CN101629319A - Method for removing diamond-like carbon film on steel surface - Google Patents
Method for removing diamond-like carbon film on steel surface Download PDFInfo
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Abstract
Description
技术领域 technical field
本发明涉及一种退除工件表面镀膜的方法，尤其涉及一种退除钢铁表面类金刚石碳膜的方法。The invention relates to a method for removing a coating film on the surface of a workpiece, in particular to a method for removing a diamond-like carbon film on a steel surface.
背景技术 Background technique
类金刚石碳膜(DLC)是一类非晶碳膜材料的统称，其碳原子的四个电子有sp2和sp3两种键合方式，结构介于晶体的金刚石和石墨之间，按照含氢的有无可细分为氢化类金刚石碳膜(a-C:H)和不含氢的四面体非晶碳膜(ta-C)。DLC碳膜具有与金刚石相类似的诸多优异性能，包括极高的硬度、电阻率、电绝缘强度，优良的耐磨性，极低的摩擦系数，在可见及近红外区具有很高的透过率，同时其在腐蚀介质中表面出极高的化学惰性等。因此，DLC膜作为一种新型功能薄膜材料，在数据存储、工模具、汽车、MEMS微机电、航空航天等领域显示出了广阔的应用前景。Diamond-like carbon film (DLC) is a general term for a class of amorphous carbon film materials. The four electrons of its carbon atoms have two bonding modes: sp 2 and sp 3. The structure is between crystal diamond and graphite. According to the content The presence or absence of hydrogen can be subdivided into hydrogenated diamond-like carbon film (aC:H) and tetrahedral amorphous carbon film without hydrogen (ta-C). DLC carbon film has many excellent properties similar to diamond, including extremely high hardness, resistivity, electrical insulation strength, excellent wear resistance, extremely low friction coefficient, and high transmittance in the visible and near-infrared regions. rate, and at the same time, it exhibits extremely high chemical inertness in corrosive media. Therefore, DLC film, as a new type of functional thin film material, has shown broad application prospects in the fields of data storage, tools and dies, automobiles, MEMS, aerospace and other fields.
目前，制备DLC碳膜的方法主要有物理气相沉积(PVD)、化学气相沉积(CVD)和液相电化学三大类，其中，PVD和CVD获取高硬度DLC碳功能膜的主要技术。然而，因主导DLC碳膜力学、摩擦学特性的亚稳态sp3碳键的形成源于高能离子对生长表面的持续轰击。而这种能量粒子的轰击，直接导致了薄膜内部的原子重组和局域致密化，使DLC碳膜中产生高残余压应力(～12GPa)。高应力的存在不仅对DLC碳膜的结构和性能产生影响，且大幅降低薄膜与基体间的结合力，易使薄膜开裂、脱落，并最终失效。通过前期预处理、过渡层、金属掺杂等方法，可在一定程度上提高DLC碳膜的膜基结合力，延长镀膜工件的使用寿命。然而，对于后续使用过程中因薄膜开裂、脱落的镀膜工件而言，如何采用合理优化的褪镀方法，将工件表面残留的DLC碳膜完全退除，并通过重新镀膜使工件再次被利用，已成为DLC碳膜工程化应用领域中亟需解决的关键技术难题之一。At present, the methods for preparing DLC carbon films mainly include physical vapor deposition (PVD), chemical vapor deposition (CVD) and liquid-phase electrochemistry. Among them, PVD and CVD are the main technologies for obtaining high-hardness DLC carbon functional films. However, the formation of metastable sp 3 carbon bonds that dominate the mechanical and tribological properties of DLC carbon films originates from the continuous bombardment of high-energy ions on the growth surface. The bombardment of this kind of energy particles directly leads to atomic recombination and local densification inside the film, resulting in high residual compressive stress (~12GPa) in the DLC carbon film. The existence of high stress not only affects the structure and performance of the DLC carbon film, but also greatly reduces the bonding force between the film and the substrate, which easily causes the film to crack, fall off, and eventually fail. Through pretreatment, transition layer, metal doping and other methods, the film-base bonding force of the DLC carbon film can be improved to a certain extent, and the service life of the coated workpiece can be extended. However, for the coated workpiece due to film cracking and falling off in the subsequent use process, how to use a reasonable and optimized stripping method to completely remove the residual DLC carbon film on the surface of the workpiece, and make the workpiece reused by re-coating has become a problem. It has become one of the key technical problems that need to be solved urgently in the field of DLC carbon film engineering application.
