CN115141015B - 一种陶瓷弹簧、制备方法 - Google Patents

一种陶瓷弹簧、制备方法 Download PDF

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CN115141015B
CN115141015B CN202210651365.5A CN202210651365A CN115141015B CN 115141015 B CN115141015 B CN 115141015B CN 202210651365 A CN202210651365 A CN 202210651365A CN 115141015 B CN115141015 B CN 115141015B
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parts
ceramic
spring
additive
powder
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CN115141015A (zh
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李伶
王营营
王伟伟
隋松林
于宏林
王守兴
屈忠宝
刘时浩
曹守刚
吕佳琪
陈云锋
李楠
马心祎
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Abstract

本发明公开了一种陶瓷弹簧、制备方法，陶瓷弹簧由以下重量份原料制备而成：按重量份，陶瓷粉末53.3‑78份，水15‑30份，所述甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物4.2‑8.5份。陶瓷粉末、水与甲基纤维素，羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物中的至少一个混合，并在脱水的过程使线材长度收缩10‑20％，弹簧坯体塑化后再次干燥、等静压收缩，避免干燥时直接完成收缩，收缩量与弹簧的塑形不匹配导致变形、开裂，有效降低因烧结时弹簧收缩导致陶瓷弹簧变形、开裂。

Description

一种陶瓷弹簧、制备方法
技术领域
本发明涉及陶瓷弹簧生产技术领域，具体提供一种陶瓷弹簧、制备方法。
背景技术
弹簧是机械结构中常用的基础性零部件，通常用于制造弹簧的材料为金属。然而普通金属弹簧的工作温度不超过200℃，使用特种合金(如镍基合金)制造的耐热弹簧工作温度也不超过800℃。此外金属材料的耐腐蚀性、耐磨性表现相比于陶瓷材料也较差。
陶瓷弹簧相比于金属弹簧就具有无可替代的优势，但是，陶瓷弹簧制备过程中存在两个技术问题，一是成型后陶瓷颗粒间会存在间隙影响陶瓷弹簧的强度，二是弹簧成型过程中收缩容易导致变形的问题。
发明内容
本发明的技术任务是针对上述存在的问题，提供一种陶瓷弹簧、制备方法。
根据本发明的一个方面，提供一种陶瓷弹簧，由以下重量份原料制备而成：
陶瓷粉末53.3-78份，水15-30份，甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物4.2-8.5份。作为可选方案，所述陶瓷弹簧的高度不小于0.6cm。具体的，所述陶瓷粉末添加量为53.3份-78份，比如可以是53.3份、56份、65份、72份、75份、78份等；水可以是15份、20份、25份、30份等，水优选为去离子水。所述水为去离子水，除去了呈离子形式杂质后的纯水。所述甲基纤维素，羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物占混合物的质量比为4.2份-8.5份，可以是4份、4.5份、5份、5.5份、6份、6.2份、7.3份或8.0份等。
