CN106365637A - 一种镀膜用C/h‑BN复合蒸发舟及其制造方法 - Google Patents

一种镀膜用C/h‑BN复合蒸发舟及其制造方法 Download PDF

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CN106365637A
CN106365637A CN201610781265.9A CN201610781265A CN106365637A CN 106365637 A CN106365637 A CN 106365637A CN 201610781265 A CN201610781265 A CN 201610781265A CN 106365637 A CN106365637 A CN 106365637A
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曹志冠
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Abstract

本发明涉及真空蒸发镀铝薄膜用蒸发元件及其制作方法，具体涉及一种镀膜用C/h‑BN复合蒸发舟及其制造方法，该复合蒸发舟的舟体由C/h‑BN复合材料制成，所述C/h‑BN复合材料由多层六方氮化硼和石墨发热体自上而下交替叠放并通过热压烧结成一整体，其特征在于：所述舟体表层为带有蒸发槽的六方氮化硼烧结层，所述舟体底层为石墨发热体，该石墨发热体表面至少涂覆一层抗氧化热阻涂层。本发明所述蒸发舟的电阻率相对稳定、发热稳定，避免了因局部发热不均而导致蒸发材料的溅射，提高了镀膜质量。同时由于六方氮化硼烧结层保护了舟体，延长了使用寿命。本发明所使用的抗氧化热阻涂层，大幅度降低了石墨发热体在真空环境下的热辐射热能散失，起到了节约电能的作用。

