CN107630204A - 用于涂覆传导性部件的方法和传导性部件的涂层 - Google Patents
用于涂覆传导性部件的方法和传导性部件的涂层 Download PDFInfo
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- CN107630204A CN107630204A CN201710587992.6A CN201710587992A CN107630204A CN 107630204 A CN107630204 A CN 107630204A CN 201710587992 A CN201710587992 A CN 201710587992A CN 107630204 A CN107630204 A CN 107630204A
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- conductive member
- gas
- supporting body
- layer
- coating
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Classifications
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
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- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/021—Cleaning or etching treatments
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C28/046—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with at least one amorphous inorganic material layer, e.g. DLC, a-C:H, a-C:Me, the layer being doped or not
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/20—Carburising
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/28—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in one step
- C23C8/30—Carbo-nitriding
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
- H01J37/32853—Hygiene
- H01J37/32862—In situ cleaning of vessels and/or internal parts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/36—Gas-filled discharge tubes for cleaning surfaces while plating with ions of materials introduced into the discharge, e.g. introduced by evaporation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/32—Processing objects by plasma generation
- H01J2237/33—Processing objects by plasma generation characterised by the type of processing
- H01J2237/332—Coating
Abstract
本发明涉及用于涂覆传导性部件的方法和传导性部件的涂层。具体描述了用于在等离子体反应器中涂覆传导性部件的方法和传导性部件的涂层,其中该方法包括清洁步骤、机械承载体沉积、通过等离子体轰击的形貌改变、化学承载体层沉积和无定形碳层沉积(类金刚石碳)。在一个实施方案中,该方法是在单一周期中。本发明涉及材料工程、物理与化学的领域。
Description
技术领域
