CN113307633B - 一种快速烧结多孔陶瓷的制备方法 - Google Patents

一种快速烧结多孔陶瓷的制备方法 Download PDF

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CN113307633B
CN113307633B CN202110766610.2A CN202110766610A CN113307633B CN 113307633 B CN113307633 B CN 113307633B CN 202110766610 A CN202110766610 A CN 202110766610A CN 113307633 B CN113307633 B CN 113307633B
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mixture
porous ceramic
firing
temperature
heating
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CN113307633A (zh
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王成
杨建荣
王子超
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Hangzhou Taofeilun New Material Co ltd
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Abstract

本发明公开了一种快速烧结多孔陶瓷的制备方法，包括步骤一：称取陶瓷主料及粘合剂等添加剂，混合均匀形成混合物；步骤二：处理步骤一所得混合物形成固体混合物或浆料；步骤三：将步骤二所得固体混合物或浆料填入模腔，通过干粉压制或浇注成型形成坯体；步骤四：对步骤三所得坯体进行烧制，设置烧制气压为10‑3～105Pa，温度低于1000℃，制得多孔陶瓷。通过在多孔陶瓷制备工艺中的烧制工艺设置气压条件10‑3～105Pa，使烧制工艺在低于1000℃温度条件下4h内完成，缩短烧制周期的同时保证甚至提高多孔陶瓷的抗弯强度、抑制主料氧化。

Description

一种快速烧结多孔陶瓷的制备方法
技术领域
本发明属于多孔陶瓷技术领域，具体涉及一种快速烧结多孔陶瓷的制备方法。
背景技术
多孔陶瓷材料是以刚玉砂、碳化硅等原料为主料，经过成型和特殊高温烧结工艺制备的一种具有开孔孔径、高开口气孔率的多孔性陶瓷材料。多孔性陶瓷材料具有耐高温高压性，抗酸碱和有机介质腐蚀性，良好生物惰性，可控的孔结构和孔隙率，使用寿命长，产品可再生等优点。通常通过挤压成型法、发泡法、浸渍法、溶胶凝胶法、3D增材打印等方法制备，广泛应用于金属熔炼滤渣网、环保处理过滤器载体、复合材料、耐火材料等领域。
多孔陶瓷制备工艺中的烧制工艺，其机理是促使固、液相烧结以满足必要的机械强度，通常需要采用不低于1200℃的高温，在常压或正压条件下烧制，且烧制周期较长(如专利CN112778020A、CN111763097A)。但在高温高压条件下，用于多孔陶瓷成型的粘合剂等添加剂，其升华、蒸发、裂解、气化等脱离过程受阻，影响脱脂排胶进程，严重时导致坯体胀裂。本发明通过优化工艺条件、优选添加剂，有效缩短烧制周期并保证产品开气孔率和抗弯强度。
发明内容
本发明的目的在于提供一种快速烧结多孔陶瓷的制备方法，采用负压烧制，选用高温粘合剂和低温粘合剂混合的粘合剂，在缩短烧制周期的同时保证甚至提高多孔陶瓷的机械强度。
本发明的目的通过以下技术方案实现：一种快速烧结多孔陶瓷的制备方法，包括以下步骤：
步骤一：称取陶瓷主料及添加剂，混合均匀形成混合物；
步骤二：处理步骤一所得混合物制成固体混合物或浆料；
步骤三：将步骤二所得固体混合物或浆料填入模腔，通过干粉压制或浇注成型形成坯体；
步骤四：对步骤三所得坯体进行烧制，设置气压值为10-3～105Pa，烧制温度低于1000℃，制得多孔陶瓷。