进一步的，还包括第一添加剂，所述第一添加剂为己基草酸，乙二醇聚氧乙烯醚、聚乙烯醇(PVA)，腐植酸钠、邻苯二甲酸二(2-乙基己)酯中一种或多种，按重量份，所述第一添加剂添加量为7.0-8.9份。可以是7份、7.5份、7.8份、8.4份、8.5份、8.6份或8.9份等，第一添加剂作为固体分散剂的载体能够对陶瓷粉体进行增塑和润滑，有利于挤出时线材的表面光滑。
进一步的，还包括第二添加剂，所述第二添加剂为异丁醇、丙二醇或邻苯二甲酸二甲酯中的一种或多种，按重量份，所述第二添加剂添加量为4.1-4.5份。可以是4.1份、4.2份、4.3份、4.4份或4.5份等，第二添加剂具有保湿作用和塑化的作用。
进一步的，还包括第三添加剂，所述第三添加剂为聚羧酸铵盐溶液、聚丙烯酸铵盐与聚羧酸铵盐混合溶液、纯碱溶液、腐植酸钠溶液、鞣性减水剂、草酸钠溶液、聚偏磷酸钠溶液、焦磷酸钠溶液、丹宁酸钠溶液中的一种或多种，按重量份，所述第三添加剂添加量为2-4份。可以是2份、2.5份、3份、3.5份、3.8份或4份等，作为分散剂及减水剂使用。
进一步的，所述陶瓷粉末为氧化锆粉末、氮化硅粉末、碳化硅粉末，或者氮化硅粉末与碳化硅粉末的混合物。
进一步的，还包括氧化物或非氧化物烧结助剂，所述氧化物或非氧化物烧结助剂包括:CuO、B2O3、ZrO2、CaO、La2O3、Li2CO3、TiO2、BaO、MnO、SiO2、Y2O3、Al2O3、MgO和CeO中的一种或多种，按重量份，所述第烧结助剂添加量为3-5份。可以是3份、3.5份、3.8份、4份、4.5份、5份等，作为分散剂及减水剂使用。
根据本发明的另一个方面，提供一种陶瓷弹簧的制备方法，包括以下步骤：
将陶瓷粉末、水与甲基纤维素，羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物中的至少一个混合，形成混合物；按重量份，所述陶瓷粉末的添加量为53.3-78份，所述水的添加量为15-30份，所述甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物的总添加量为4.2-8.5份。具体的，所述陶瓷粉末添加量为53.3份-78份，比如可以是53.3份、56份、65份、72份、75份、78份等；水可以是15份、20份、25份、30份等，水优选为去离子水。所述水为去离子水，除去了呈离子形式杂质后的纯水。所述甲基纤维素，羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物占混合物的质量比为4.2-8.5份，可以是4份、4.5份、5份、5.5份、6份、6.2份、7.3份或8.0份等。
将所述混合物挤出成型为线材，所述线材的直径为0.6-3mm，可以是0.6mm、0.8mm、1mm、1.5mm、1.8mm、2mm、2.1mm、2.5mm或者3mm等；
将所述线材进行脱水，并在脱水的过程使线材长度收缩10-20％；
将脱水后的所述线材通过有机溶剂进行塑化，使陶瓷材料通过钢材弹簧的加工生产方式生产出来，相比于采用陶瓷注模成型然后进行后续切削处理的陶瓷弹簧生产方式可有效节省至少40-70％的原材料消耗。
将塑化后的线材缠绕成具有一定匝数的线圈并进行冷等静压成型得到弹簧坯体；作为可选方案，塑化时浸入有机溶剂的时间为50-150秒，可以是50秒、60秒、70秒、80秒、90秒、100℃、105秒、110秒、115秒、120秒、125秒、130秒、140秒或者150秒等。
