CN108558408A - 一种一体化微通道板的制备方法 - Google Patents

一种一体化微通道板的制备方法 Download PDF

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CN108558408A
CN108558408A CN201810567029.6A CN201810567029A CN108558408A CN 108558408 A CN108558408 A CN 108558408A CN 201810567029 A CN201810567029 A CN 201810567029A CN 108558408 A CN108558408 A CN 108558408A
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李钰龙
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Abstract

本发明提供了一种一体化微通道板的制备方法：将空心的微管内部填充液体状态的低熔点的芯料，然后两端封端降温至芯料熔点以下，得到微通道模具；在压制模具中加入一半量的陶瓷粉末，再将微通道模具放入，然后逐步加入剩余的陶瓷粉末，压合成微通道板坯；将微通道板坯放入烧结炉初步烧结定型；将微通道模具开封，在高温条件下使芯料融化，气体压出；然后将微管分解，形成一体化微通道板；再将微通道板放入烧结炉中缓慢升温烧结，得到一体化微通道板成品。本发明通过采用含芯料微通道模具制备内部有规则的微通道的特种陶瓷板的方法制备一体化微通道板，该方法简单、成品率高。

Description

一种一体化微通道板的制备方法
技术领域
本发明属于设备加工技术领域，特别涉及一种特种陶瓷一体化微通道板的制备方法。
背景技术
迄今为止，国内外特种陶瓷微通道板加工微通道的方法大都采用分体式加工，以光刻、微机械加工、微蚀刻、多纤维拉制、激光化学三维写入、三D打印、石蜡酸蚀、模块式构件组装及微图形转印等工艺方法的技术路线；其微通道几乎均在平面上形成二分之一的微通道后再用对称的另一部分弥合继而才能形成微通道整体构造，加工工艺复杂，加工成本高，组装困难、密度不够，压合、粘合都存在。目前这种“两片式”的微通道都采用压合或者粘合的方式密封，缺点是密封面易渗漏等问题，且耐高温高压的效果较差，在长期使用过程中易在结合处泄露原料，造成环境污染、及其它不安全因素，甚至造成使用者的人身危险。
中国专利201310262110.0一种微通道芯体制造工艺，提供了一种一体化的微通道板的制作过程，以无纺布形成最终的微通道。然而，该微通道板属于载体微通道，形成的微通道形状不规则、孔隙太小，微通道内壁粗糙。流体微通道板的微通道内表面需尽量光滑防止产物吸附，而且通道的形状有确定的形状；因此上述通过无纺布形成微通道的方法不适合流体微通道的生产。
中国专利201310262182.5一种微通道芯体制造工艺，提供了一种采用微丝束形成微通道芯体的方法。然而，微丝的机械强度有限，在形成具有确定形状的的微通道时容易发生形变造成微通道形状与最初设计形状不同，而且微通道内表面也会有不光滑的现象。另外，对于复杂平面通道形状的微通道没有办法生产。
发明内容
针对现有技术中缺乏制备一体化微通道板的方法的问题，本发明提供一种制备一体化微通道板的方法，方法简单、成品率高，制备的产品耐腐蚀、耐高压，不渗漏、易组装，减少密封面积。
为实现上述目的，本发明采用如下技术方案。
一种一体化微通道板的制备方法，包括以下步骤：
（1）将空心的微管内部填充液体状态的低熔点的芯料，然后两端封端降温至芯料熔点以下，得到微通道模具；
所述微管的材料为纯金属、合金或树脂聚合物，如环氧树脂、醇醚、聚酰亚胺、亚克力、聚丙烯塑料；优选为合金。更优选的，合金的成分为铝55-56%、锡35-36%，铟10-11%和不可避免的杂质；合金的制备方法可采用常规的合金制备方法。
所述芯料的熔点为50-100℃；优选为60-80℃。所述芯料选自无机盐或有机化合物。
（2）在压制模具中加入一半量的陶瓷粉末，再将步骤（1）中微通道模具放入，然后逐步加入剩余的陶瓷粉末，压合成微通道板坯；
所述陶瓷材料优选为碳化硅、氮化硅、氮化硼、氧化锆、氧化铝；最优选为碳化硅。所述陶瓷粉末的粒径优选为1-10μm。所述压合的压强为80Mpa-300Mpa。
（3）将步骤（2）中的微通道板坯放入烧结炉初步烧结定型；
步骤（3）中，所述烧结温度为600-1800℃，保温时间为2h-4h。
（4）将微通道模具开封，在高温条件下使芯料融化，气体压出；然后将微管分解，形成具有光滑微通道内壁的一体化微通道板；
所述步骤（4）中，高温温度为60-120℃，优选为80-100℃。
所述微管分解方法为腐蚀、溶解或微波振荡。腐蚀法的溶剂为稀酸；更优选为硫酸与盐酸的混酸；最优选为15%wt硫酸与20%wt盐酸的混酸。
（5）将步骤（4）得到的微通道板放入烧结炉中缓慢升温烧结，得到一体化微通道板成品。
作为优选，步骤（3）或（5）的升温速率如下：20-200℃，30-50℃/h；200-600℃，50-100℃/h；600-2000℃，100-150℃/h；2000-2200℃，30-50℃/h。
所述成品的密度为3-3.15g/cm3。
作为优选，步骤（5）的烧结步骤采用阶梯升温：分别在升温至200℃600℃、2000℃、最终烧结温度时保温1-2h。
作为优选，步骤（5）还包括对烧结后的微通道板粗磨、抛光的过程。
本发明还包括一种上述制备方法获得的微通道板。
本发明具有以下优点：
本发明通过采用含芯料微通道模具制备内部有规则的微通道的特种陶瓷板的方法制备一体化微通道板，该方法简单、成品率高。通过注芯的方法提高空心管在压制微通道板时的耐压能力，防止压制板坯时变性；通过特有的金属材料制备空心微管，一方面提高了机械强度、耐压性能，另一方面金属材料的易腐蚀性，后续步骤中可容易的去除，制备的微通道内壁光滑。本发明制备的产品可以耐2000℃高温、6Mpa工作压力，180℃以上瞬间热冲击，可实现超高温、超高压的液液、气液、气气等化学反应，耐腐蚀、高耐压，不易渗漏，大大拓展目前的化学反应设计空间。
附图说明
图1为实施例1中制备的微通道管道；
图2为实施例1中制备的微通道板成品。
具体实施方式
下面结合实施例和附图对本发明做进一步说明，但本发明不受下述实施例的限制。
实施例1 一体化微通道板的制备
（1）将主成分为铝55%、铟10%、锡35%的合金根据微通道的形状铸成弯曲的空心合金微管；将弯曲的空心合金微管内部填充85℃的液体状态的芯料（吡啶苄甲胺），然后两端封端自然降温至室温，得到微通道模具，如图1所示：中心银白色的微管即微通道模具；
（2）在压制模具中加入一半量的碳化硅陶瓷粉末，细度为3μm，再将步骤（1）中微通道模具放入，然后逐步加入剩余的碳化硅陶瓷粉末，逐渐增压至200 Mpa压合成微通道板坯；
（3）将步骤（2）中的微通道板坯放入烧结炉升温至1800℃，升温速率如下：20-200℃，30℃/h，保温2h；200-600℃，100℃/h，保温2h；600-1800℃，150℃/h，保温2h后随炉降温，初步烧结定型；
（4）将微通道模具开封，在120℃下使芯料融化，用高压氮气压出液体芯料；然后用15%wt硫酸与20%wt盐酸的混酸将微管分解，形成具有光滑微通道内壁的一体化微通道板；
（5）将步骤（4）得到的微通道板放入烧结炉中缓慢升温至2160℃烧结，升温速率如下：20-200℃，50℃/h，保温2h；200-600℃，100℃/h，保温2h；600-2000℃，150℃/h，保温1h；2000-2160℃，50℃/h，保温2h；随炉降温得到成型的微通道板，密度为3.15g/cm3，粗磨、抛光后获得一体化微通道板成品，如图2所示：表面镜面光滑，侧面无接缝。
经测试，该微通道板工作压力可达6Mpa以上，180℃瞬间热冲击。