优选的，所述步骤一陶瓷主料碳化硅、刚玉砂、氧化锆、碳化硼、氧化铝、氮化硅、金刚石中的一种或多种；所述添加剂包括低温粘合剂和高温粘合剂，所述低温粘合剂为石蜡、聚乙烯醇、乳化石蜡、蜂糖胶、硅胶、木质素磺酸钠中的一种或多种；所述高温粘合剂为硅树脂249、硅玻璃粉、磷酸二氢铝、冰晶石、低温熔盐中的一种或多种。
优选的，所述步骤二中的固体混合物通过分样筛或喷雾干燥制粒，并控制水分范围为≤2.0wt％后再进行步骤三。
优选的，所述步骤三中的浆料浇筑成型后脱模取坯，60～90℃干燥坯体5～7h。
优选的，所述步骤四中烧制温度在100～350℃进行脱脂，150～650℃进行排胶，700～980℃烧结成型；烧制过程时间小于4h。
优选的，所述步骤四中在气压2×10-3～4×104Pa进行脱脂，4×10-3～7×104Pa进行排胶，1×10-3～9×104Pa烧结成型。
优选的，所述步骤四中在气压1×10-2～9×103Pa进行脱脂，3×10-2～6×10Pa进行排胶，2×10-3～6×10Pa烧结成型。
与现有技术相比，本发明的有益效果在于：
1)本发明通过设置多孔陶瓷制备工艺中的烧制工艺气压条件为负压10-3～105Pa，促进粘合剂等添加剂的升华、蒸发、裂解、气化等脱离过程，促进脱脂排胶进程，使烧制工艺在低于1000℃温度条件下完成，且烧制时间不超过4h。
2)本发明通过优选粘合剂为低温粘合剂和高温粘合剂的混合物，促进多孔陶瓷主料间的粘合作用，降低烧制工艺条件要求，使之在负压10-3～105Pa、低于1000℃，烧制不超过4h即可烧制成型。
3)本发明负压烧制所得多孔陶瓷产品，能保持抗弯强度高于2MPa，甚至提高抗弯强度，为常压压制产品的1.2～2倍；并能够抑制易氧化陶瓷主料(如碳化硼、碳化硅)的氧化过程，使氧化产物由约50％将至约0.01％。
附图说明
图1为实施例1步骤四中烧制工艺温度、气压曲线；
图2为实施例3步骤四中烧制工艺温度、气压曲线；
图3为实施例4步骤四中烧制工艺温度、气压曲线。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步的说明。
实施例1
步骤一：称取1000g粒径D50为5μm的碳化硅，并加入85g全精炼石蜡、50g磷酸二氢铝，形成混合物；
步骤二：将步骤一所得混合物加热至石蜡形成液态，与碳化硅颗粒、磷酸二氢铝充分混合均匀，再冷却至石蜡形成固态，形成块状固体混合物；将块状固体混合物通过60目分样筛造粒，制得造粒粉；
步骤三：将步骤二所得造粒粉填入模腔，干粉压制，压力55kgf/cm2，坯体尺寸100mm×100mm×20mm；
步骤四：对步骤三所得坯体进行烧制，烧制过程温度曲线(如图1所示)：从室温以升温速度4.5℃/min，升温50min至240℃，恒温保持20min；再以升温速度11℃/min，升温30min至460℃，恒温保持20min；再以升温速度12℃/min，升温40min至940℃，恒温保持20min；最后随炉冷却至室温；
窑炉进气口、出气口设置气压控制阀，通过调节气体(空气、氧气、氩气、氮气或二氧化碳)调节气压，负压曲线(一个标准大气压为1.013×105Pa)(如图1所示)：从0min开始炉内气压2×104Pa恒定压力保持50min；烧制时间第50min至第70min将气压稳步调至4×104Pa，恒定压力保持30min；烧制时间第100min至第120min将气压稳步调至7×104Pa，恒定压力保持40min；烧制时间第160min至第180min将气压稳步调至9×104Pa；保持气压直至温度降至200℃以下；制得碳化硅多孔陶瓷。
负压烧制碳化硅多孔陶瓷性能检测结果如下：
名称 体积分数(％) 抗弯强度(MPa) 开气孔率(％)
样1 54.3 2.9 95.4
样2 54.6 2.8 95.6
样3 54.4 3.0 95.3
对比例1
与实施例1的区别在于：
步骤一：称取1000g粒径D50为5μm的碳化硅，并加入100g聚乙烯醇(有效固含量10％)，30g柠檬酸钠，10g润滑剂(洛阳烨方YF-125，其有效固含量为40％)形成混合物；