机械研磨退膜法精确度低，易损坏工件基体，且不适用于形状复杂的零件；等离子体轰击退除法精确度高，但时间长，成本高，不利于大规模推广使用。The mechanical grinding stripping method has low precision, is easy to damage the workpiece substrate, and is not suitable for parts with complex shapes; the plasma bombardment stripping method has high accuracy, but it takes a long time and high cost, which is not conducive to large-scale promotion and use.
发明内容 Contents of the invention
本发明所要解决的技术问题是针对钢铁工件提供一种退除表面类金刚石碳膜的方法，旨在实现不合格工件产品的重新镀膜和再利用，有效提高其使用寿命。The technical problem to be solved by the present invention is to provide a method for removing the diamond-like carbon film on the surface of iron and steel workpieces, aiming to realize re-coating and reuse of unqualified workpiece products, and effectively improve their service life.
本发明为解决上述技术问题所采取的技术方案为：一种退除钢铁表面类金刚石碳膜的方法，其特征在于步骤依次为：The technical scheme that the present invention takes for solving the above-mentioned technical problem is: a kind of method of removing the diamond-like carbon film on steel surface, it is characterized in that the steps are as follows:
(1)将钢铁工件置于真空腔室中，利用线性离子束源提供氧等离子体束流，利用偏压使离子束流攻击工件，引起工件表面类金刚石膜改性并且局部翘曲、脱落；(1) Place the iron and steel workpiece in a vacuum chamber, use a linear ion beam source to provide an oxygen plasma beam, and use a bias voltage to make the ion beam attack the workpiece, causing the diamond-like film on the surface of the workpiece to be modified and partially warped and peeled off;
(2)室温下以镀膜钢铁工件为阳极，在酸性电解液中进行电解，直至薄膜褪尽为止；(2) At room temperature, use the coated steel workpiece as the anode, and perform electrolysis in an acidic electrolyte until the film fades away;
(3)将工件取出浸泡于50g/l～150g/l浓度的氢氧化钠溶液中10～15min，中和工件表面残留的酸液；(3) Take out the workpiece and soak it in a sodium hydroxide solution with a concentration of 50g/l-150g/l for 10-15min to neutralize the residual acid on the surface of the workpiece;
(4)将工件取出，水洗烘干后，从而将钢铁工件上的类金刚石碳膜退除，所述的类金刚石碳膜包括含氢类金刚石碳膜(a-C:H)，不含氢的类金刚石碳膜(ta-C)或者金属掺杂类金刚石碳膜(Me-DLC，Me包括Ti、Cr、W等)；(4) Take out the workpiece, wash and dry it with water, thereby remove the diamond-like carbon film on the steel workpiece. The diamond-like carbon film includes hydrogen-containing diamond-like carbon film (a-C:H), and the hydrogen-free Diamond carbon film (ta-C) or metal-doped diamond-like carbon film (Me-DLC, Me includes Ti, Cr, W, etc.);
所述的酸性电解液是由磷酸、硫酸、丙三醇及去离子水按一定比例混合而成，其中磷酸的体积浓度为5％～30％，硫酸的体积浓度为0.1％～5％，丙三醇的体积浓度为0.1％～5％。The acidic electrolyte is formed by mixing phosphoric acid, sulfuric acid, glycerol and deionized water in a certain proportion, wherein the volume concentration of phosphoric acid is 5% to 30%, the volume concentration of sulfuric acid is 0.1% to 5%, and the volume concentration of propane The volume concentration of triol is 0.1%-5%.
所述的类金刚石碳膜为多层薄膜，其中过渡层包括Cr、Ti、CrN、TiN、CrC、或者TiC等。采用该方法可以将多层薄膜一同除去。The diamond-like carbon film is a multilayer film, wherein the transition layer includes Cr, Ti, CrN, TiN, CrC, or TiC. Using this method, multiple layers of film can be removed together.
所述的电解时的电流密度为3～20A/dm2。所述的电解时间为5～15min。The current density during electrolysis is 3-20A/dm 2 . The electrolysis time is 5-15 minutes.