本发明描述了一种用于在等离子体反应器中涂覆传导性部件的方法和传导性部件的涂层,其中该方法包括步骤:清洁,机械承载体沉积,通过等离子体轰击的形貌(topographic)改变,化学承载体层沉积和无定形碳层沉积(类金刚石碳)。本发明涉及材料工程、物理与化学的领域。
背景技术
类金刚石碳(DLC)膜是基于碳的膜,通常是无定形的,即具有类金刚石结构,但是不具有存在于其四面体结构中的结合角,而是存在sp2和sp3结合,并且进一步存在一定量的氢。sp3和sp2键之间的比例影响特征,因此限定膜的类型。一般较高的比例表示较接近于金刚石的性能(例如较高的硬度),而较低的比例表示考虑膜较具石墨性,即具有类似于石墨的性能(图1)。
在最近几年,这些膜主要由于例如如下的性能吸引了特别的注意:提供低的摩擦系数、高的化学稳定性、高的硬度、光学透明性、高电阻率和低的电子亲合能的能力。以这种方式,它们可以在宽范围的应用中使用,其中有光电器件、具有摩擦或化学应用的涂层、汽车部件、模具涂层和生物相容的部件。
无定形碳膜的一种最令人感兴趣的性能是具有提供低摩擦系数的能力,兼具高的耐磨性,否则,该膜将迅速磨损。通过在金属-金属接触部之间使用无定形碳膜,可实现低于0.2的摩擦系数,在高真空中达到0.01的非常低水平,并将磨损率减少到10-10mm3/Nm的水平。
最常用于生产无定形或非无定形的碳膜的技术是脉冲激光沉积(PLD)、等离子体辅助(或增强)化学气相沉积(PA-CVD或PE-CVD)、离子束溅射(IBS)、离子束辅助沉积(IBAD)、等离子体浸没(或源)离子注入(PIII或PSII)。在这些技术中,离子用于沉积或将元素注入期望的基材中,该基材可以是石英、硅、钢及其合金、铝及其合金、钨及其合金,等等。注入或沉积离子的方式对结构且因此对所形成的膜的性能具有很大的影响。
前述方法的缺点是:需要用高毒性的化学溶剂或试剂来清洁或蚀刻待沉积的表面;通过与碳膜的沉积工艺分开的工艺产生机械承载体层,需要移除浴(电化学),炉(热解)或反应器(沉积)的工件,将接收碳膜的表面暴露到不同的气氛,该表面因此被改变;所述部件的几何约束;和安排过程的难度。
文献BRPI0803774A2(WO2009149526A8)公开了一种可能的热化学处理类型(氮化)的改进,通过与氮化过程一起进行清洁处理,基本上改变等离子体源在一个步骤和另一个步骤之间的切换,其消除了在沉积碳膜之前将工件的表面暴露于不同气氛的缺点,并赋予提高的生产率。
发明内容
因此,本发明涉及用在等离子体反应器中涂覆传导性部件的方法解决存在于现有技术中的问题,其中该方法包括:清洁、机械承载体沉积、通过等离子体轰击的形貌改变、化学承载体层沉积和无定形碳层沉积(类金刚石碳)。
在第一个目的,本发明提供了一种用于涂覆传导性部件的方法,其中在等离子体反应器中传导性部件与能够进行极性反转的承载体接触,该方法包括步骤:
a)在20和300℃之间的温度范围内,在0.1和10乇之间的工作压力下,采用正电势的承载体,通过电子轰击清洁该传导性部件的表面,其中等离子体气氛中的气体选自氢气、氧气、氩气、氮气或它们的组合;
b)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下,在传导性部件中沉积机械承载体,其包括选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
c)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下进行形貌改变,其包括选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
d)在200和350℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-300和-1000伏之间的电压下,以直流源脉冲时间的75至90%的等离子体源(所述直流源以50-150kHz的频率工作)的连接时间,通过气体离子轰击在传导性部件中沉积化学承载体层,其中气体选自含有与碳具有化学亲和性的元素的液体前体或气态前体;
e)在200和350℃之间的温度范围内,在1和3乇之间的工作压力和施加到传导性部件承载体的-300和-1000伏之间的电压下,在50-150kHz的频率下以75至90%的等离子体源的连接时间,通过气态烃离子轰击在化学承载体层的表面上沉积无定形碳层,其中等离子体气氛中的气体选自具有至少一种金属原子团的至少一种液体前体或这样的前体与至少一种可电离的烃气体的组合,其产生沉积在部件上的离子。
在第二个目的,本发明的特征在于通过用于涂覆传导性部件的所述方法产生的传导性部件的涂层,其中该涂层包含:
-至少第一机械承载体层,与所述传导性部件的表面直接接触;
-至少一个化学承载体层,在所述机械承载体层和无定形碳层之间;
-粘附到化学承载体层上的至少一个无定形碳层。
另外,所有要求保护的上下文共有的发明概念是用于在等离子体反应器中涂覆传导性部件的方法,其中该方法包括步骤:清洁,通过热化学处理的形貌改变,化学承载体层的沉积和无定形碳层的沉积(类金刚石碳)。
本发明的这些和其他目的容易得到本领域技术人员和公司感兴趣的部门理解,并且在以下描述中更详细地对其描述以对其再现。
附图简要说明
以下,借助于附图,对本发明进行更详细的描述:
图1示出了sp3和sp2键之间的比例和它们对于膜特征的影响的示意图,其中的a-C:H=无定形氢化的,ta-C=无氢的四面体,ta-C:H=氢化的四面体。
图2示出了烃气体对无定形碳膜的沉积速率的影响和图。
图3示出了该涂层的一个实施方案的多层系统的示意图。
图4示出了基材的表面硬度与层深度的比率的图。改编自ASM International。
具体实施方式
在本发明中,披露了一种用于在等离子体反应器中涂覆传导性部件的方法,其中该方法包括步骤:清洁、机械层沉积、形貌改变、化学承载体层沉积和无定形碳层的沉积(类金刚石碳)。该方法可以得到规模化,相对于通过等离子体的其他方法(工业生产)呈现低成本,并允许获得具有高附着力和改进的摩擦性能的膜。
作为其目标之一,本发明提供了一种使用等离子体反应器进行生产,而不需要进一步的操作的方法,并且在几何形状、自润滑部件中不经历不希望的限制,这是因为在其表面上存在碳膜,通过有效的清洁步骤,有利于随后沉积层的附着力的适宜性形貌结构,通过改变工艺参数,主要是气体类型、气流、等离子体源的连接时间、等离子体源的电压、以及承载体(所述部件位于其中)的极化反转。
本文件报告了通过在反应器(为此方法开发的)中的等离子体辅助(或增强)化学气相沉积(PE-CVD)的碳膜生产法,该生产法可以在单一周期内进行(无反应器的打开,承载体、装置或零件的交换)。该方法可基本上分为:清洁、机械承载体层沉积、形貌改变、至少一个中间层(化学承载体层)的沉积和至少一个无定形碳层的沉积。在该周期中,具有几个可以影响膜的结构和品质的参数,例如:用于清洁、形貌改变和沉积的气体类型(例如氩气、氢气、乙炔、甲烷、甲苯)、单一和总共气流、工作压力、等离子体源电压、等离子体源的连接时间、在每个步骤中花费的时间、沉积的时间,等等。
该方法的每一个可能步骤(机械承载体沉积、清洁、形貌改变、中间层沉积和碳层沉积)具有特定的参数,而且即使小的变化也可以导致具有完全不同性能的膜。例如,在中间层的沉积过程中,沉积时间或等离子体源电压的增加可导致更厚的中间层,这将直接影响沉积膜的附着性能,因为过厚的中间层在该周期内或伴随部件的机械应力可完全离开该基材。另一个重要参数是用于在膜沉积过程中产生等离子体的气体(碳前体气体)种类,其已知于文献中(参见图2)。通常在H2或Ar中稀释碳前体气体。该稀释的比例也对所形成的膜的特征和性能具有影响。
DLC膜的摩擦学性能不仅取决于膜的特征(硬度、附着力、粗糙度、残留应力),还取决于需求该膜的方式,包括环境因素和加载参数。例如,这意味着当在干燥氮气或在潮湿的空气中测试时,相同的DLC膜可表现出完全不同的性能。
受工艺参数影响且对膜的摩擦性质有直接影响的一种性能是碳膜对基材的附着力。除了上述的工艺参数,它还直接与其中将会沉积膜的基材的类型和表面性能有关。已知DLC膜一般对于硅基材比对于钢具有更好的附着力。为了使膜具有更好的附着力,有必要增加化学亲和性和降低膜与基材之间的性能例如弹性模量的不兼容性。这通常通过使用多层系统,也称为中间层进行(参见图3的示意图),其中下方层提供了机械承载体,且与膜直接接触的层提供化学附着力。
在本发明中,待涂覆的部件必须是可以通过不同的制造方法,例如冶炼、挤压、轧制、构造(conformation)、粉末冶金和机加工来生产的电导体,而不限制它的几何形状,只要它允许由等离子体产生的电离气体到达其所有表面扩展,而不产生电弧。在一个实施方案中,该部件由硅或普通钢或不锈钢或工具钢或高结合钢(highly bonded steel)或钨及其合金或铝及其合金构成,优选的组成是低碳钢,这是由于其低成本。
部件的表面精加工(finishing)影响它的形貌,这影响该方法,由此优选具有呈现具有较低数目的谷和低的峰-谷比的形貌的部件。然而,在形貌改变步骤中,在机械承载体的形成(热化学处理)步骤中或这些改变的总和中,可改变该形貌,使得它虽是重要的,但不是该方法的限制。在一个实施方案中,所述部件具有选自机加工、在粗磨(flat grinding)中调整、在无心磨中调整、在通用的外圆磨削中调整、抛光、调整且抛光等中的表面精加工。或者,甚至具有粗糙表面的部件(没有精加工过程)。