步骤二：向步骤一所得的混合物中加入适量去离子水，用搅拌机搅拌至充分均匀，采用喷雾造粒的方式制备碳化硅微型粉体，过20目分样筛，并控制水分控制0.3％～1.0％之间，制得造粒粉；
负压烧制碳化硅多孔陶瓷性能检测结果如下：
名称 体积分数(％) 抗弯强度(MPa) 开气孔率(％)
样1' 53.9 2.4 94.3
样2' 53.1 2.4 95.1
样3' 53.5 2.3 94.8
对比例2
与对比例1的区别在于：
步骤四：对步骤三所得坯体进行烧制，烧制过程常压，温度曲线：从室温以升温速度2℃/min，升温165min至350℃，恒温保持100min，进行脱脂；再以升温速度3℃/min，升温100min至650℃，恒温保持30min，进行排胶；再以升温速度4℃/min，升温150min至1250℃，恒温保持120min；再以升温速度2℃/min，升温180min至1780℃，恒温保持180min，再以6℃/min，降温100min至1200℃恒温20min，随炉冷大概720min至100℃以内，烧结成型，制得碳化硅细颗粒重结晶多孔陶瓷。
常压烧制碳化硅多孔陶瓷性能检测结果如下：
名称 体积分数(％) 抗弯强度(MPa) 开气孔率(％)
样4’ 51.2 1.8 83.2
样5’ 51.4 2.0 82.8
样6’ 51.0 1.5 82.6
实施例2
步骤一：称取1000g粒径D50为120μm的刚玉砂陶瓷原料，并加入350g聚乙烯醇(PVA)1788水溶液(其有效固含量为10％)，65g硼玻璃粉(粒径为20μm)，50g聚乙二醇(其有效固含量为20％)，10g润滑剂(洛阳烨方YF-125，其有效固含量为40％)，形成混合物；
步骤二：向步骤一所得的混合物中加入适量去离子水，用搅拌机搅拌至充分均匀形成浆料；再置于设定温度为70℃的电阻丝干燥箱内，干燥4h，形成固体混合物；将固体混合物用50目分样筛造粒，并置于密闭容器水分均化处理，控制水分范围为0.3％～2.0％；
步骤三：将步骤二所得造粒粉填入模腔内，干粉压制，压力55kgf/cm2，坯体尺寸100mm×100mm×20mm；
步骤四：对步骤四所得坯体进行烧制，烧制过程温度曲线：从室温以升温速度5.5℃/min，升温40min至240℃，恒温保持20min；再以升温速度8.8℃/min，升温25min至460℃，恒温保持20min；再以升温速度10.5℃/min，升温40min至880℃，恒温保持20min；最后随炉冷却至室温；
窑炉进气口、出气口设置气压控制阀，通过调节气体(空气、氧气、氩气、氮气或二氧化碳)调节气压，气压曲线：从0min开始炉内气压2×103Pa恒定压力保持40min；烧制时间第40min至第60min将气压稳步调至4×103Pa，恒定压力保持25min；烧制时间第85min至第105min将气压稳步调至7×103Pa，恒定压力保持40min；烧制时间第145min至第165min将气压稳步调至1×104Pa；保持气压直至温度降低于150℃以下，回至常压；制得刚玉砂多孔陶瓷。
负压烧制刚玉砂多孔陶瓷性能检测结果如下：
名称 体积分数(％) 抗弯强度(MPa) 开气孔率(％)
样4 51.3 2.6 98.0
样5 51.2 2.4 98.2
样6 51.2 2.6 98.0
对比例3
与实施例2的区别在于所述步骤四：对步骤三所得坯体进行烧制，烧制过程温度曲线：从室温以升温速度2℃/min，升温110min至240℃，恒温保持80min；再以升温速度4℃/min，升温55min至460℃，恒温保持40min；再以升温速度3℃/min，升温140min至880℃，恒温保持60min；最后随炉冷却至室温，制得刚玉砂多孔陶瓷。
常压烧制刚玉砂多孔陶瓷性能检测结果如下：
名称 体积分数(％) 抗弯强度(MPa) 开气孔率(％)
样7' 49.6 1.9 95.3
样8' 50.2 2.0 94.9
样9' 50.1 2.0 95.0
实施例3
