN ceramic film on the surface of low-carbon steel. The method comprises: polishing the surface of low-carbon steel, removing impurities such as oil and dust on the surface, and bombarding the surface with a high-current pulsed electron beam; and then using multi-arc ion plating technology to prepare a TIN ceramic film on the surface of low-carbon steel. The present invention can prepare a TIN ceramic film with high hardness, good wear resistance, high bonding strength and good mechanical properties on the surface of low-carbon steel.
Description
技术领域 technical field
本发明属于表面处理技术领域，涉及到低碳钢金属表面制备TIN陶瓷膜的技术，特别涉及到低碳钢表面高结合强度TIN陶瓷膜的制备方法。 The invention belongs to the technical field of surface treatment, and relates to a technology for preparing a TIN ceramic film on a low-carbon steel metal surface, in particular to a preparation method for a high-bonding-strength TIN ceramic film on a low-carbon steel surface.
背景技术 Background technique
随着表面技术的飞速发展，新的涂层技术层出不穷。工艺的改进，结构的调整，现代检测手段的不断引入使涂层性能不断提高。以TiN为代表的硬质单层膜，由于明显改善材料表面的力学性能和摩擦性能，而广泛应用在机械、冶金、电子等领域 With the rapid development of surface technology, new coating technologies emerge in an endless stream. The improvement of the process, the adjustment of the structure, and the continuous introduction of modern detection methods have continuously improved the performance of the coating. The hard single-layer film represented by TiN is widely used in machinery, metallurgy, electronics and other fields due to the obvious improvement of the mechanical properties and friction properties of the material surface.
脉冲电子束技术起源于20世纪60年代。直到20世纪80年代，低能强流脉冲电子束才开始在材料表面改性方面获得重视和使用。该技术能够实现较高的能量沉积(0~50J/cm2)使材料表层在时间（ns~102μs）和空间（0μm~102μm）高度压缩的情况下，形成103K数量级的温度场、108~109K/s的退火速率和102~103MPa的应力场，诱发一系列非平衡态的剧烈的物理化学变化，从而提高金属材料表层的硬度、耐磨耐蚀性能，甚至疲劳性能，实现材料表面性能的强化和优化。但由于设备的原因，目前只有俄罗斯，德国，美国，日本等的个别科研单位在这方面进行了一些探索性工作。 Pulsed electron beam technology originated in the 1960s. It was not until the 1980s that low-energy high-current pulsed electron beams began to gain attention and use in surface modification of materials. This technology can achieve high energy deposition (0~50J/cm 2 ), so that the surface layer of the material can form a 10 3 K order of magnitude under the condition of highly compressed time (ns~10 2 μs) and space (0μm~10 2 μm). The temperature field, the annealing rate of 10 8 ~10 9 K/s and the stress field of 10 2 ~10 3 MPa induce a series of violent physical and chemical changes in the non-equilibrium state, thereby improving the hardness, wear resistance and corrosion resistance of the metal material surface Performance, even fatigue performance, to achieve the strengthening and optimization of material surface properties. But due to equipment reasons, only individual scientific research units in Russia, Germany, the United States, Japan, etc. have carried out some exploratory work in this area.
将脉冲电子束技术与多弧离子镀技术结合到一起，目前还没有相关的报道。 Combining pulsed electron beam technology with multi-arc ion plating technology has not been reported yet.
发明内容 Contents of the invention
本发明的目的之一是提供一种低碳钢表面高结合强度TIN陶瓷膜的制备方法。 One of the purposes of the present invention is to provide a method for preparing a TIN ceramic film with high bonding strength on the surface of low carbon steel.
采用高能电子束对离子镀处理前的表面进行高能束流进行表面清洗的方法。 The method adopts high-energy electron beam to perform high-energy beam current on the surface before ion plating treatment to clean the surface.
采用的技术方案是 The technical solution adopted is
低碳钢表面高结合强度TIN陶瓷膜的制备方法，包括下工艺步骤： The preparation method of TIN ceramic film with high bonding strength on the surface of low carbon steel comprises the following process steps:
（1）打磨碳钢部件表面，除去表面的大尺寸缺陷； (1) Grinding the surface of carbon steel parts to remove large-scale defects on the surface;
（2）将经过步骤（1）处理的低碳钢部件表面清洗，除去油污、杂质； (2) Clean the surface of the low-carbon steel parts treated in step (1) to remove oil stains and impurities;
（3）将经过步骤（2）处理的部件放到真空室中进行高能脉冲电子束处理，高能脉冲电子束处理主要是对低碳钢表面进行深度清洗； (3) Put the parts treated in step (2) into a vacuum chamber for high-energy pulsed electron beam treatment. The high-energy pulsed electron beam treatment is mainly for deep cleaning of the surface of low-carbon steel;
（4）采用多弧离子镀设备对通过步骤（3）处理的碳钢部件表面进行离子镀处理，使其表层镀上一层TIN陶瓷膜。 (4) Use multi-arc ion plating equipment to perform ion plating treatment on the surface of the carbon steel part treated in step (3), so that the surface layer is coated with a layer of TIN ceramic film.