在将所述部件放置在所述承载体中后,关闭等离子体反应器,将压力降低至中度真空,通过脉冲DC源(直流)引入等离子体活化的气流和通过使用电阻式系统加热该反应器。
在一个实施方案中,将其中沉积涂层(碳膜)的部件放置在合适的承载体中,以协助均匀的膜沉积和在等离子体反应器中允许反转极性的方式设计该承载体。在一个实施方案中,该方法利用树状承载体,这允许分配大量的零件,从而增加生产率。
可以采用承载体的正极化和使用气体如氩气、氢气、氮气、氧气或它们的组合进行清洁步骤。根据部件的数量与反应器腔室的尺寸限定气流。限定工作压力,使得具有的气态物质足以清洁部件表面,但小于对电弧闭合和等离子体中断所必要的。在整个周期中,推荐使用0.1和10乇之间的压力。可以在20℃至300℃进行这样的步骤,优选在加热过程中进行,而不需要温度阈值。
由通过带负电荷的承载体的极化通过等离子体离子轰击进行部件的表面改变(形貌)。这种步骤的温度在200和650℃之间。通过等离子体可能的不同形貌改变基本取决于工作压力,等离子体源的连接时间和使用的气体的类型(离子尺寸)。增大的工作压力和/或等离子体源上的连接时间表明,对于相同的工艺时间,更大量的物质将到达部件的表面,这将导致其形貌的更积极改变,该源的更高施加电压增加每离子的能量,引起相似的效果。此外,较大的离子尺寸具有相同的效果。以这种方式,当用氩离子进行表面改变步骤时,预期比用氢离子进行这样的步骤时更大的表面改变。用于这样的改变的可能气体是:氩气,氢气,氮气和氧气。
所述参数具有彼此相互作用的效果,因此除了部件的表面精加工(预周期)、部件材料的硬度和改变部件形貌的其它后续步骤,在这样的步骤结束时的部件的表面形貌还取决于该周期的这些参数的组合,因而具有多种待产生的形貌的可能性。这些不同的形貌会导致碳膜对零件的不同附着力并影响其摩擦性能。
所述机械承载体层不必是连续和致密的。基本将这些变化概述为提高的耐磨损性、疲劳、腐蚀和基材的表面硬度的逐渐增加,以提供足够的机械承载以允许无定形碳膜的预期摩擦性能(图4)。此外,机械承载体层的形成总是暗示着一些形貌改变,其强度取决于所形成的层的类型和工艺参数。不像其他的表面处理工艺,此热化学处理不会导致整个过程中的基质相变,它也不需要通过快速冷却的转换,这意味着残余应力产生和处理的部件中的尺寸畸变的减小。这样的方法的优点是:低水平的污染物残留(相对于电化学涂覆处理),减少的工艺时间,工艺变量控制的便利,自动化的便利和改进的尺寸控制。
在一个实施方案中,连同改变所述形貌,热化学处理可以发展机械承载体层,其可以通过渗氮、渗碳、渗硼、碳氮共渗、用元素如钼的表面富集等等来获得。待用来产生这样的机械承载体的元素限制基本上是指使用的气体、靶材或前体的种类,其必须为可由等离子体电离的,使得离子可以在零件中沉积。在比所述形貌改变高的温度范围内(通常在250和650℃)进行这样的步骤,且工艺参数,即,压力、等离子体源的连接时间、气流、气体类型是可变的,且根据待产生的层类型和其中碳膜将被沉积的部件(材料)的类型而限定。
用于产生机械承载体层的可能的热化学处理为:渗碳、气态渗氮、盐浴渗氮、离子渗氮、淬火、回火等。任何形成机械承载体层的热化学工艺,无论是否离子渗氮,都引起经处理零件的表面的形貌特征的变化,例如粗糙度。在机械承载体层形成的处理(原料、调整、抛光、机加工的基材等)前,这些变化将不仅取决于所使用的工艺,也取决于基材的内在特征。
这种处理的特征是与离子相关的低能量,因而与例如通过离子束和等离子体离子的浸入和注入所辅助的沉积的工艺不同,不在部件中注入离子。在一个实施方案中,在这样的步骤中可出现离子的沉积,其随后扩散到材料中,产生具有扩散原子的区域,其可通过固溶或形成高硬度/析出的相而硬化该材料,在这种情况下不产生层,但该硬化的区域还提供了对碳膜的机械承载,这增加了其对位移(扩散层)的抵抗力。在不存在机械承载体层下,可进行碳膜的沉积,但已知承载体层提供更好的膜性能,尤其是附着力,并且在这种情况下,通常是优选的方案。
在形貌改变之后,沉积化学承载体层,这是中间层,更优选化学附着的中间层。这种步骤由机械承载层沉积的步骤的相同限制的所控制(关于使用的气体或前体的类型),然而它必须在较低的温度范围内(通常在200和350℃之间)进行,否则它可能发生该层的失效或前体的劣化(由于高温)。周期参数取决于使用的气体或前体和材料的类型(以及取决于机械承载体层的沉积步骤)。对于这样的层的形成,它通常使用DC源的脉冲时间的75和90%之间的连接源时间,该DC源在50至150kHz的频率下工作。
