CN108977766B - 一种多层复合类金刚石薄膜材料及其制备方法 - Google Patents
一种多层复合类金刚石薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种多层复合类金刚石薄膜材料及其制备方法。该多层复合类金刚石薄膜通过掺杂Ti含氢非晶碳和无掺杂含氢非晶碳周期性按比例交替沉积获得。本发明制备的Ti‑DLC/α‑C:H薄膜具有高结合强度、高韧性、优良的减摩耐磨性,涂覆于切削刀具加工玻璃纤维增强复合材料可使得刀具寿命提高2倍,且相对传统单层类金刚石涂层刀具寿命可提高48%。本发明制备工艺先进、生产效率高、成本低,易于工业化生产,具有推广价值。
Description
技术领域
本发明涉及类金刚石薄膜材料领域,尤其涉及多层复合类金刚石薄膜材料及其制备方法。
背景技术
类金刚石(Diamond-like Carbon,DLC)薄膜主要是由金刚石结构的sp3杂化碳原子以及石墨结构的sp2杂化碳原子构成的非晶或纳米晶—非晶复合体,拥有众多与金刚石薄膜相似的优异性能如高硬度、低摩擦系数、耐磨损、化学性能稳定等,拥有巨大的应用前景。但是由于其本身存在膜基结合强度不足、韧性差以及摩擦学性能不稳定等问题,严重制约了薄膜优异性能的发挥。因此,如何改变薄膜设计理念,开发新型DLC薄膜,进而改善并提高DLC薄膜的综合性能,对实现DLC薄膜在世界范围内的大规模应用具有重大的现实和社会价值。
研究发现通过在非晶碳基网络中掺入异质元素可以有效改善DLC薄膜的综合性能。Zou等人(Zou C W,Wang H J,Feng L,et al.Effects of Cr concentrations on themicrostructure,hardness,and temperature-dependent tribological properties ofCr-DLC coatings,J.Applied Surface Science,2013,286:137-141)利用中频磁控溅射结合离子束沉积技术制备了Cr掺杂DLC薄膜,与未掺杂DLC相比,内应力从0.98GPa降低至0.49GPa,但薄膜硬度却从23GPa左右削减至12GPa;Pauleau等人(Pauleau Y,Thiery F,Barna P B,et al.Nanostructured copper/hydrogenated amorphous carbon compositefilms prepared by microwave plasma-assisted deposition process fromacetylene-argon gas mixtures,J.Reviews on Advanced Materials Science,2004,6(2):140-149)采用等离子体辅助磁控溅射法制备Cu掺杂DLC薄膜,发现复合薄膜中界面强化效应及金属纳米颗粒良好的延展性的协同作用可以提高DLC薄膜韧性,但薄膜耐磨性能下降,黏着磨损将加剧。由此可以发现,引入DLC碳基网络的元素往往一方面在降低DLC薄膜内应力、改善薄膜高脆性的同时,对薄膜的机械强度或耐磨性能有一定程度削弱。
多层构筑DLC薄膜是一种新型DLC制备方法,研究表明这种构筑体系可以使DLC薄膜获得更加优异的力学和摩擦学性能。目前最常见的体系有金属/金属碳化物或金属氮化物/DLC、软/硬DLC多层体系。Liu等人(Hongxi L,Yehua J,Rong Z,et al.Wear behaviourand rolling contact fatigue life of Ti/TiN/DLC multilayer films fabricated onbearing steel by PIIID,J.Vacuum,2012,86(7):848-853)采用等离子体注入法在GCr15轴承钢基体表面制备了Ti/TiN/DLC多层复合薄膜,结果发现DLC与金属基体之间结合强度得到了显著提高,且与GCr15对磨后耐磨性有了明显提高;Zhang等人(Zhang Y,Zhai Y,LiF,et al.Effect of microstructure and mechanical properties difference betweensub-layers on the performance of alternate hard and soft diamond-like carbonmultilayer films,J.Surface and Coatings Technology,2013,232:575-581)通过改变DLC沉积过程中基体偏压大小实现软/硬层DLC的控制,并以软/硬层DLC交替制备形成多层交替复合结构,发现薄膜韧性相较单层DLC薄膜提高了2倍,并且在干摩擦和水润滑情况下表现出更为优秀的耐磨性能。但是考虑到尽管同质外延相对异质外延更利于薄膜均匀生长,但制备方法不变,仅通过改变单一工艺参数来实现同种薄膜软硬层的交替制备,同时又要保证软硬层各自的优异性能,难度较大,不易实现。因此多层复合DLC薄膜制备工艺有待进一步研究和探索。
