CN108193173B - 一种低粘附轮胎模具的多层复合涂层及其制备方法 - Google Patents

一种低粘附轮胎模具的多层复合涂层及其制备方法 Download PDF

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CN108193173B
CN108193173B CN201711479913.6A CN201711479913A CN108193173B CN 108193173 B CN108193173 B CN 108193173B CN 201711479913 A CN201711479913 A CN 201711479913A CN 108193173 B CN108193173 B CN 108193173B
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张�林
张世宏
蔡飞
温永红
杨英
林玥
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Hefei Armored Film New Material Technology Co.,Ltd.
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Abstract

本发明公开了一种低粘附轮胎模具的多层复合涂层及其制备方法,由模具基体到表面依次包括Cr粘结层、Cr/CrN纳米多层结构的过渡层和CrNiN工作层,所述Cr粘结层涂覆在模具基体上,所述CrNiN工作层中,按照原子数百分比计,包括Cr30~45%,Ni15~25%,N35~50%。用电弧离子镀技术在轮胎的模具基体表面依次沉积得到Cr粘结层、Cr/CrN纳米多层结构的过渡层和CrNiN工作层,各层界面相互匹配,涂层具有较好的结合力和韧性,增强了整个轮胎模具的耐磨性能、耐腐蚀性能和抗粘附性能,提高了其使用寿命。轮胎模具的涂层采用绿色环保方法制造,且增强了脱模能力,解决了轮胎模具容易粘胶和污染问题,模具表面水接触角达到110°以上。