本发明可以退除钢铁表面类金刚石碳膜，同时不对基体产生破坏性腐蚀，对工件尺寸及形状改变微小。由于类金刚石碳膜导电性差，预先采用氧等离子体轰击一方面能够使碳膜局部脱落露出金属基体或过渡层，使工件在电解退镀过程中保持良好的导电性。另一方面，氧等离子体轰击能够使类金刚石碳膜发生改性，出现疏松及微裂纹，从而使溶液更容易进入薄膜与基体的界面以及多层膜各膜层之间的界面，使工件表面残留的未脱落及磨损的薄膜也能够轻松的被除掉。电解液选择以磷酸为主要成分，一方面由于磷酸的酸性较弱，对金属的腐蚀性较小。另一方面，工件表面很多部位在使用过程中和氧等离子体轰击后碳膜已经脱落，金属基体或薄膜过渡层已经暴露出来，上述位置溶解速度远远大于碳膜覆盖处的溶解速度，这会导致工件表面碳膜已脱落部位的过腐蚀。采用磷酸能够与从阳极溶解下来的金属离子形成溶解度小、黏性大、扩散速度小的磷酸盐，构成黏滞性较大的电解液层，该黏膜在基体或过渡层暴露部位分布较厚，降低该处的电流密度，从而减缓该处的溶解速度。电解溶液中加入少量的硫酸能够提高薄膜退除的速度，同时可以适当减少磷酸用量，从而降低成本，减少磷酸对环境造成的污染。丙三醇能起到良好的缓蚀作用，磷酸虽不是强酸，但是也会对钢铁造成腐蚀，丙三醇能与之形成C3H5(OH)2PO4络合物，这种络合物的金属衍生物可以形成复杂的磷酸盐膜，防止电解液在不通电的情况下腐蚀基体。The invention can remove the diamond-like carbon film on the surface of the iron and steel without destructive corrosion on the base body and little change in the size and shape of the workpiece. Due to the poor conductivity of the diamond-like carbon film, the pre-bombardment of oxygen plasma can make the carbon film partially fall off to expose the metal matrix or transition layer, so that the workpiece can maintain good conductivity during the electrolytic deplating process. On the other hand, the oxygen plasma bombardment can modify the diamond-like carbon film, causing looseness and microcracks, so that the solution can more easily enter the interface between the film and the substrate and the interface between the layers of the multilayer film, making the surface of the workpiece Residual unflapped and worn films can also be easily removed. The electrolyte is chosen to use phosphoric acid as the main component. On the one hand, due to the weak acidity of phosphoric acid, it is less corrosive to metals. On the other hand, many parts of the surface of the workpiece have fallen off the carbon film after being bombarded with oxygen plasma during use, and the metal substrate or thin film transition layer has been exposed. Lead to over-corrosion of the part where the carbon film on the surface of the workpiece has fallen off. Phosphoric acid can form a phosphate with low solubility, high viscosity and low diffusion speed with the metal ions dissolved from the anode, forming a viscous electrolyte layer. The mucosa is thicker in the exposed parts of the matrix or transition layer. Reduce the current density at this place, thereby slowing down the dissolution rate at this place. Adding a small amount of sulfuric acid to the electrolytic solution can increase the removal speed of the film, and at the same time can properly reduce the amount of phosphoric acid, thereby reducing costs and reducing environmental pollution caused by phosphoric acid. Glycerol can play a good corrosion inhibition effect. Although phosphoric acid is not a strong acid, it can also cause corrosion to steel. Glycerol can form a C 3 H 5 (OH) 2 PO 4 complex with it. The metal derivatives of substances can form a complex phosphate film to prevent the electrolyte from corroding the substrate without electricity.
与现有技术相比，本发明的优点是：工艺简单，可操作性好，退膜效率高，成本低廉且实用性强，更适合在实际生产中应用。Compared with the prior art, the present invention has the advantages of simple process, good operability, high film-removing efficiency, low cost and strong practicability, and is more suitable for application in actual production.
附图说明 Description of drawings
图1为实施例1中工件表面的多层薄膜结构图。Fig. 1 is the multilayer thin film structure diagram on the workpiece surface in embodiment 1.
图2为实施例1中工件的退膜工艺流程图。Fig. 2 is the process flow diagram of the film removal process of the workpiece in embodiment 1.
具体实施方式 Detailed ways
以下通过具体的实施例对本发明的技术方案作进一步的描述。The technical solution of the present invention will be further described below through specific examples.
