CN113265611B - 模具内表面易脱模涂层制备方法 - Google Patents

模具内表面易脱模涂层制备方法 Download PDF

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CN113265611B
CN113265611B CN202110811532.3A CN202110811532A CN113265611B CN 113265611 B CN113265611 B CN 113265611B CN 202110811532 A CN202110811532 A CN 202110811532A CN 113265611 B CN113265611 B CN 113265611B
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杨红娜
蔡风园
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Beijing Aerospace Tianmei Technology Co ltd
Beijing Aerospace Hexing Technology Co Ltd
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    • 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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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C33/3842—Manufacturing moulds, e.g. shaping the mould surface by machining
    • 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
    • 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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    • 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
    • C23C28/04—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
    • 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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    • 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
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C23C8/80—After-treatment
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00—Moulds or cores; Details thereof or accessories therefor
    • B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
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Abstract

本申请涉及涂层制备领域，提供一种模具内表面涂层，改善模具表面易腐蚀、不易脱模、硬度不高、耐磨性不强的技术问题，防止模具本体与被成型材料之间出现粘连现象，通过在模具内腔表面形成类金刚石涂层得到易脱模模具，在制备涂层前对基体进行渗碳处理，提高涂层与基体之间的结合力，避免类金刚石在使用过程中脱落，提高模具整体的使用寿命。