Description

一种镀膜用C/h-BN复合蒸发舟及其制造方法
技术领域
本发明涉及真空蒸发镀铝薄膜用蒸发元件及其制作方法，具体涉及一种镀膜用C/h-BN复合蒸发舟及其制造方法。
背景技术
用蒸发材料（金属、特别是铝）涂覆基材最常用的方法是在高真空环境下采用物理沉积蒸镀法。使用的方法是将蒸发材料接触蒸发舟表面，蒸发材料受热便熔化并气化或升华，将待涂覆的基材通过蒸发舟上方，蒸发材料作为薄的蒸发材料层沉积在基材表面上。
为了产品需要的恒定蒸气流，将蒸发舟直接通电加热到1450～1650℃，连接输入蒸发材料，使其在蒸发舟表面液化、气化或升华 ，并在高真空环境中蒸发，在镀膜设备的蒸镀系统中设置一列蒸发舟，使得在基材上涂敷厚度均匀的蒸发材料层。
二硼化钛/氮化硼/氮化铝复合导电陶瓷蒸发舟是目前绝大多数镀膜设备的标准配置。该导电陶瓷蒸发舟由于高温铝腐蚀，其使用寿命一般只有 12-16 小时，最高不会超过20小时。由于该蒸发舟的不均匀腐蚀，同时也由于被蒸发的铝液也参与导电发热，到蒸发舟寿命的中后期容易造成铝液飞溅、烧穿基材、形成针孔的问题。其原因是：现有的蒸发舟在使用过程中，部分舟体表面因高温出现的微裂纹导致逐渐腐蚀，在蒸发过程中留下裂纹或空穴，这样熔融的蒸发材料（特别是活性铝液）会渗入这些裂纹或空穴中，使蒸发舟的电阻发生变化，并导致蒸发舟致密度下降，导致局部散热不均，使得蒸发过程中蒸发材料在蒸发舟表面润湿铺展不良，引起蒸发材料发生溅射现象，从而影响镀膜质量并缩短了蒸发舟的使用寿命，同时高温下蒸发舟表面由于热辐射也散失较多的热能，能耗较高。
发明内容
根据以上现有技术的不足，本发明所要解决的技术问题是：1.改善蒸发舟高温使用中产生裂纹或空穴的问题，延长其使用寿命；2.改善了蒸发材料在蒸发舟表面的润湿铺展能力；3.降低蒸发舟在使用过程中的能量损耗；为了解决上述问题，本发明提供一种镀膜用C/h-BN复合蒸发舟，能够减少蒸发舟在使用过程中由于蒸发材料的浸蚀蒸发而产生裂纹或空穴，同时降低蒸发舟的热辐射；本发明的另一目的是提供该复合蒸发舟的制造方法。
本发明所采用的技术方案是：一种镀膜用C/h-BN复合蒸发舟，该复合蒸发舟的舟体由C/h-BN复合材料制成，所述C/h-BN复合材料由多层六方氮化硼和石墨发热体自上而下交替叠放并通过热压烧结成一整体，其中所述舟体表层为带有蒸发槽的六方氮化硼烧结层，所述舟体底层为石墨发热体，该石墨发热体表面至少涂覆一层抗氧化热阻涂层。
所述抗氧化热阻涂层厚度为50～400μm。所述抗氧化热阻涂层优选方案采用氧化锆涂层。
石墨材料作为早期蒸镀金属的蒸发源材料,具有许多优良的性质,如良好的耐高温性、热稳定性,良好的导电性,较好的抗热震性能等。然而石墨材料在高温下易氧化、易与蒸镀的金属发生化学反应导致坩埚开裂,影响使用寿命。六方氮化硼(h-BN)与石墨是等电子体，具有类似石墨的层状结构，有白色石墨之称，有良好的润滑性，电绝缘性导热性和耐化学腐蚀性，具有中子吸收能力）与石墨具有相同的晶体结构,极为相似的热膨胀系数和热导率,优良的耐冷热循环冲击特性,是最理想的热匹配体系。而且BN对熔融金属的耐腐蚀性也很好,具有良好的高温电绝缘性和机械加工性能。
将石墨与六方氮化硼制成C/h-BN叠层状复合材料,根据复合材料的加和性,C/h-BN复合材料可保持单相的性质,同时具有两者共同优良的性质。由于六方氮化硼烧结层隔绝了蒸发材料对石墨电热体（导电材料）的浸蚀，使得蒸发舟在通电加热过程中电阻率相对稳定、发热稳定，提高了镀膜质量并延长了使用寿命。同时由于蒸发舟表面难以被蒸发材料腐蚀和氧化，使得蒸镀过程中蒸发材料润湿铺展均匀，受热均匀，不易发生蒸发材料飞溅现象。
本发明舟体下部的石墨电热体通电发热，通过热传导将热量传递到蒸发槽面用以熔化、气化蒸发材料 。由于六方氮化硼的耐腐蚀性，从而保护了舟体中的石墨电热体，延长了蒸发舟的使用寿命；由于六方氮化硼的绝缘性，从而保证了舟体中的石墨电热体的电阻率不受待蒸发材料的影响，从而保持相对稳定，蒸发舟发热稳定。
本发明蒸发舟底层石墨电热体表面的抗氧化热阻涂层具有对高温热辐射的抑制作用，有效的降低了石墨电热体通过热辐射的热能散失，同时促进了热能向槽体的流动，既提高了热传导的热流量，又降低了热能损耗，同时涂层也提高了石墨电热体的高温抗氧化能力。
本发明的制备方法步骤如下：
（1）按重量百分比计算，取90﹪～99﹪BN、0～7﹪CaO、0.5﹪～3﹪B2O3、 0.5﹪～3﹪Y2O3或取45﹪～99﹪BN、0﹪～45﹪AlN、0～7﹪CaO、0.5﹪～3﹪B2O3、 0.5﹪～3﹪Y2O3作为原料，将上述原料粉碎成颗粒为100～200目的粉体并进行混合；
（2）将混合后的粉体搅拌15～20分钟，再与酒精以重量百分比1：1.5～2的比例混合并搅拌10～15小时，将所述混合搅拌和的粉料在60～70℃加热10～15小时，烘干粉料并去除粉料中的酒精；
（3）将石墨块表面加工成适合的接头，然后在接头表面进行喷砂处理，然后涂覆或铺展过渡层材料，该过渡层材料为A、B两种组分的混合物，其中A组分为酚醛树脂、呋喃树脂、COPNA树脂、煤沥青液体或粉体中的任何一种或多种组合，B组分为石墨、碳化硅、碳化硼、氧化硼、立方氮化硼粉体中的任何一种或多种组合，A组分与B组分的质量百分比为100： 50～150；