实施例1：Example 1:
待处理的工件为高速钢麻花钻，表面为多层膜结构，自下而上依次为铬/碳化铬/a-C:H(也包括类似的Ti/TiC/a-C:H，W/WC/a-C:H)，工件表面薄膜结构图如图1所示。去除其表面的多层膜包括以下步骤：The workpiece to be processed is a high-speed steel twist drill, the surface is a multi-layer film structure, and the order from bottom to top is chromium/chromium carbide/a-C:H (including similar Ti/TiC/a-C:H, W/WC/a-C: H), the film structure diagram on the surface of the workpiece is shown in Figure 1. Removing the multilayer film on its surface includes the following steps:
①将工件置于真空腔室中，利用线性离子束源提供氧等离子体束流，在一定偏压下使离子束流加速攻击工件，引起工件表面类金刚石膜改性并且局部脱落。① Place the workpiece in a vacuum chamber, use a linear ion beam source to provide an oxygen plasma beam, and accelerate the ion beam to attack the workpiece under a certain bias voltage, causing the diamond-like film on the surface of the workpiece to be modified and partially peeled off.
②采用磷酸体积浓度为5％～10％，硫酸体积浓度为1％～5％，丙三醇体积浓度为0.1％～2％的复合酸性电解液，优选，磷酸体积浓度为8％，硫酸体积浓度为3％，丙三醇体积浓度为0.7％的复合酸性电解液，以工件为阳极，室温下，在5～15A/dm2的电流密度下电解，优选10A/dm2的电流密度，根据薄膜的厚度及结合力的不同，电解时间也不同，一般为10～15min。②The volume concentration of phosphoric acid is 5%-10%, the volume concentration of sulfuric acid is 1%-5%, and the volume concentration of glycerol is 0.1%-2%. Preferably, the volume concentration of phosphoric acid is 8%, and the volume concentration of sulfuric acid is Concentration is 3%, glycerol volume concentration is 0.7% composite acidic electrolyte, with the workpiece as the anode, at room temperature, under the current density of 5 ~ 15A/dm 2 , the current density of 10A/dm 2 is preferred, according to The thickness of the film and the binding force are different, and the electrolysis time is also different, generally 10 to 15 minutes.
③薄膜褪尽后将工件取出，在50g/l～150g/l浓度的的氢氧化钠溶液中浸泡10min，质量浓度优选10％的氢氧化钠溶液。③Take out the workpiece after the film fades away, and soak it in 50g/l～150g/l sodium hydroxide solution for 10min, preferably 10% sodium hydroxide solution.
④用自来水将工件洗净烘干准备重新镀膜。实施例1的退膜工艺流程图如图2所示。④Wash and dry the workpiece with tap water to prepare for re-coating. The process flow chart of film removal in Example 1 is shown in FIG. 2 .
实施例2：Example 2:
待处理的工件为碳素钢缝纫机针杆部件，表面为多层膜结构，自下而上依次为Cr/CrC/a-C:H(也包括类似的Ti/TiC/a-C:H，W/WC/a-C:H)。去除其表面的多层膜包括以下步骤：The workpiece to be processed is a carbon steel sewing machine needle bar part, and the surface is a multilayer film structure, which is Cr/CrC/a-C:H from bottom to top (including similar Ti/TiC/a-C:H, W/WC/ a-C:H). Removing the multilayer film on its surface includes the following steps:
①将工件置于真空腔室中，利用线性离子束源提供氧等离子体束流，在一定偏压下使离子束流加速攻击工件，引起工件表面类金刚石膜改性并且局部脱落。① Place the workpiece in a vacuum chamber, use a linear ion beam source to provide an oxygen plasma beam, and accelerate the ion beam to attack the workpiece under a certain bias voltage, causing the diamond-like film on the surface of the workpiece to be modified and partially peeled off.