Claims (10)

1.一种一体化微通道板的制备方法，其特征在于，包括以下步骤：
（1）将空心的微管内部填充液体状态的低熔点的芯料，然后两端封端降温至芯料熔点以下，得到微通道模具；
（2）在压制模具中加入一半量的陶瓷粉末，再将步骤（1）中微通道模具放入，然后逐步加入剩余的陶瓷粉末，压合成微通道板坯；
（3）将步骤（2）中的微通道板坯放入烧结炉初步烧结定型；
（4）将微通道模具开封，在高温条件下使芯料融化，气体压出；然后将微管分解，形成具有光滑微通道内壁的一体化微通道板；
（5）将步骤（4）得到的微通道板放入烧结炉中缓慢升温烧结，得到一体化微通道板成品。
2.根据权利要求1所述的制备方法，其特征在于，所述微管的材料为纯金属、合金或树脂聚合物；优选的，所述微管的材料为合金；更优选的，合金的成分为铝55-56%、锡35-36%，铟10-11%和不可避免的杂质。
3.根据权利要求1所述的制备方法，其特征在于，所述芯料的熔点为50-100℃。
4.根据权利要求1所述的制备方法，其特征在于，所述陶瓷材料选自为碳化硅、氮化硅、氮化硼、氧化锆、氧化铝；最优选为碳化硅；优选的，所述陶瓷粉末的粒径优选为1-10μm。
5.根据权利要求1所述的制备方法，其特征在于，步骤（2）中，所述压合的压强为80Mpa-300Mpa；步骤（4）中，所述温度为60-120℃。
6.根据权利要求1所述的制备方法，其特征在于，所述微管分解方法为腐蚀、溶解或微波振荡；腐蚀法的溶剂优选为稀酸；更优选为硫酸与盐酸的混酸；最优选为15%wt硫酸与20%wt盐酸的混酸。
7.根据权利要求1所述的制备方法，其特征在于，步骤（3）中，所述烧结温度为600-1800℃，保温时间为2h-4h；步骤（5）的烧结步骤采用阶梯升温：分别在升温至200℃600℃、2000℃、最终烧结温度时保温1-2h；
优选的，步骤（3）或（5）的升温速率如下：20-200℃，30-50℃/h；200-600℃，50-100℃/h；600-2000℃，100-150℃/h；2000-2200℃，30-50℃/h。
8.根据权利要求1所述的制备方法，其特征在于，所述成品的密度为3-3.15g/cm3。
9.根据权利要求1所述的制备方法，其特征在于，步骤（5）还包括对烧结后的微通道板粗磨、抛光的过程。
10.一种如权利要求1-9任一所述的制备方法获得的微通道板。
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CN110407582A (zh) * 2019-08-05 2019-11-05 衢州学院 一种基于凝胶成型的碳化硅微反应器制备方法
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CN115140942B (zh) * 2022-07-27 2024-03-12 之江实验室 一种玻璃陶瓷微反应器的制备方法及微反应器

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