步骤一：称取150g粒径D50为100μm的碳化硼(碳化硼含量为90％)，50g粒径D50为20μm的碳化硼(碳化硼含量为90％)，并加入31.58g蜂糖胶(有效固含量38％)，8g磷酸二氢铝(浓度40％)，1.2g柠檬酸钠，形成混合物；
步骤二：向步骤一所得的混合物中加入适量蒸馏水，用搅拌机搅拌至充分均匀，再室温真空度10Pa抽真空处理60min形成浆料；
步骤三：将步骤二所得浆料导入石膏模腔内浇注成型，脱模取坯，60～90℃干燥坯体5～7h，坯体尺寸
Figure BDA0003151937440000051
步骤四：对步骤三所得坯体进行烧制，采用真空炉烧制，烧制过程温度曲线(如图2所示)：从室温以升温速度10℃/min，升温36min至350℃，恒温保持30min；再以升温速度6℃/min，升温50min至650℃，恒温保持20min；再以升温速度6℃/min，升温45min至920℃，恒温保持30min；最后随炉冷却至室温，制得碳化硼多孔陶瓷。
气压曲线(如图2所示)，真空度为10-3～103Pa，在气压2×102～2×10Pa进行脱脂，10-1～6×10Pa进行排胶，10-2～6×10-2Pa烧结成型。
负压烧制碳化硼多孔陶瓷性能检测结果如下：
Figure BDA0003151937440000061
实施例4
与实施例3的区别在于：
步骤四：对步骤三所得坯体进行烧制，采用真空炉烧制，烧制过程温度曲线(如图3所示)：从室温以升温速度6.5℃/min，升温50min至350℃，恒温保持20min；再以升温速度5℃/min，升温60min至650℃，恒温保持20min；再以升温速度6℃/min，升温45min至920℃，恒温保持30min；最后随炉冷却至室温。
气压曲线(如图3所示)：升温之前，炉内抽真空保持气压低于5×10-3Pa，第0min，充氩气气压调整至1×103Pa，恒定压力至第50min，烧制时间从第50min至第70min，将气压稳步调整至10Pa，恒定气压至第130min，烧制时间从第130min至第150min，将气压稳步调整至3×10-2Pa，恒压至烧制结束(温度100℃以内)，制得碳化硼多孔陶瓷。
负压烧制碳化硼多孔陶瓷性能检测结果如下：
Figure BDA0003151937440000062
对比例4
与实施例3的区别在于：
步骤四：对步骤三所得坯体进行烧制，烧制过程为常压。
常压烧制碳化硼多孔陶瓷性能检测结果如下：
Figure BDA0003151937440000063
Figure BDA0003151937440000071
以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (1)

1.一种快速烧结多孔陶瓷的制备方法，其特征在于，包括以下步骤：
步骤一：称取150 g粒径D50为100 μm的碳化硼，50 g粒径D50为20 μm的碳化硼，并加入31.58 g蜂糖胶，8 g磷酸二氢铝，1.2 g柠檬酸钠，形成混合物；其中碳化硼含量为90%，蜂糖胶的有效固含量为38%，磷酸二氢铝的浓度为40%；
步骤二：向步骤一所得的混合物中加入适量蒸馏水，用搅拌机搅拌至充分均匀，再室温真空度10 Pa抽真空处理60 min形成浆料；
步骤三：将步骤二所得浆料导入石膏模腔内浇注成型，脱模取坯，60~90℃干燥坯体5~7h，坯体尺寸φ40 mm×30 mm；
步骤四：对步骤三所得坯体进行烧制，采用真空炉烧制，烧制过程温度曲线：从室温以升温速度10 ℃/min，升温36 min至350 ℃，恒温保持30 min；再以升温速度6 ℃/min，升温50 min至650 ℃，恒温保持20 min；再以升温速度6 ℃/min，升温45 min至920 ℃，恒温保持30 min；最后随炉冷却至室温，制得碳化硼多孔陶瓷；
气压曲线，真空度为10-3~103 Pa，在气压2×102 ~2×10Pa进行脱脂，10-1 ~6×10 Pa进行排胶，10-2 ~6×10-2 Pa烧结成型。
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