②采用磷酸体积浓度为7％～12％，硫酸体积浓度为0.5％～3％，丙三醇体积浓度为0.1％～3％的复合酸性电解液，优选，磷酸体积浓度为9％，硫酸体积浓度为2％，丙三醇体积浓度为1％的复合酸性电解液，以工件为阳极，室温下，在10～18A/dm2的电流密度下电解10～15min，优选15A/dm2的电流密度。②The volume concentration of phosphoric acid is 7%-12%, the volume concentration of sulfuric acid is 0.5%-3%, and the volume concentration of glycerol is 0.1%-3%. Preferably, the volume concentration of phosphoric acid is 9%, and the volume concentration of sulfuric acid is 9%. Concentration of 2%, glycerol volume concentration of 1% composite acidic electrolyte, with the workpiece as the anode, at room temperature, electrolysis at a current density of 10 to 18A/ dm2 for 10 to 15min, preferably at a current of 15A/ dm2 density.
③薄膜褪尽后将工件取出，在100g/l～150g/l浓度的氢氧化钠溶液中浸泡12min，质量浓度优选10％的氢氧化钠溶液。③Take out the workpiece after the film fades away, and soak it in 100g/l-150g/l sodium hydroxide solution for 12min, preferably 10% sodium hydroxide solution.
④用自来水将工件洗净烘干准备重新镀膜。④Wash and dry the workpiece with tap water to prepare for re-coating.
实施例3：Example 3:
待处理的工件为不锈钢手机外壳，表面镀有a-C:H单层膜。去除其表面类金刚石碳膜包括以下步骤：The workpiece to be treated is a stainless steel mobile phone case, the surface of which is coated with a-C:H single-layer film. Removing its surface diamond-like carbon film comprises the following steps:
①将工件置于真空腔室中，利用线性离子束源提供氧等离子体束流，在一定偏压下使离子束流加速攻击工件，引起工件表面类金刚石膜改性并且局部脱落。① Place the workpiece in a vacuum chamber, use a linear ion beam source to provide an oxygen plasma beam, and accelerate the ion beam to attack the workpiece under a certain bias voltage, causing the diamond-like film on the surface of the workpiece to be modified and partially peeled off.
②采用磷酸体积浓度为15～30％，硫酸体积浓度为0.1％～2％，丙三醇体积浓度为1％～5％的复合酸性电解液，优选磷酸体积浓度为20％，硫酸体积浓度为1％，丙三醇体积浓度为3％的复合酸性电解液，以工件为阳极，室温下，在10～20A/dm2的电流密度下电解5～10min，优选15A/dm2的电流密度。② Use a composite acidic electrolyte with a phosphoric acid volume concentration of 15-30%, a sulfuric acid volume concentration of 0.1%-2%, and a glycerol volume concentration of 1%-5%. The preferred phosphoric acid volume concentration is 20%, and the sulfuric acid volume concentration is 1%, a composite acidic electrolyte with a glycerol volume concentration of 3%, using the workpiece as an anode, electrolyzing at a current density of 10-20A/ dm2 for 5-10min at room temperature, preferably a current density of 15A/ dm2 .
③薄膜褪尽后将工件取出，在80g/l～150g/l浓度的氢氧化钠溶液中浸泡15min，质量浓度优选10％的氢氧化钠溶液。③Take out the workpiece after the film fades away, and soak it in 80g/l-150g/l sodium hydroxide solution for 15 minutes, preferably 10% sodium hydroxide solution.
④用自来水将工件洗净烘干准备重新镀膜。④Wash and dry the workpiece with tap water to prepare for re-coating.
综上所述，该退膜工艺简单，可操作性好，退膜效率高，与激光辐照、等离子体轰击等退膜方法相比，成本低廉且实用性强，更适合在实际生产中应用。In summary, the stripping process is simple, easy to operate, and high in stripping efficiency. Compared with laser irradiation, plasma bombardment, and other stripping methods, the cost is low and the practicability is strong, and it is more suitable for application in actual production. .
上述实施例只是本发明的具体应用举例，尽管为说明的目的公开了本发明的最佳实施例，但是本领域的技术人员可以理解：在不脱离本发明及所附的权利要求精神和范围内，各种替换、变化和修改都是可能的。因此，本发明不应局限于最佳实施例所公开的内容，凡采用等同变换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。Above-mentioned embodiment is only the concrete application example of the present invention, although the preferred embodiment of the present invention is disclosed for the purpose of illustration, but those skilled in the art can understand: within the spirit and scope of not departing from the present invention and appended claims , various substitutions, changes and modifications are possible. Therefore, the present invention should not be limited to the content disclosed in the preferred embodiment, and any technical solution formed by equivalent transformation or equivalent replacement falls within the protection scope of the present invention.
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