Description

一种低粘附轮胎模具的多层复合涂层及其制备方法
技术领域
本发明涉及一种轮胎模具的处理工艺,尤其涉及的是一种低粘附轮胎模具的多层复合涂层及其制备方法。
背景技术
随着轮胎产品向着高速、高精度、更环保、更节能的方向发展,对轮胎模具的质量和技术水平提出了更高的要求。然而,轮胎模具长期在化学腐蚀环境以及热、压力、摩擦作用下工作,使用过程中不可避免的受到橡胶、配合剂以及脱模剂的综合沉积污染,出现粘胶、积碳、腐蚀、磨损等问题,造成轮胎脱模困难和轮胎质量下降。随着纤维增强工程塑料和玻璃纤维的大量采用,轮胎模具需要具有良好的耐磨损、防粘、易脱膜、自清洁、耐腐蚀等完整的表面工作性能。粘附性直接受固体表面能的影响,通常将水接触角所代表的疏水性作为衡量粘附效果的标准。低表面能表面在粘附界面形成弱的分子键作用力,增加了粘附界面的孔隙率,降低了粘附强度,有利于改善疏水性和抗粘附性。良好的疏水性是模具实现脱模、防粘、自清洁等功能的前提,模具表面的低表面能疏水化成为减小粘附现象的有效途径。
传统的模具表面处理方法如采用单纯的脱模剂,使用周期短,需要对模具频繁清洗、重复喷涂,占用大量的生产时间,而且脱模剂也是轮胎模具污染的重要原因之一。同样,采用电镀的方法虽然在一定程度上提升模具的性能和使用寿命,但电镀技术所带来的环境污染问题一直备受各界人士的关注。因此,急需设计一种具有低粘附、高硬度和高耐磨等特性的模具及其涂层材料,以用于生产具备各种高性能要求的轮胎。
物理气相沉积(PVD)是一种应用广泛,对环境无污染的绿色环保的表面处理方法,其在模具表面沉积的涂层具有高硬度,高耐磨性等特性,并且能够沉积高强韧抗粘附复合涂层,提高轮胎模具的综合性能,这必然是成为这一领域必须深入研究的内容之一。
发明内容
本发明的目的在于克服现有技术的不足,提供了一种低粘附轮胎模具的多层复合涂层及其制备方法,实现轮胎模具的低粘附、高硬度和高耐磨性。
本发明是通过以下技术方案实现的,本发明的一种低粘附轮胎模具的多层复合涂层,由模具基体到表面依次包括Cr粘结层、Cr/CrN纳米多层结构的过渡层和CrNiN工作层,所述Cr粘结层涂覆在模具基体上,所述CrNiN工作层中,按照原子数百分比计,包括Cr30~45%,Ni15~25%,N35~50%。
作为本发明的优选方式之一,所述模具基体为模具钢或铝合金模具。用于硫化成型各类轮胎的模具。
所述Cr粘结层的厚度为0.1~0.5μm。纯Cr粘结层具有很强的界面融合性能,能较好的连结模具基体和Cr/CrN纳米多层结构的过渡层,实现纳米多层结构的过渡层与模具基体很高的结合强度。
所述Cr/CrN纳米多层结构的过渡层为至少交替沉积10次的Cr层和CrN层,过渡层的总厚度为2~5μm,每个Cr层的厚度为70~110nm,每个CrN层的厚度为80~125nm。纳米结构的Cr/CrN纳米多层结构的过渡层能够提高结合力,纳米多层中间层使整个涂层的成分、结构和性能平缓过渡,缓解涂层应力,同时引入多层界面结构,减少PVD涂层针孔缺陷,提高涂层致密性。
所述CrNiN工作层的厚度为1~2μm。具有低表面能,减小与高温橡塑的润湿性,提高涂层抗粘附性。
一种低粘附轮胎模具的多层复合涂层的制备方法,包括以下步骤:
(1)将轮胎的模具基体经过研磨抛光清洗并烘干后放入基片转架上,对基体表面进行辉光放电清洗;
(2)粘结层沉积:通入Ar气,打开金属Cr靶,设置基体偏压、靶材电流及沉积温度,沉积纯Cr粘结层;
(3)纳米多层结构的过渡层沉积:打开金属Cr靶,通入Ar气和N2气,控制N2气流量,交替沉积Cr层和CrN层;
(4)工作层沉积:通入N2气,开启Cr靶和CrNi合金靶,在过渡层上沉积CrNiN工作层。
所述步骤(1)中,模具基体研磨抛光后表面粗糙度Ra≤0.1μm,辉光放电清洗的条件为:当真空室的本底真空度为5×10-4Pa时,通入Ar气,保持气压为1.0~4.0Pa,基片温度为300~500℃,模具基体偏压为-800~-1000V,轰击时间为5~30min。
所述步骤(2)中,辉光放电清洗后,工作气体压力调节为0.3~0.8Pa,打开金属Cr靶,靶材电流为60~80A,转架速度控制在2~4rpm,模具基体偏压保持在-100V~-200V,温度加热到450℃,沉积时间为10~60min,获得Cr粘结层。
所述步骤(3)中,Cr粘结层沉积结束后,保持模具基体温度、工作气压、Cr靶电流不变,基体偏压为-80V~-100V,沉积Cr层,沉积时间为5~10min,完成单个Cr层的沉积,然后通入N2气,N2气流量为400~600sccm,沉积CrN层,沉积时间为6~12min,完成单个CrN层的沉积,通过控制N2气质量流量计开关,重复上述工艺,交替沉积Cr层和CrN层。
所述步骤(4)中,开启CrNi合金靶开关,调节CrNi合金靶电流为60~85A,基体偏压为-80V~-120V,N2气流量为400~600sccm,沉积温度和工作压力与过渡层的相同,沉积时间为90~150min,获得CrNiN工作层。