将所述弹簧坯体依次进行烧结和回火处理后，即得，其中，烧结温度为1400℃-1800℃，回火处理的温度不高于烧结温度。根据原料的不同，烧结温度可以选择1400℃、1450℃、1500℃、1550℃、1600℃、1650℃、1700℃、1750℃或者1800℃，必要时需要使用惰性气体保护。将烧结后的线圈进行回火处理，优选，在氮气气氛中低压低速升温烧结，根据原料不同选择烧结温度1200℃-1600℃，可以选择1200℃、1300℃、1400℃、1500℃、1600℃，氮气压力为0.1-2MPa，升温速率为0.5-10℃/min。
进一步的，所述混合物中包括第一添加剂，所述第一添加剂为己基草酸，乙二醇聚氧乙烯醚、聚乙烯醇(PVA)，腐植酸钠、邻苯二甲酸二(2-乙基己)酯等一种或多种混合物，按重量份，所述第一添加剂添加量为7-8.9份。
进一步的，所述混合物中包括第二添加剂，所述第二添加剂为异丁醇、丙二醇、丙三醇或邻苯二甲酸二甲酯一种或多种，所述第二添加剂占混合物的质量比为4.1-4.5份。
进一步的，所述混合物中包括第三添加剂，所述第三添加剂为聚羧酸铵盐溶液、聚丙烯酸铵盐与聚羧酸铵盐混合溶液、纯碱溶液、腐植酸钠溶液、鞣性减水剂、草酸钠溶液、聚偏磷酸钠溶液、焦磷酸钠溶液、丹宁酸钠溶液中的一种或多种，所述第三添加剂占混合物的质量比为2-4份。
进一步的，所述有机溶剂为醇、酮、芳族烃、脂肪族烃或氯代烃类中的一种或两种以上的混合物，亦或者，所述有机溶剂也可以为异丙醇、丙酮、甲基丁酮、甲基异丁酮、三氯乙烯、四氯乙烯，三乙醇胺、乙腈、吡啶、苯酚中的一种或多种。
进一步的，所述陶瓷粉末为氧化锆粉末、氮化硅粉末、碳化硅粉末，或者氮化硅粉末与碳化硅粉末的混合物。
进一步的，将所述线圈高温烧结过程中加入氧化物或非氧化物烧结助剂，所述氧化物或非氧化物烧结助剂包括:CuO、B2O3、ZrO2、CaO、La2O3、Li2CO3、TiO2、BaO、MnO、SiO2、Y2O3、Al2O3、MgO和CeO中的一种或多种，按重量份，所述第烧结助剂添加量为3-5份。
进一步的，将所述线材进行脱水的过程为：将所述线材在惰性气体保护下，使用微波间断加热，加热温度为100-300℃。可以是100℃、150℃、200℃、250℃或300℃等。
进一步的，将塑化后的线材缠绕成具有一定匝数的线圈，包括：将线材缠绕至芯棒上形成螺旋状线圈，将螺旋状线圈及芯棒放入烘干箱中，将所述线材进行惰性气体气氛间断式微波干燥。可以是110℃、120℃、130℃、140℃、150℃、160℃、170℃、190℃、200℃、等，惰性气体成分可以使用氦气，氖气，氩气一种或多种。
进一步优选的，芯棒与线圈的材质相同，所述芯棒的直径为2-10cm，可以是2cm、2.5cm、3cm、4cm、5cm、6cm、8cm或者10cm。
冷等静压成型过程为：将烘干后的螺旋线圈连同芯棒后，放入胶套中心，周围采用氮化硼、氮化硅，碳化硅，氧化铝粉末一种或多种填充。放置在冷等静压机中，压力为90-110MPa，时间为3-9min。
与现有技术相比，本发明一种陶瓷弹簧及制备方法和用于燃料电池密封的用途，具有以下突出的有益效果：
1、本发明陶瓷粉末、水与甲基纤维素，羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物中的至少一个混合，并在脱水的过程使线材长度收缩10-20％，弹簧坯体塑化后再次干燥、等静压收缩，避免干燥时直接完成收缩，收缩量与弹簧的塑形不匹配导致变形、开裂，有效降低因烧结时弹簧收缩导致陶瓷弹簧变形、开裂。
2、本发明回火处理，能够使得晶界玻璃相再次填充陶瓷颗粒间的间隙，消除点缺陷，增强陶瓷弹簧的机械强度和使用寿命。