（4）将上述处理好的原料粉体和处理好的石墨块自上而下交替放入高温炉模具中，交替铺放1～15层后送入高温真空炉进行热压烧结，高温真空炉内通入N2，温度为1750～2150℃，炉内气压为25～40MPa，加热3～15小时，退热冷却制得C/h-BN复合块体；将制得的C/h-BN复合块体进行切割和铣槽，制得C/h-BN复合蒸发舟毛坯；
（5）对上述步骤制得的C/h-BN复合蒸发舟毛坯的石墨面进行喷砂处理，再在该石墨面上涂覆至少一层抗氧化热阻涂层，涂层材料为金属材料或陶瓷材料，涂层厚度控制在50～400μm，最终得到蒸发舟产品。
进一步的，所述步骤（4）中，所述高温炉对原料进行热压烧结时，高温真空炉内压力＜0.2Pa时开始向炉内通入N2，炉内气压随炉温而变化：温度150℃加压至5MPa ；温度升至1100℃，加压力至10MPa ；当温度升到1850℃，加压至25MPa ；在温度为1850℃，压力为25MPa 下保温、保压60 分钟。
有益效果：本发明所述蒸发舟的电阻率相对稳定、发热稳定，避免了因局部发热不均而导致蒸发材料的溅射，提高了镀膜质量。同时由于六方氮化硼烧结层保护了舟体，延长了使用寿命。本发明所使用的抗氧化热阻涂层，大幅度降低了石墨发热体在真空环境下的热辐射热能散失，起到了节约电能的作用，有效的降低了使用成本，具有显著的经济和社会效益。
附图说明
下面参照附图结合实施例对本发明作进一步的描述。
图1为本发明表层结构的局部示意图。
图中：1. 六方氮化硼烧结层，2.石墨电热体，3. 抗氧化热阻涂层，4. 蒸发槽，5.隔流槽，6. 石墨电热体接头。
具体实施方式
实施例一：
本实施例所述的镀膜用C/h-BN复合蒸发舟，将颗粒为100～200目的原料粉体，以重量百分比BN:94﹪、CaO: 5﹪、B2O3：1﹪进行混合；
将厚8mm的石墨块进行上下表面加工，得到适合的接头形式，然后在其上下表面进行喷砂处理 ，然后涂覆酚醛树脂和石墨、立方氮化硼的混合物，其质量百分比为1：0.5：0.5；
将混合后的粉体和处理好的石墨块按厚度2：1，交替铺放入高温炉模具中，共计各6层，放入高温真空炉进行热压烧结。
高温真空炉内压力＜0.2Pa时开始向炉内通入N2，温度150℃加压至5MPa ；温度升至1100℃，加压力至10MPa ；当温度升到1850℃，加压至25MPa ；在温度为1850℃，压力为25MPa 下保温、保压60 分钟。
将制得的C/h-BN复合块体进行切割和铣槽制得毛坯C/h-BN复合蒸发舟，再进行石墨面喷砂处理，再在石墨面上涂覆300μm氧化锆涂层。
C/h-BN复合蒸发舟在真空镀膜机中工作电流控制在650～900A之间。其蒸镀效果良好，平均使用寿命在20小时以上，节约电能在30﹪以上。
实施例二：
本实施例所述的镀膜用C/h-BN复合蒸发舟，将颗粒为100-200目的原料粉体，以重量百分比BN:96﹪、CaO: 3﹪、B2O3：1﹪进行混合；
将厚8mm的石墨块进行上下表面加工，得到适合的接头形式，然后在其上下表面进行喷砂处理 ；
将颗粒为100-200目的中温煤沥青粉体和立方氮化硼粉体按质量百分比为1：0.5进行混合；
将混合后的BN粉体、煤沥青/氮化硼混合物粉体涂覆或铺展在石墨块表面，先铺一层煤沥青/氮化硼混合物粉体，再铺一层BN粉体混合物，依次按厚度100：1：200一层一层铺放入高温炉模具中，共计各6层进行热压烧结。
高温真空炉内压力＜0.2Pa时开始向炉内通入N2，温度450℃加压至5MPa ；温度升至1100℃，加压力至20MPa ；当温度升到1850℃，加压至40MPa ；在温度为2150℃，压力为40MPa 下保温、保压90 分钟。
将制得的C/h-BN复合块体进行切割和铣槽制得C/h-BN复合蒸发舟毛坯，再进行石墨面喷砂处理，再在石墨面上涂覆300μm氧化锆涂层。
经实际测试，本实施例制得的C/h-BN复合蒸发舟在真空镀膜机中工作电流控制在650～900A之间。其蒸镀效果良好，平均使用寿命在20小时以上，节约电能在30﹪以上。
实施例三：
本实施例所述的镀膜用C/h-BN复合蒸发舟，将颗粒为100-200目的原料粉体，以重量百分比BN:51﹪、AlN: 45﹪、CaO: 3﹪、B2O3：1﹪进行混合；
将厚8mm的石墨块进行上下表面加工，得到适合的接头形式，然后在其上下表面进行喷砂处理 ；
将颗粒为100-200目的中温煤沥青粉体和立方氮化硼粉体按质量百分比为1：0.5进行混合；
将混合后的BN粉体、煤沥青粉体混合物涂覆或铺展在石墨块表面，先铺一层煤沥青粉体混合物，再铺一层BN粉体混合物，依次按厚度100：1：200一层一层铺放入高温炉模具中，共计各6层进行热压烧结。
高温真空炉内压力＜0.2Pa时开始向炉内通入N2，温度450℃加压至5MPa ；温度升至1300℃，加压力至20MPa ；当温度升到1850℃，加压至40MPa ；在温度为2150℃，压力为40MPa 下保温、保压90 分钟。
将制得的C/h-BN复合块体进行切割和铣槽制得毛坯C/h-BN复合蒸发舟，再进行石墨面喷砂处理，再在石墨面上涂覆300μm氧化锆涂层。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (6)