Description

模具内表面易脱模涂层制备方法
技术领域
本申请涉及涂层制备领域，具体涉及一种易脱模涂层制备方法。
背景技术
弹翼是飞航器至关重要的增程部件，为飞行提供升力，飞行过程中其翼面承受气动均布载荷，需满足一定强度要求和耐高温要求。为了实现轻量化，弹翼常采用轻合金、碳纤维复合材料制备得到。与其他材料相比，碳纤维复合材料具有很高的比强度和比模量，并且具有可设计性强等优势。因而大量采用碳纤维复合材料，是弹翼轻量化的重要途径之一。
碳纤维复合材料的成型技术有很多，模压成型具有较高的生产效率，适于大批量生产，制品尺寸精确，表面光洁，多数结构复杂的制品可一次成型，无需有损于制品性能的辅助加工，制品外观及尺寸的重复性好等优势。但是，复合材料模压成型模具的设计与制造较复杂，而且产品在启模过程中容易受模腔限制，产品脱模困难；有时不当的模具结构设计会造成产品受压不均，产品内部质量欠佳。
在模具模腔内表面制备特种涂层能够提高其脱模效果，避免在固化碳纤维增强预浸布脱模过程中出现黏胶、脱模难的问题。
发明内容
本申请改善模具表面易腐蚀、不易脱模、硬度不高、耐磨性不强的技术问题，防止模具本体与被成型材料之间出现粘连现象，通过在模具内腔表面形成类金刚石涂层得到易脱模模具，在制备涂层前对基体进行渗碳处理，提高涂层与基体之间的结合力，避免类金刚石在使用过程中脱落，提高模具整体的使用寿命。
模具处理第一步对模具内表面进行渗碳处理，具体步骤为：模具表面清洗：为了去除油渍，先用浓度为2.0～3.0％碳酸钠碱液清洗模具15～25min，清洗时温度为80～85℃；然后为了去除氧化皮在浓度为4.2～5.0％稀盐酸中清洗20～25min；再将模具先后放入丙酮溶液、乙醇溶液和去离子水中超声40～45min，以提高模具表面活性，吹干待用；模具在渗碳炉中，渗碳炉炉内温度为845-860℃，渗碳过程中的碳浓度为0.4-0.6％，渗碳时间为20-30min，随后进行回火处理，回火处理温度390-395℃，时间60min，最终冷却至室温。
渗碳过程中对渗碳炉炉内温度、碳浓度以及时间进行控制，使得模具模腔内表面得到含碳渗层即可，避免渗层过厚导致模具表面硬度过高，使得与后续制备得到的类金刚石层发生失配，在重复使用脱模过程中涂层与固化树脂粘连而从模具表面脱落。较高的碳势及温度还容易引起表面的畸变，导致最终产品形状的不规则，影响产品的气动外形。渗碳层的形成会在表面得到含碳化合物层，提高基体与后续DLC层的结合性能，避免发生DLC层与固化树脂粘连而脱落的现象。
模具处理第二步为CVD法类金刚石制备，具体工艺为：通入CH4、四甲基硅烷，气流比例3.0-5.0，保持真空度8×10-4～4×10-3Pa，偏压为500-600V，沉积时间1-2h，在模具基材内表面获得Si-DLC涂层。
通过参数调整，制备得到Si掺杂的DLC层，其有利于固化后的碳纤维增强预浸布从模具表面脱离。在模具表面形成微纳米结构的DLC涂层，Si的加入能够降低涂层表面能，使固化碳纤维树脂复合材料与模具两者不相亲，从而抑制粘附。在降低表面能的同时通过形成微纳结构增加比表面积，可以进一步降低复合材料在模具表面发生粘附的可能。
具体实施方式
实施例1：
第一步对模具内表面进行渗碳处理，具体步骤为：模具表面清洗：为了去除油渍，先用浓度为2.0％碳酸钠碱液清洗模具20min，清洗时温度为80℃；然后为了去除氧化皮在浓度为5.0％稀盐酸中清洗25min；再将模具先后放入丙酮溶液、乙醇溶液和去离子水中超声45min，以提高模具表面活性，吹干待用；模具在渗碳炉中，渗碳炉炉内温度为850℃，渗碳过程中的碳浓度为0.5％，渗碳时间为25min，随后进行回火处理，回火处理温度395℃，时间60min，最终冷却至室温。
第二步类金刚石制备，具体工艺为：通入CH4、四甲基硅烷，气流比例4:1，保持真空度1×10-3Pa，偏压为540V，沉积时间1.5h，在模具基材内表面获得Si-DLC涂层。
制备得到的模具进行碳纤维增强预浸布制备弹翼的热固化成型，模具中120℃加热固化2h后拆除成型工装。表1中给出了在使用后脱模过程中是否出现粘连现象的测试结果，存在粘连现象以“○”表示，无粘连现象“√”表示。实施例1技术方案经150次循环使用后脱模过程中仍未出现粘连现象
实施例2-4及对比例1-7