随后,在将化学承载体层沉积的相似温度(200-350℃)下发生碳膜的沉积。再次,沉积参数和气体取决于待获得的层类型和期望的层厚度。对于本发明的方法,允许使用碳前体气体,例如甲烷、乙炔、丁烷、环己烷、丙烷等,即,待使用的气体的限制再次依赖于其由DC等离子体源电离的可能性。已知通过设置沉积条件(源参数和等离子体反应器),使用两种不同的气体例如甲烷和乙炔导致不同厚度的层;对于本文描述的方法,乙炔具有至多是甲烷六倍的生长率。该层的形态和化学组成也得到改变,其进而改变参数,例如这些层的硬度、附着力和摩擦性能。虽然它具有较高的厚度,但相比于甲烷,通过乙炔气体产生的层是较低硬度、较低附着力和较差摩擦性能的层。然而,由于它具有高的沉积和生长速率,因此在这样的步骤中用乙炔进行的周期比用甲烷进行的周期更快。
在一个实施方案中,在单一周期中进行本文描述的方法,而不需要等离子体反应器的打开、承载体或装置的交换。每个步骤的参数的选择,以及某些任选的步骤(机械承载体沉积层)的实现与否的选择,固有地取决于待获得的膜的类型和性能例如厚度、硬度、附着力、在摩擦测试中的耐久性,应该考虑这些,但也有必要评估与每个步骤和完整周期相关的成本。在本专利中描述的方法,当以其完整形式(覆盖所有步骤)进行时,具有约8小时的持续时间。所有周期考虑反应器完全加载,合计600个具有约5cm×2cm×2cm尺寸的部件。与已知的工业方法(其中分开即以不同的周期进行各步骤,即清洁、机械承载体层沉积、化学承载体层沉积和碳层沉积)相比,该方法的总时间与用于形成具有类似于所述方法的厚度的层相似或大于8小时。
在第一个目的,本发明提供了一种用于涂覆传导性部件的方法,其中在等离子体反应器中,传导性部件与能够进行极性反转的承载体接触,该方法包括步骤:
a)在20和300℃之间的温度范围内,在0.1和10乇之间的工作压力下,采用正电势的承载体,通过电子轰击清洁该传导性部件的表面,其中等离子体气氛中的气体选自氢气、氧气、氩气、氮气或它们的组合;
b)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下,在传导性部件中沉积机械承载体,其包括选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
c)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下进行形貌改变,其包括选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
d)在200和350℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-300和-1000伏之间的电压下,以直流源脉冲时间的75至90%的等离子体源(所述直流源以50-150kHz的频率工作)的连接时间,通过气体离子轰击在传导性部件中沉积化学承载体层,其中气体选自含有与碳具有化学亲和性的元素的液体前体或气态前体;
e)在200和350℃之间的温度范围内,在1和3乇之间的工作压力和施加到传导性部件承载体的-300和-1000伏之间的电压下,以直流源脉冲时间的75至90%的等离子体源(所述直流源以50-150kHz的频率工作)的连接时间,通过气态烃离子轰击在化学承载体层的表面上沉积无定形碳层,其中等离子体气氛中的气体选自具有至少一种金属原子团的至少一种液体前体或这样的前体与至少一种可电离的烃气体的组合,其产生沉积在部件上的离子。
在一个实施方案中,步骤d)的气体是由具有至少一种金属原子团的至少一种液体前体或这样的前体与至少一种可电离的烃气体的组合的组,且其产生沉积在部件上的离子。
在一个实施方案中,在单一周期中进行用于涂覆传导性部件的方法。
在一个实施方案中,步骤b)包括:
-通过渗氮、渗碳、碳氮共渗、渗硼形成至少一个机械承载体层;或
-形成具有传导性部件的基体硬化元素的至少一个表面富集扩散层;或
-它们的组合。
在一个实施方案中,在机械承载体的形成(步骤b))之前或在机械承载体层的形成之后进行步骤c),或与化学承载体层沉积步骤(步骤d)的步骤相结合)共同进行步骤c);
在第二个目的,本发明的特征在于通过用于涂覆传导性部件的所述方法产生的传导性部件的涂层,其中该涂层包含:
-至少第一机械承载体层,与所述传导性部件的表面直接接触;
-至少一个化学承载体层,在所述机械承载体层和无定形碳层之间;