1.一种镀膜用C/h-BN复合蒸发舟，该复合蒸发舟的舟体由C/h-BN复合材料制成，所述C/h-BN复合材料由多层六方氮化硼和石墨发热体自上而下交替叠放并通过热压烧结成一整体，其特征在于：所述舟体表层为带有蒸发槽的六方氮化硼烧结层，所述舟体底层为石墨发热体，该石墨发热体表面至少涂覆一层抗氧化热阻涂层。
2.根据权利要求1所述一种镀膜用C/h-BN复合蒸发舟，其特征在于：所述舟体表层两端设有防止蒸发材料溢流到电极端的隔流槽，其宽度为2～5mm，深1～2mm。
3.根据权利要求1所述一种镀膜用C/h-BN复合蒸发舟，其特征在于：所述抗氧化热阻涂层厚度为50～400μm。
4.根据权利要求3所述一种镀膜用C/h-BN复合蒸发舟，其特征在于：所述抗氧化热阻涂层是金属涂层或氧化锆涂层。
5.一种制备权1所述一种镀膜用C/h-BN复合蒸发舟的方法，其特征在于具有以下步骤：
（1）按重量百分比计算，取90﹪～99﹪BN、0～7﹪CaO、0.5﹪～3﹪B2O3、 0.5﹪～3﹪Y2O3或取45﹪～99﹪BN、0﹪～45﹪AlN、0～7﹪CaO、0.5﹪～3﹪B2O3、 0.5﹪～3﹪Y2O3作为原料，将上述原料粉碎成颗粒为100～200目的粉体并进行混合；
（2）将混合后的粉体搅拌15～20分钟，再与酒精以重量百分比1：1.5～2的比例混合并搅拌10～15小时，将所述混合搅拌和的粉料在60～70℃加热10～15小时，烘干粉料并去除粉料中的酒精；
（3）将石墨块表面加工成适合的接头，然后在接头表面进行喷砂处理，然后涂覆或铺展过渡层材料，该过渡层材料为A、B两种组分的混合物，其中A组分为酚醛树脂、呋喃树脂、COPNA树脂、煤沥青液体或粉体中的任何一种或多种组合，B组分为石墨、碳化硅、碳化硼、氧化硼、立方氮化硼粉体中的任何一种或多种组合，A组分与B组分的质量百分比为100： 50～150；
（4）将上述处理好的原料粉体和处理好的石墨块自上而下交替放入高温炉模具中，交替铺放1～15层后送入高温真空炉进行热压烧结，高温真空炉内通入N2，温度为1750～2150℃，炉内气压为25～40MPa，加热3～15小时，退热冷却制得C/h-BN复合块体；将制得的C/h-BN复合块体进行切割和铣槽，制得C/h-BN复合蒸发舟毛坯；
（5）对上述步骤制得的C/h-BN复合蒸发舟毛坯的石墨面进行喷砂处理，再在该石墨面上涂覆至少一层抗氧化热阻涂层，涂层材料为金属材料或陶瓷材料，涂层厚度控制在50～400μm，最终得到蒸发舟产品。
6.按照权利要求5所述一种镀膜用C/h-BN复合蒸发舟的制备方法，其特征为：所述步骤（4）中，所述高温炉对原料进行热压烧结时，高温真空炉内压力＜0.2Pa时开始向炉内通入N2，炉内气压随炉温而变化：温度150℃加压至5MPa ；温度升至1100℃，加压力至10MPa ；当温度升到1850℃，加压至25MPa ；在温度为1850℃，压力为25MPa 下保温、保压60 分钟。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109890094A (zh) * 2019-03-15 2019-06-14 西安交通大学 一种高温发热膜及其制备方法
CN112981327A (zh) * 2019-12-12 2021-06-18 中国科学院大连化学物理研究所 一种真空热蒸镀用一体化蒸发源

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109890094A (zh) * 2019-03-15 2019-06-14 西安交通大学 一种高温发热膜及其制备方法
CN112981327A (zh) * 2019-12-12 2021-06-18 中国科学院大连化学物理研究所 一种真空热蒸镀用一体化蒸发源

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