仅调整渗碳处理参数，具体采用的其他实施参数与实施例1相同，具体参见表1，制备得到的模具进行碳纤维增强预浸布制备弹翼的热固化成型，模具中120℃加热固化2h后拆除成型工装。经实施例2-4中技术方案处理后的模具内表面在150次循环使用后，脱模过程仍未出现粘连现象。对比例1-3在实施例1的基础上对渗碳温度进行了调整，测试显示在100次循环使用或150次循环使用过程中出现了脱模粘连现象，渗碳温度的变化，会影响模具在多次使用后的脱模过程，温度改变会导致渗碳层硬度的变化，引起模具与后续DLC不匹配的发生，导致循环使用后DLC层出现脱落，导致防粘连作用消失。对比例4-5在实施例1的基础上对渗碳浓度进行了调整，测试显示在100次循环使用或150次循环使用过程中出现了脱模粘连现象，较高的碳浓度会导致渗层厚度增加、硬度提高，使得与后续制备得到的类金刚石层发生失配，在重复使用脱模过程中类金刚石层与固化树脂粘连而从模具表面脱落，较低的碳浓度又无法有效形成连续的渗层，导致未在模具的全部表面得到含碳化合物层，无法提高基体与后续DLC层的结合性能，在循环使用过程中DLC层同样容易与固化树脂粘连而从模具表面脱落，可见碳浓度的变化同样会引起多次使用后脱模过程粘连问题的出现。对比例6-7相对于实施例1对渗碳时间进行调整，测试显示在150次循环使用过程中出现了脱模粘连现象，较长的渗碳时间会导致渗层厚度增加、硬度提高，使得与后续制备得到的类金刚石层发生失配，在重复使用脱模过程中类金刚石层与固化树脂粘连而从模具表面脱落，较短的时间又无法有效形成连续的渗层，导致未在模具的全部表面得到含碳化合物层，无法提高基体与后续DLC层的结合性能，在循环使用过程中DLC层同样容易与固化树脂粘连而从模具表面脱落。此外对比例5中，处理后模具成型后的弹翼外形不合格率较高。
渗碳炉炉内温度为845-860℃，渗碳过程中的碳浓度为0.4-0.6％，渗碳时间为20-30min，渗碳过程中对渗碳炉炉内温度、碳浓度以及时间进行控制，使得模具模腔内表面得到含碳渗层即可，避免渗层过厚导致模具表面硬度过高，使得与后续制备得到的类金刚石层发生失配，在重复使用脱模过程中涂层与固化树脂粘连而从模具表面脱落。较高的碳势及温度还容易引起表面的畸变，导致最终产品形状的不规则，影响产品的气动外形。
表1 渗碳处理参数表
Figure DEST_PATH_IMAGE001
实施例5-9及对比例8-12
仅调整DLC制备参数，具体采用的其他实施参数与实施例1相同，具体参见表2，制备得到的模具进行碳纤维增强预浸布制备弹翼的热固化成型，模具中120℃加热固化2h后拆除成型工装。经实施例5-9处理的模具在150次循环使用后脱模过程中仍未出现粘连现象。对比例8未通入四甲基硅烷，在150次循环使用脱模过程中出现了较为严重的粘连现象，DLC层中为掺杂Si无法降低涂层的表面能，固化碳纤维树脂复合材料与模具亲和性更高，无法抑制粘附。对比例9-12在实施例1的基础上调整了掺杂Si的浓度，也在150次循环使用脱模过程中出现了不同程度的粘连现象。Si掺杂的比例会导致微纳结构表面粗糙度的变化以及涂层表面能的不同，通过工艺参数调整，在降低表面能的同时通过形成微纳结构增加比表面积，可以进一步降低复合材料在模具表面发生粘附和可能。
CVD法获得Si-DLC涂层的具体工艺为通入CH4、四甲基硅烷，气流比例3.0-5.0，保持真空度8×10-4～4×10-3Pa，偏压为500-600V，沉积时间1-2h，制备得到Si掺杂的DLC层，在模具表面形成微纳米结构的DLC涂层，Si的加入能够降低涂层表面能，使固化碳纤维树脂复合材料与模具两者不相亲，从而抑制粘附。控制CH4、四甲基硅烷气流比例，在降低表面能的同时通过形成微纳结构增加比表面积，可以进一步降低复合材料在模具表面发生粘附的可能。
表2 DLC制备参数表
Figure 183629DEST_PATH_IMAGE002

Claims (2)

1.一种模具内表面涂层的制备方法，其特征在于，首先对模具进行清洁，而后模具在渗碳炉中，渗碳炉炉内温度为845-860℃，渗碳过程中的碳浓度为0.4-0.6％，渗碳时间为20-30min，随后进行回火处理，回火处理温度390-395℃，时间60min，最终冷却至室温，最后在经处理的模具内表面通过CVD法获得Si-DLC涂层，CVD法获得Si-DLC涂层的具体工艺为通入CH4、四甲基硅烷，气流比例3.0-5.0，保持真空度8×10-4～4×10-3Pa，偏压为500-600V，沉积时间1-2h，在模具基材内表面获得Si-DLC涂层，所述模具为固化碳纤维增强预浸布所用模具。
2.如权利要求1所述的模具内表面涂层的制备方法，其特征在于，具体的模具清洁方法为先用浓度为2.0～3.0％碳酸钠碱液清洗模具15～25min，清洗时温度为80～85℃；然后为了去除氧化皮在浓度为4.2～5.0％稀盐酸中清洗20～25min；再将模具先后放入丙酮溶液、乙醇溶液和去离子水中超声40～45min，吹干待用。
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