3、本发明使用陶瓷弹簧作为中高温燃料电池压密封装置，其具有耐高温性能同时具备高回弹性，使中高温燃料电池升降温过程中，电池堆始终处于压密封状态。保证中高温燃料电池的正常运行，延长燃料电池使用寿命，避免了各种材料热膨胀系数不适配问题，同时成功解决了中高温燃料电池不断升降温带来的密封松弛问题。
附图说明
图1是本发明陶瓷弹簧的结构示意图。
具体实施方式
下面将结合附图和实施例，对本发明作进一步详细说明。
实施例1
一种陶瓷弹簧，由以下重量份原料制备而成，陶瓷粉末53.3-78份，水15-30份，羧甲基纤维素钠4.2-8.5份。其中，陶瓷粉末为氧化锆粉末、氮化硅粉末、碳化硅粉末，或者氮化硅粉末与碳化硅粉末的混合物
第一添加剂添加量为7.0-8.9份，第一添加剂为己基草酸，乙二醇聚氧乙烯醚、聚乙烯醇(PVA)，腐植酸钠、邻苯二甲酸二(2-乙基己)酯中一种或多种；
第二添加剂添加量为4.1-4.5份，第二添加剂为异丁醇、丙二醇或邻苯二甲酸二甲酯中的一种或多种
第三添加剂添加量为2-4份，第三添加剂为聚羧酸铵盐溶液、聚丙烯酸铵盐与聚羧酸铵盐混合溶液、纯碱溶液、腐植酸钠溶液、鞣性减水剂、草酸钠溶液、聚偏磷酸钠溶液、焦磷酸钠溶液、丹宁酸钠溶液中的一种或多种。
氧化物或非氧化物烧结助剂3-5份，氧化物或非氧化物烧结助剂，所述氧化物或非氧化物烧结助剂包括:CuO、B2O3、ZrO2、CaO、La2O3、Li2CO3、TiO2、BaO、MnO、SiO2、Y2O3、Al2O3、MgO和CeO中的一种或多种。
一种陶瓷弹簧的制备方法，包括以下步骤：
步骤(1)，按重量份将陶瓷粉末，水，羧甲基纤维素钠，第一添加剂，第二添加剂，第三添加剂，氧化物或非氧化物烧结助剂混合，得混合物；
步骤(2)通过捏合机捏合，将上述混合物充分搅拌均匀并形成具有一定塑性和可成型性的喂料。
步骤(3)然后将该喂料倒入挤出机进行第一次成型并生产出线径为0.6-3mm的线材。
步骤(4)将所述线材在惰性气体保护下，气氛为氩气，使用微波间断加热，加热温度为100-300℃，线材的陶瓷颗粒表面和颗粒间的水分挥发产生气孔，并在脱水的过程使线材长度收缩10-20％。
步骤(5)将脱水后的所述线材通过有机溶剂进行塑化，所述有机溶剂为醇、酮、芳族烃、脂肪族烃或氯代烃类中的一种或两种以上的混合物。亦或者，所述有机溶剂也可以为异丙醇、丙酮、甲基丁酮、甲基异丁酮、三氯乙烯、四氯乙烯，三乙醇胺、乙腈、吡啶、苯酚中的一种或多种。塑化时浸入有机溶剂的时间为50-150秒，当线材浸入有机溶剂，溶剂将通过产品表面气孔进入陶瓷产品，陶瓷颗粒表面和颗粒间的溶剂会使该线材有一定的塑性。有机溶剂也能使粘结剂软化，以此使陶瓷产品塑化。
步骤(6)然后将再次塑化后的线材通过绕簧机缠绕至平均直径为2-10cm的芯棒上形成具有一定匝数的线圈。集体为：包括：将线材缠绕至芯棒上形成螺旋状线圈，将螺旋状线圈及芯棒放入烘干箱中，并采用氮气气氛于100-200℃下进行惰性气体气氛间断式微波干燥。
然后冷等静压成型：将烘干后的螺旋线圈连同芯棒后，放入胶套中心，周围采用氮化硼、氮化硅，碳化硅，氧化铝粉末一种或多种填充，比如可以是【氧化铝及氮化硼粉末(比例1:2)填充】，放置在冷等静压机中，压力为90-110MPa，时间为3-9min，得到弹簧坯体。
步骤(7)将所述弹簧坯体依次进行烧结和回火处理后，即得，烧结和回火处理时将将螺旋状线圈及芯棒一同加热。其中，烧结温度为1400℃-1800℃，回火处理的温度不高于烧结温度。优选，回火处理在氮气气氛中低压低速升温烧结，根据原料不同选择烧结温度1200℃-1600℃，氮气压力为0.1-2MPa，升温速率为0.5-10℃/min。
步骤(8)将回火处理后的线圈进行后续加工(上下端打磨、表面处理)后得到陶瓷弹簧成品。