中频反应磁控溅射是近年来发展起来的一种新型溅射技术,具有靶材利用率高、运行稳定等优点。不仅可以有效增加薄膜沉积速率,而且可减轻或避免靶中毒现象,在靶的寿命期内,可实现长期稳定的运行。而阳极层线性离子源技术具有不受空间电荷限制、离子束发射角大、离子束流密度高等特点。本发明即综合两种技术的优势,分别以中频反应磁控溅射制备Ti-DLC,阳极层线性离子源制备α-C:H,两种不同薄膜周期性交替沉积来获得综合性能极佳的新型DLC多层复合薄膜。目前尚未有相关的技术报道。
发明内容
本发明的目的在于改善传统DLC薄膜存在的膜基结合强度不足、韧性差以及摩擦学性能不稳定等问题,提供一种多层复合类金刚石薄膜材料及其制备方法。
多层复合类金刚石薄膜为以金属层Ti为过渡缓冲层,多层结构为交替的Ti-DLC和α-C:H;多层结构调制层数为4~12层。
本发明的以中频反应磁控溅射制备Ti-DLC和阳极层线性离子源制备α-C:H为基础前提,通过调节两种单层薄膜调制周期和调制比,制备出具有高结合强度、高韧性、优良的减摩耐磨性的DLC多层复合薄膜。
上述多层复合DLC薄膜制备方法是:
步骤1,镀膜前将硬质合金基体打磨抛光,经过石油醚、无水乙醇、丙酮和去离子水超声波清洗并晾干;
步骤2,将基体固定于腔体内试样架,对腔体抽真空并加热;
步骤3,真空室内通入150ml/min的氩气,打开阳极层线性离子源电源对样品进行离子束预清洗;
步骤4,打开直流磁控溅射电源,开始缓冲层/过渡层金属Ti的沉积;
步骤5,分别打开中频反应磁控溅射电源和阳极层线性离子源电源进行Ti-DLC和α-C:H薄膜的沉积,控制调制周期和调制比获得最终多层复合Ti-DLC/α-C:H薄膜。
进一步的,步骤(1)中,硬质合金经过金相砂纸打磨抛光,表面粗糙度Ra约为0.1μm,随后经过石油醚、无水乙醇、丙酮和去离子水超声波清洗,各步骤清洗时间均为15min,随置于大气中烘干。
进一步的,步骤(2)中,对真空室进行抽真空至本底真空度5×10-3Pa。随后对真空室进行100℃加热,并保持30min,对真空室继续抽真空,直至重新回到本底真空度5×10- 3Pa。
进一步的,步骤(3)中,腔体真空度为2Pa,阳极层线性离子源电源电压设置为1000V,占空比60%,同时对基体施加-1200V,占空比60%的脉冲负偏压,离子束清洗时间为30min。
进一步的,步骤(4)中,通入150ml/min的氩气,并设置真空度为1.5Pa。直流磁控溅射电源恒流电流6A,脉冲负偏压为-500V,占空比30%,过渡层Ti制备时间6min,厚度约为0.1μm。
进一步的,步骤(5)中,腔体真空度为1.5Pa,Ti-DLC薄膜制备工艺为中频反应磁控溅射电源恒流5A,占空比80%,脉冲负偏压为-700V,占空比70%,初始温度为100℃,沉积时间9~24min;α-C:H薄膜制备工艺为真空度0.3Pa,阳极层线性离子源电压-1000V,占空比60%,脉冲负偏压为-1400V,占空比60%,初始温度为50℃,沉积时间为11~32min。Ti-DLC/α-C:H薄膜的调制周期控制在183~550nm,调制比控制在3/1~1/3范围内。
本发明与现有技术相比,具有以下显著优点:
(1)本发明分别采用中频反应磁控溅射技术和阳极层线性离子源技术制备多层薄膜,首先可有效避免因为单一元素掺杂,造成的薄膜性能顾此失彼现象;此外,分别采用不同的工艺可更方便获得性能条件良好的单层薄膜。
(2)本发明获得的Ti-DLC/α-C:H复合薄膜,与传统单层DLC薄膜相比,结合强度、韧性、耐磨性能均有显著提高,并在应用于涂层刀具切削加工玻璃纤维复合材料试验中,有效提高刀具寿命,相对于单层DLC涂层刀具寿命提高30%~43%,极具推广价值。
附图说明
图1为实施例2制备的多层复合DLC薄膜(Ti-DLC/α-C:H)截面SEM形貌。
图2为实施例2制备的多层复合DLC薄膜涂层刀具外观形貌。
具体实施方式
下面结合附图技术实施例多本发明做进一步说明
本发明为一种多层复合DLC薄膜制备方法。
本发明利用中频反应磁控溅射以及阳极层线性离子源技术,交替沉积单层DLC薄膜,最终获得力学性能良好的多层复合DLC薄膜。
实施例1
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜24min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜30min。如此重复2次,制得调制周期550nm,调制比1:1,调制层数4层的Ti-DLC/α-C:H薄膜。
实施例2
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜17min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜21min。如此重复3次,制得调制周期366nm,调制比1:1,调制层数6层的Ti-DLC/α-C:H薄膜。
实施例3