物理气相沉积Cr基涂层表现优良的抗粘附性,尤其是添加合金元素Ni,会进一步降低Cr基涂层的表面能。通过设计粘结层/纳米多层结构的过渡层/低表面能工作层的复合结构,在保持力学性能的基础上,显著提高Cr基涂层的韧性、抗粘附和腐蚀防护能力。粘结层用来改善涂层与基体的结合;纳米多层结构的过渡层使整个涂层的成分、结构和性能平缓过渡,缓解涂层应力,同时引入多层界面结构,减少PVD涂层针孔缺陷,提高涂层致密性;最顶层是具有极低表面能的工作层,不仅提高涂层的耐蚀性,而且减小与高温橡塑的润湿性,提高涂层抗粘附性。
本发明相比现有技术具有以下优点:本发明用电弧离子镀技术在轮胎的模具基体表面依次沉积得到Cr粘结层、Cr/CrN纳米多层结构的过渡层和CrNiN工作层,各层界面相互匹配,涂层具有较好的结合力和韧性,增强了整个轮胎模具的耐磨性能、耐腐蚀性能和抗粘附性能,提高了其使用寿命。轮胎模具的涂层采用绿色环保方法制造,且增强了脱模能力,解决了轮胎模具容易粘胶和污染问题,模具表面水接触角达到110°以上。
附图说明
图1是本发明的多层复合涂层的结构示意图;
图2是实施例1的轮胎模具截面照片;
图3是实施例1的轮胎模具表面水接触角照片。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
本实施例的复合涂层制作方法如下:
将模具钢制作的轮胎模具基体研磨抛光至粗糙度Ra=50nm,先用丙酮和酒精超声波清洗15分钟,然后烘干并放置电弧离子镀炉腔的基片架上,在阴极弧源位置上一部分安装单质Cr靶,一部分安装CrNi(Ni=30at.%)合金靶,关闭真空室腔门。
依次打开机械泵、罗茨泵和分子泵将真空室的真空抽到5×10-4Pa,通入氩气到2.0Pa,基片温度加热到450℃,施加-1000V的负偏压引发辉光放电,进行溅射清洗20分钟。
辉光清洗结束后,调节氩气流量,控制真空室气压在0.6Pa,转架速度控制在3rpm,基体偏压设置为-150V,打开金属Cr靶,靶材弧电流为65A,沉积Cr粘结层,沉积时间为40分钟。
Cr粘结层沉积结束后,基片偏压调整为-100V,沉积Cr层,沉积时间为7分钟。
然后通入氮气,氮气流量为500sccm,保持工作气压、基片偏压和靶材电流不变,沉积CrN层,沉积时间为8分钟,通过控制氮气质量流量计开关,交替沉积Cr/CrN涂层,总沉积时间为180分钟。
Cr/CrN过渡层沉积结束后,在不关闭Cr靶的条件下,开启CrNi合金靶,设置合金靶弧电流为80A,持续沉积CrNiN低表面能工作层90分钟。到时候依次停弧、停偏压、停气,维持真空随炉冷却60分钟后,开启真空室取出轮胎模具。低表面能的CrNiN工作层包含40at.%Cr、22at.%Ni和38at.%N。
在轮胎模具钢基体表面合成总厚度为3μm的Cr基多层复合涂层,如图1和图2所示,由模具基体1到表面依次包括Cr粘结层2、Cr/CrN纳米多层结构的过渡层3和CrNiN工作层4,所述Cr粘结层2涂覆在模具基体1上。
涂覆上多层复合涂层的轮胎模具的表面硬度≥1600HV,水接触角≥110°,如图3所示,膜基结合力达到HF1级。
实施例2
本实施例的复合涂层制作方法如下:
将铝合金轮胎模具基体1研磨抛光至粗糙度Ra=70nm,先用丙酮和酒精超声波清洗15分钟,然后烘干并放置电弧离子镀炉腔的基片架上,在阴极弧源位置上一部分安装单质Cr靶,一部分安装CrNi(Ni=20at.%)合金靶,关闭真空室腔门。
依次打开机械泵、罗茨泵和分子泵将真空室的真空抽到5×10-4Pa,通入氩气到2.0Pa,基片温度加热到450℃,施加-1000V的负偏压引发辉光放电,进行溅射清洗20分钟。
辉光清洗结束后,调节氩气流量,控制真空室气压在0.6Pa,转架速度控制在3rpm,基体偏压设置为-150V,打开金属Cr靶,靶材弧电流为65A,沉积Cr粘结层,沉积时间为40分钟。
Cr粘结层沉积结束后,基片偏压调整为-100V,沉积Cr层,沉积时间为10分钟。
然后通入氮气,氮气流量为500sccm,保持工作气压、基片偏压和靶材电流不变,沉积CrN层,沉积时间为12分钟,通过控制氮气质量流量计开关,交替沉积Cr/CrN涂层,总沉积时间为240分钟。
Cr/CrN过渡层沉积结束后,在不关闭Cr靶的条件下,开启CrNi合金靶,设置合金靶弧电流为100A,持续沉积CrNiN工作层150分钟。到时候依次停弧、停偏压、停气,维持真空随炉冷却60分钟后,开启真空室取出轮胎模具。低表面能的CrNiN工作层包含45at.%Cr、15at.%Ni和40at.%N。
在轮胎模具钢基体表面合成总厚度为4μm的Cr基多层复合涂层,使得模具表面硬度≥1600HV,水接触角≥110°,膜基结合力达到HF1级。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。