-粘附到化学承载体层的至少一个无定形碳层。
在一个实施方案中,该传导性部件的涂层包含在所述传导性部件的表面上的扩散层。
在一个实施方案中,该传导性部件的涂层包含:
-在传导性部件的表面上厚250至300μm的至少一个扩散层;
-厚10μm的至少一个机械承载体层,由与所述传导性部件的表面直接接触的氮化物构成;
-至少一个化学承载体层,在所述机械承载体层和无定形碳层之间;
-至少一个无定形碳层。
在一个实施方案中,化学承载体层由硅、碳和氢构成,并且厚1.2μm。在一个实施方案中,化学承载体层增强了无定形碳层的附着力。
在一个实施方案中,涂覆的部件是自润滑的。在一个实施方案中,自润滑的涂覆部件用于轴承系统中,例如压缩机中的轴承系统。
在一个实施方案中,提出本文描述的方法作为使所有的这些步骤(这些步骤通常分开进行)在单一周期内进行成为可能的发明,而不需要反应器的打开、承载体或设备的交换。只有采用本发明的六个主要特征的组合,这才是可能的。
第一特征涉及通过在封闭反应器中的等离子体实现所有步骤,其具有受控气氛,具有改变参数例如温度、压力、等离子体源的连接的时间、电压、气流、气体类型和承载体(零件位于其中)的极化的可能性,将所述极化从正(清洁步骤)变为负(在后面的步骤)。
第二个特征涉及承载体的适当设计以允许这种极化交换,而不影响部件或在部件的感兴趣的区域中产生等离子体边缘效应(在作为尖锐边缘的零件末端附近的不均匀性),且其在所有零件中维持等离子体稳定和均匀。此外,存在于腔室(不与所述传导性部件接触)的第二承载体的极化交换也稳定通过等离子体的工艺。
第三个特征涉及部件对环境或不希望的气氛的非暴露,暴露会导致感兴趣的部件表面的固有污染,在所述表面中沉积碳膜(或甚至机械承载体层和化学承载体层),且因此在其它步骤之间引入额外的清洁步骤。由于单一周期这种非暴露才是可能的,使得所述部件仅在该周期的开始被清洁一次,且伴随在需要时稳定和无污染地沉积的碳膜和任选的层离开反应器,所述污染可负面地影响涉及附着力和摩擦方面的性质。
第四个特征涉及通过等离子体(对于每种材料和部件的初始表面特征具有特定的参数)进行的表面改变(形貌),并允许无定形碳膜的沉积,因形貌改变而在部件的摩擦学性质方面具有重要的改进。
第五特征涉及到向等离子体反应器中引入气体(气态前体)以及液体前体的能力,所述液体前体经蒸发可以被等离子体电离,类似于以已为气体的形式引入该工艺中的元素。
第六特征涉及了解每个步骤的相对和特定的参数(气体类型、气流、气体含量、温度、压力、等离子体源的连接时间和电压),以获取每个步骤的严格控制和确保以期望的厚度和特定顺序沉积具有已知特征和组成的多层系统。
因而,该方法允许以高生产率和受控的参数生产很多系列的同等零件。
在一个实施方案中,本发明允许在单一周期内生产自润滑部件,该生产由以下几个步骤组成:有效的清洁,合适形貌的构建(其有利于随后沉积的层的附着力),机械承载体层和化学承载体层的形成和无定形碳膜的沉积。每个步骤都有特定的功能,但它们都是在等离子体反应器中随后进行的,因而使得大规模生产成为可能,并具有含自润滑碳膜的部件可再现性,这有利于其工业实施和在市场中的广泛的应用。
在一个实施方案中,本发明提供了用于获得这些部件的方法而不需要额外的操作,该方法在单一周期中在相同的设备进行。以这种方式,在清洁过程的开始之前,等离子体反应器的装载只发生一次,且在该周期的结束时,部件包含自润滑碳膜。进行的试验表明本发明的方法比组合以下三个过程的常规方法表现出更低的成本:清洁、机械承载体层沉积和化学附着和DLC沉积(通过等离子体)。另外,在单一周期中产生的部件呈现比前面提到的那些优异的摩擦性能和附着力。该方法允许以高生产率和受控参数的生产很多系列同等零件。
在本文中,术语“等离子体反应器”应理解为能够产生等离子体气氛的任何装置。
在本文中可理解,用于该导体的合适承载体是不产生不希望的边缘效应且允许极性反转的承载体。
实施例-实施方案
机械承载体的沉积的实施例
为了产生由约10微米厚的氮化物和其紧下方在普通SAE 1020钢上具有250-300μm厚度的扩散层构成的层,使用以下参数:400V的脉冲负电压,在50kHz的频率下75%的等离子体源的连接时间,2乇的压力,550℃的温度,气体混合物由氮气(90%)、氢气(9%)和甲烷(1%)组成,1000sccm的气流和90分钟的沉积保持时间。
化学承载体沉积的实施例