为了进一步提高涂层的硬度、耐磨性和结合强度等综合性能，上述步骤（3）中高能脉冲电子束处理参数为：电流密度100~150A，脉冲电压12~15kV，脉冲频率2~10Hz，脉冲次数2~10次； In order to further improve the comprehensive properties of the coating such as hardness, wear resistance and bonding strength, the parameters of the high-energy pulsed electron beam treatment in the above step (3) are: current density 100~150A, pulse voltage 12~15kV, pulse frequency 2~10Hz, Pulse times 2~10 times;
为了进一步提高涂层的硬度、耐磨性和结合强度等综合性能，上述步骤（4）中多弧离子镀参数为：金属蒸发源，钛合金靶蒸发并电离；电弧电流为40~80A；负偏压-90~-120V；气体离子源加速电压10~15 kV、电流强度5~10mA；工作压强为0.2Pa；沉积时间10~60min。 In order to further improve the comprehensive properties of the coating such as hardness, wear resistance and bonding strength, the multi-arc ion plating parameters in the above step (4) are: metal evaporation source, titanium alloy target evaporation and ionization; arc current 40~80A; Bias voltage -90~-120V; gas ion source acceleration voltage 10~15 kV, current intensity 5~10mA; working pressure 0.2Pa; deposition time 10~60min.
the
上述步骤（1）中所述打磨，砂纸粒度应在600目以内； For the grinding described in the above step (1), the sandpaper particle size should be within 600 mesh;
上述步骤（2）中所述表面油污及灰尘的清除，可采用酒精、丙酮等有机溶剂，或热碱等其他溶液或方式，清洗10分钟以上。 The surface oil and dust mentioned in the above step (2) can be cleaned with organic solvents such as alcohol and acetone, or other solutions or methods such as hot alkali, and cleaned for more than 10 minutes.
具体地说：高能束流复合方法制备TIN陶瓷膜技术，其包括： Specifically: TIN ceramic membrane technology prepared by high-energy beam composite method, which includes:
（1）采用粒度600目以内砂纸打磨钛合金部件表面，除去表面的大尺寸缺陷，保证处理表面的精度； (1) Use sandpaper with a particle size of less than 600 mesh to polish the surface of titanium alloy parts to remove large-scale defects on the surface and ensure the accuracy of the treated surface;
（2）采用酒精、丙酮等有机溶剂，或热碱等其他溶液或方式，清洗经过步骤（1）处理的钛合金部件表面10分钟以上，除去油污、杂质等； (2) Use organic solvents such as alcohol, acetone, or other solutions or methods such as hot alkali to clean the surface of the titanium alloy parts treated in step (1) for more than 10 minutes to remove oil stains and impurities;
（3）采用高能脉冲电子束处理，处理参数为：电流密度100~150A，脉冲电压12~15kV，脉冲频率2~10Hz，脉冲次数2~10次，将经过步骤（2）处理的部件表面进行表面清洗处理，制备清洁、平整的低碳钢表面； (3) Using high-energy pulsed electron beam processing, the processing parameters are: current density 100~150A, pulse voltage 12~15kV, pulse frequency 2~10Hz, pulse number 2~10 times, and the surface of the component treated in step (2) is treated Surface cleaning treatment to prepare clean and smooth low carbon steel surface;
（4）采用多弧离子镀对通过步骤（3）处理的低碳钢部件表面进行离子镀处理，工艺参数为电弧电流为40~80A；负偏压-90~-120V；气体离子源加速电压10~15 kV、电流强度5~10mA；工作压强为0.2Pa；沉积时间10~60min。 (4) Use multi-arc ion plating to perform ion plating treatment on the surface of the low carbon steel parts treated in step (3), the process parameters are arc current 40~80A; negative bias voltage -90~-120V; gas ion source acceleration voltage 10~15 kV, current intensity 5~10mA; working pressure 0.2Pa; deposition time 10~60min.
本发明所具有的效果： The effect that the present invention has:
本发明方法一操作，制备的TIN陶瓷膜，既具有与金属基体的高结合强度，又具有高硬度、高耐磨性、高耐蚀性的特点。 Once the method of the present invention is operated, the prepared TIN ceramic film not only has high bonding strength with the metal substrate, but also has the characteristics of high hardness, high wear resistance and high corrosion resistance.
另外，高能脉冲电子束处理不仅起到表面清洁的作用，还起到表层金属活化的作用，这样，TIN涂层与金属基体的结合强度更高，有望解决传统TIN涂层过早剥落的问题。 In addition, high-energy pulsed electron beam treatment not only cleans the surface, but also activates the surface metal. In this way, the bonding strength between the TIN coating and the metal substrate is higher, which is expected to solve the problem of premature peeling off of the traditional TIN coating.