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜13min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜17min。如此重复4次,制得调制周期275nm,调制比1:1,调制层数8层的Ti-DLC/α-C:H薄膜。
实施例4
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜10min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜14min。如此重复5次,制得调制周期220nm,调制比1:1,调制层数10层的Ti-DLC/α-C:H薄膜。
实施例5
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜9min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜11min。如此重复6次,制得调制周期183nm,调制比1:1,调制层数12层的Ti-DLC/α-C:H薄膜。
实施例6
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜23.5min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜11min。如此重复3次,制得调制周期366nm,调制比3:1,调制层数6层的Ti-DLC/α-C:H薄膜。
实施例7
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜21.5min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜15min。如此重复3次,制得调制周期366nm,调制比2:1,调制层数6层的Ti-DLC/α-C:H薄膜。
实施例8
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜12min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜28.5min。如此重复3次,制得调制周期366nm,调制比1:2,调制层数6层的Ti-DLC/α-C:H薄膜。
实施例9
以YG8硬质合金为基体,经由预清洗后放置真空室内,抽真空后100℃加热30min,再次抽真空至本底真空度5×10-5Pa。打开离子源电压和脉冲负偏压进行30min离子束溅射清洗。通入150ml/min氩气,真空度恒定保持1.5Pa,直流磁控溅射恒流6A,脉冲负偏压-500V,占空比30%,沉积6min钛过渡层。打开中频磁控溅射电源恒流5A,占空比80%,脉冲负偏压-700V,占空比70%,沉积Ti-DLC薄膜9min;打开阳极层线性离子源恒压1000V,占空比60%,真空度0.3Pa,脉冲负偏压-1400V,占空比60%,沉积α-C:H薄膜32min。如此重复3次,制得调制周期366nm,调制比1:3,调制层数6层的Ti-DLC/α-C:H薄膜。
实施例10
将实例2多层复合DLC薄膜与传统单层DLC薄膜统一涂覆于YG8型硬质合金车刀表面,刀具前角γo=20°,后角αo=0°,主偏角κr=45°,刃倾角λs=0°。φ80mm的玻璃纤维增强复合材料作为涂层刀具车削加工对象,其纤维为无碱类E型玻璃纤维,基体为热固性环氧树脂。选择的切削条件分别为:切削深度ap=0.6mm,进给量f=0.1mm/r,切削速度250m/min。切削方式为干式无冷却连续切削。以后刀面磨损量VB=0.3mm作为磨钝标准,对比无涂层刀具、传统单层DLC薄膜涂层刀具以及本次发明的多层复合DLC薄膜涂层刀具加工寿命及加工表面质量。
表1实施例1~9参数
表2实施例10~16参数
Claims (3)
1.一种多层复合类金刚石薄膜材料,其特征在于,该多层复合DLC薄膜为以金属层Ti为过渡缓冲层,多层结构为交替的Ti-DLC和α-C:H;多层结构调制层数为4~12层,该多层复合类金刚石薄膜材料通过如下方法制得,包括如下步骤:
(1)将镀膜机腔体在真空度5×10-3Pa下进行100℃加热预激活,时间为30min;
(2)以氩气和乙炔作为工作气体,通过中频磁控溅射沉积Ti-DLC薄膜,中频恒流5A,占空比80%,频率80KHz;脉冲负偏压-700V,占空比70%;
(3)以乙炔作为工作气体,通过阳极层线性离子源沉积α-C:H薄膜,离子源恒压1000V,占空比60%;脉冲负偏压-1400V,占空比60%;
(4)Ti-DLC薄膜和α-C:H薄膜交替形成的多层结构,按调制周期183~550nm,调制比3/1~1/3获得多层复合DLC薄膜。
2.如权利要求1所述的多层复合类金刚石薄膜材料,其特征在于,步骤(2)中,氩气和乙炔的进气量分别为80~120mL /min和20mL /min,薄膜生长时间为9~24min。
3.如权利要求2所述的多层复合类金刚石薄膜材料,其特征在于,步骤(3)中,乙炔进气流量为15~30mL /min,薄膜生长时间为11~32min。
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