为了产生化学承载体层,所选择的液体前体是六甲基二硅氧烷。通过位于等离子体反应器外的六甲基二硅氧烷储存器和六甲基二硅氧烷蒸发的反应器腔室之间的压力差,将其引入腔室并由等离子体电离。在这种情况下,发生含有硅、氢和碳的化学附着层的沉积。为了在非抛光的、调整的SAE 1020钢部件(该部件经受了轻度形貌改变且具有机械承载体层)上沉积厚度约为1.2μm的化学附着层,使用以下参数:电压500V(负),在50kHz频率下75%的等离子体源的连接时间,1乇的压力,250℃的温度,氢气(30%),氩气(30%),甲烷(38%)和六甲基二硅氧烷(2%),1000sccm的气体流量,和35分钟的沉积时间。
Claims (8)
1.用于涂覆传导性部件的方法,其特征在于在等离子体反应器中,传导性部件与能够进行极性反转的承载体接触,该方法包括步骤:
a)在20和300℃之间的温度范围内,在0.1和10乇之间的工作压力下,采用正电势的承载体,通过电子轰击清洁该传导性部件的表面,其中等离子体气氛中的气体选自氢气、氧气、氩气、氮气或它们的组合;
b)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下,在传导性部件中沉积机械承载体,其包括选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
c)在200和650℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-200和-1000V之间的电压下进行形貌改变,其包含选自以下组中的两种以上气体的组合的气体离子轰击:氢气、氧气、氩气、氮气、甲烷、乙炔、或其它可电离的烃气体;
d)在200和350℃之间的温度范围内,在0.1和10乇之间的工作压力和施加到导体部件承载体的-300和-1000伏之间的电压下,以直流源脉冲时间的75至90%的等离子体源的连接时间,通过气体离子轰击在传导性部件中沉积化学承载体层,其中气体选自含有与碳具有化学亲和性的元素的液体前体或气态前体,所述直流源以50-150kHz的频率工作;
e)在200和350℃之间的温度范围内,在1和3乇之间的工作压力和施加到传导性部件承载体的-300和-1000伏之间的电压下,以直流源脉冲时间的75至90%的等离子体源的连接时间,通过气态烃离子轰击在化学承载体层的表面上沉积无定形碳层,其中等离子体气氛中的气体选自具有至少一种金属原子团的至少一种液体前体或这样的前体与至少一种可电离的烃气体的组合,且其产生沉积在部件上的离子,所述直流源以50-150kHz的频率工作。
2.根据权利要求要求1的用于涂覆传导性部件的方法,其特征在于步骤d)的气体是由具有至少一种金属原子团的至少一种液体前体或该前体与至少一种可电离的烃气体的组合构成的组,且其产生沉积在部件中的离子。
3.根据权利要求1或2的用于涂覆传导性部件的方法,其特征在于在单一周期中发生涂覆过程。
4.根据权利要求1至3的任一项的用于涂覆传导性部件的方法,其特征在于步骤b)包括:
-通过渗氮、渗碳、碳氮共渗、渗硼形成至少一个机械承载体层;或
-用传导性部件的基体硬化元素形成至少一个表面富集扩散层;或
-它们的组合。
5.传导性部件的涂层,其特征在于它是通过如权利要求4中所限定的用于涂覆传导性部件的方法产生的,其中该涂层包括:
-至少一个第一机械承载体层,与所述传导性部件的表面直接接触;
-至少一个化学承载体层,在所述机械承载体层和无定形碳层之间;
-粘附到化学层承载体的至少一个无定形碳层。
6.根据权利要求5的传导性部件的涂层,其特征在于它包含在传导性部件的表面上的扩散层。
7.根据权利要求6的传导性部件的涂层,其特征在于它包含:
-在传导性部件的表面上厚250至300μm的至少一个扩散层;
-与所述传导性部件的表面直接接触的厚10μm的至少一个机械承载体层,其由氮化物构成;
-在所述机械承载体层和无定形碳层之间的至少一个化学承载体层;
-至少一个无定形碳层。
8.根据权利要求中5-7任一项的传导性部件的涂层,其特征在于化学承载体层由硅、碳和氢组成,且具有1.2μm的厚度。
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US20130059093A1 (en) * | 2010-05-31 | 2013-03-07 | Jtekt Corporation | Method of producing coated member |
CN103469205A (zh) * | 2013-08-01 | 2013-12-25 | 合肥永信等离子技术有限公司 | 一种荷叶类金刚石膜的镀膜工艺 |
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