Claims (6)

1.一种低粘附轮胎模具的多层复合涂层,其特征在于,由模具基体到表面依次包括Cr粘结层、Cr/CrN纳米多层结构的过渡层和CrNiN工作层,所述Cr粘结层涂覆在模具基体上,所述CrNiN工作层中,按照原子数百分比计,包括Cr30~45%,Ni15~25%,N35~50%;
所述低粘附轮胎模具的多层复合涂层的制备方法,包括以下步骤:
(1)将轮胎的模具基体经过研磨抛光清洗并烘干后放入基片转架上,对基体表面进行辉光放电清洗;
(2)粘结层沉积:辉光放电清洗后,工作气体压力调节为0.3~0.8Pa,打开金属Cr靶,靶材电流为60~80A,转架速度控制在2~4rpm,模具基体偏压保持在-100V~-200V,温度加热到450℃,沉积时间为10~60min,获得Cr粘结层;
(3)纳米多层结构的过渡层沉积:Cr粘结层沉积结束后,保持模具基体温度、工作气压、Cr靶电流不变,基体偏压为-80V~-100V,沉积Cr层,沉积时间为5~10min,完成单个Cr层的沉积,然后通入N2气,N2气流量为400~600sccm,沉积CrN层,沉积时间为6~12min,完成单个CrN层的沉积,通过控制N2气质量流量计开关,重复上述工艺,交替沉积Cr层和CrN层;
(4)工作层沉积:开启CrNi合金靶开关,调节CrNi合金靶电流为60~85A,基体偏压为-80V~-120V,N2气流量为400~600sccm,沉积温度和工作压力与过渡层的相同,沉积时间为90~150min,获得CrNiN工作层。
2.根据权利要求1所述的一种低粘附轮胎模具的多层复合涂层,其特征在于,所述模具基体为模具钢或铝合金模具。
3.根据权利要求1所述的一种低粘附轮胎模具的多层复合涂层,其特征在于,所述Cr粘结层的厚度为0.1~0.5μm。
4.根据权利要求1所述的一种低粘附轮胎模具的多层复合涂层,其特征在于,所述Cr/CrN纳米多层结构的过渡层为至少交替沉积10次的Cr层和CrN层,过渡层的总厚度为2~5μm,每个Cr层的厚度为70~110nm,每个CrN层的厚度为80~125nm。
5.根据权利要求1所述的一种低粘附轮胎模具的多层复合涂层,其特征在于,所述CrNiN工作层的厚度为1~2μm。
6.根据权利要求1所述的一种低粘附轮胎模具的多层复合涂层,其特征在于,所述步骤(1)中,模具基体研磨抛光后表面粗糙度Ra≤0.1μm,辉光放电清洗的条件为:当真空室的本底真空度为5×10-4Pa时,通入Ar气,保持气压为1.0~4.0Pa,基片温度为300~500℃,模具基体偏压为-800~-1000V,轰击时间为5~30min。
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