具体实施方式 Detailed ways
实施例1 Example 1
低碳钢表面高结合强度TIN陶瓷膜的制备方法，具体包括以下步骤： The preparation method of TIN ceramic film with high bonding strength on the surface of low carbon steel specifically comprises the following steps:
（1）采用粒度600目砂纸打磨钛合金部件表面，除去表面的大尺寸缺陷，保证处理表面的精度； (1) Use 600-mesh sandpaper to polish the surface of titanium alloy parts to remove large-scale defects on the surface and ensure the accuracy of the treated surface;
（2）采用酒精，清洗经过（1）处理的钛合金部件表面15分钟，除去油污、杂质； (2) Use alcohol to clean the surface of the titanium alloy parts treated in (1) for 15 minutes to remove oil and impurities;
（3）采用高能脉冲电子束处理，处理参数为：电流密度120A，脉冲电压13kV，脉冲频率5Hz，脉冲次数6次，将经过步骤（2）处理的部件表面进行表面清洗处理，制备清洁、平整的低碳钢表面； (3) Using high-energy pulsed electron beam treatment, the processing parameters are: current density 120A, pulse voltage 13kV, pulse frequency 5Hz, pulse number 6 times, and the surface of the component treated in step (2) is cleaned to prepare clean and smooth low carbon steel surface;
（4）采用多弧离子镀对通过步骤（3）处理的低碳钢部件表面进行离子镀处理，工艺参数为电弧电流为50A；负偏压-90V；气体离子源加速电压12 kV、电流强度8mA；工作压强为0.2Pa；沉积时间40min。 (4) Use multi-arc ion plating to perform ion plating on the surface of the low-carbon steel parts treated in step (3). The process parameters are arc current 50A; negative bias -90V; gas ion source acceleration voltage 12 kV, current intensity 8mA; working pressure 0.2Pa; deposition time 40min.
实施例2 Example 2
低碳钢表面高结合强度TIN陶瓷膜的制备方法，具体包括以下步骤： The preparation method of TIN ceramic film with high bonding strength on the surface of low carbon steel specifically comprises the following steps:
（1）采用粒度400目砂纸打磨钛合金部件表面，除去表面的大尺寸缺陷，保证处理表面的精度； (1) Grind the surface of titanium alloy parts with 400-mesh sandpaper to remove large-scale defects on the surface and ensure the accuracy of the treated surface;
（2）采用90℃热碱溶液清洗经过（1）处理的低碳钢部件表面20分钟，除去油污、杂质； (2) Use 90°C hot alkali solution to clean the surface of the low-carbon steel parts treated in (1) for 20 minutes to remove oil and impurities;
（3）采用高能脉冲电子束处理，处理参数为：电流密度150A，脉冲电压5kV，脉冲频率10Hz，脉冲次数5次，将经过步骤（2）处理的部件表面进行表面清洗处理，制备清洁、平整的低碳钢表面；； (3) Using high-energy pulsed electron beam treatment, the processing parameters are: current density 150A, pulse voltage 5kV, pulse frequency 10Hz, pulse number 5 times, and the surface of the component treated in step (2) is cleaned to prepare clean and smooth mild steel surface;
（4）采用多弧离子镀对通过步骤（3）处理的低碳钢部件表面进行离子镀处理，工艺参数为电弧电流为80A；负偏压-120V；气体离子源加速电压10kV、电流强度5mA；工作压强为0.2Pa；沉积时间60min。。 (4) Use multi-arc ion plating to perform ion plating treatment on the surface of the low carbon steel parts treated in step (3), the process parameters are arc current 80A; negative bias voltage -120V; gas ion source acceleration voltage 10kV, current intensity 5mA ; The working pressure is 0.2Pa; the deposition time is 60min. .
经过本方法制备的涂层厚度为5μm，涂层表面致密无缺陷，磨损量降低50%以上。 The thickness of the coating prepared by the method is 5 μm, the surface of the coating is dense and defect-free, and the wear amount is reduced by more than 50%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110923636A (en) * | 2019-11-29 | 2020-03-27 | 南京航空航天大学 | Electron beam composite plasma alloying treatment method for surface of gamma-TiAl alloy |
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| CN101363110A (en) * | 2008-09-24 | 2009-02-11 | 四川大学 | A physical vapor phase preparation method of C-SiC coating for hydrogen (tritium) barrier |
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| JP2006066272A (en) * | 2004-08-27 | 2006-03-09 | Canon Inc | Image display device |
| CN1847449A (en) * | 2006-05-15 | 2006-10-18 | 西安宇杰表面工程有限公司 | TiNx film preparing process on the surface of cutter for machining gear in automobile gear box |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110923636A (en) * | 2019-11-29 | 2020-03-27 | 南京航空航天大学 | Electron beam composite plasma alloying treatment method for surface of gamma-TiAl alloy |
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Application publication date: 20120502 |