将线材缠绕至同材质的芯棒上，在排胶及烧结过程中实现芯棒与线圈的共同收缩，且芯棒提供支撑保证线圈不变形。
在平板式SOFC中，单电池集成为电池堆时，需要用连接体将其串联起来，同时需要对电池堆施加一定压力使其形成压密封状态，使用陶瓷弹簧作为燃料电池压密封装置，其具有耐高温性能同时具备高回弹性，使中高温燃料电池升降温过程中，电池队始终处于压密封状态。保证中高温燃料电池的正常运行。本实施例的陶瓷弹簧。可以应用于燃料电池密封领域，具体用于高温燃料电池的密封。使用陶瓷弹簧作为中高温燃料电池压密封装置，其具有耐高温性能同时具备高回弹性，使中高温燃料电池升降温过程中，电池堆始终处于压密封状态。保证中高温燃料电池的正常运行，延长燃料电池使用寿命，避免了各种材料热膨胀系数不适配问题，同时成功解决了中高温燃料电池不断升降温带来的密封松弛问题。
以上所述仅为本申请的较佳实施例，并不用以限制本申请，凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的保护范围之内。

Claims (3)

1.一种陶瓷弹簧的制备方法，其特征在于，用于高温燃料电池压密封装置，
制备工艺包括以下步骤：
一：将以下原料混合，得混合物，配比如下：
陶瓷粉末，所述陶瓷粉末为氧化锆粉末、氮化硅粉末、碳化硅粉末或者氮化硅粉末与碳化硅粉末的混合物，所述的陶瓷粉末添加量为53.3-78份；
水15-30份；
甲基纤维素、羧甲基纤维素钠、羟丙基甲基纤维素与聚乙烯醇缩丁醛的混合物4.2-8.5份；
第一添加剂，所述第一添加剂为己基草酸、乙二醇聚氧乙烯醚、腐殖酸钠、邻苯二甲酸二（2-乙基己酯）中的一种或多种，按重量份，所述第一添加剂添加量为7.0-8.9份；
第二添加剂，所述第二添加剂为异丁醇、丙二醇中的一种或多种，按重量份，所述第二添加剂添加量为4.1-4.5份；
第三添加剂，所述第三添加剂为纯碱溶液、腐殖酸钠溶液、鞣性减水剂、草酸钠溶液、聚偏磷酸钠溶液、单宁酸钠溶液中的一种或多种，按重量份，所述第三添加剂加为2-4份；
二：将所述混合物挤出成型为线材，线材直径为0.6-1mm或2-3mm；
三：将所述线材进行脱水，并在脱水过程使线材长度收缩10-20%；脱水过程为将线材在惰性气体保护下，使用微波间断加热，加热温度100-300摄氏度；
四：将脱水后的所述线材通过有机溶剂进行塑化，所述有机溶剂为芳族烃、脂肪族烃、氯代烃类中的一种或两种以上的混合物；
五：将塑化后的线材缠绕成具有一定匝数的线圈，包括将线材缠绕至芯棒上形成螺旋状线圈，将螺旋状线圈及芯棒放入烘干箱中，进行惰性气氛间断式微波干燥；
六：然后冷等静压成型得到弹簧坯体，冷等静压成型压力为90-110MPa，时间为3-9min，冷等静压成型过程为：将烘干后的螺旋线圈连同芯棒，放入胶套中心，周围采用氮化硼、氮化硅、碳化硅、氧化铝粉末中的一种或多种填充；
七：将所述弹簧坯体依次进行烧结和回火处理后即得，其中烧结温度为1400-1800℃；回火处理的温度不高于烧结温度，回火是在氮气气氛中低压低速升温烧结，依据原料不同选择烧结温度1200-1600℃，氮气压力0.1-2MPa，升温速率为0.5-10℃/min。
2.根据权利要求1所述的陶瓷弹簧的制备方法，其特征在于，制备陶瓷弹簧的原料还包括氧化物或非氧化物烧结助剂，所述氧化物或非氧化物烧结助剂包括：CuO、B2O3、ZrO2、La2O3、Li2CO3、BaO中的一种或多种，按重量份，所述氧化物或非氧化物烧结助剂添加量为3-5份。
3.一种陶瓷弹簧，其特征在于，采用权利要求1-2任意一种方法制备而得。
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