CN107140996B - 一种碳化硅-石墨升液管及制备方法 - Google Patents

一种碳化硅-石墨升液管及制备方法 Download PDF

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CN107140996B
CN107140996B CN201710347258.2A CN201710347258A CN107140996B CN 107140996 B CN107140996 B CN 107140996B CN 201710347258 A CN201710347258 A CN 201710347258A CN 107140996 B CN107140996 B CN 107140996B
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钱凡
李红霞
杨文刚
黄辉
于建宾
马天飞
刘国齐
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

本发明属于耐火材料技术领域，主要涉及一种碳化硅‑石墨升液管及制备方法。其特征在于：将碳化硅、石墨两种低膨胀性且难烧结的材料利用酚醛树脂粉结合剂，糠醛作为溶剂，并引入金属硅、碳化硼、硼玻璃粉，在高速混料器中混炼，并控制坯料合适的挥发份，在液压机中高压成型，氮气氛炉内热处理制成。该升液管的主要特点是热震性能好，高致密(显气孔率3%以下），可以有效满足低压铸造行业对升液管的使用要求，可代替目前使用普遍的铸造效率低的铸铁升液管，以及氮化硅结合碳化硅或钛酸铝材质等高性能但造价昂贵的升液管。

Description

一种碳化硅-石墨升液管及制备方法
技术领域
本发明属于耐火材料技术领域，主要涉及一种碳化硅-石墨升液管及其制备方法。
背景技术
低压铸造升液管是低压铸造机上的关键部件之一，工作时铝熔液( 温度700~900℃) 每隔3~5min从升液管内被压送到模具型腔。这种工况要求该部件具有耐高温、抗热震、与金属熔液不润湿、良好的气密性和长期的抗热冲击疲劳性等性能。目前，国内铸铝用升液管主要是铸铁升液管，而铁在铝熔液中的渗熔，会极大地降低铸铝件的质量。国外多采用陶瓷质升液管，如日本多采用Si3N4反应结合SiC陶瓷升液管，具有使用寿命长、耐侵蚀、不污染铝液等优点，而极大地提高铸铝产品的质量和生产效率，但由于Si3N4 反应结合SiC陶瓷升液管生产成本高，价格昂贵，在我国推广较困难。同时，国内外开发出了钛酸铝陶瓷质的升液管，正常情况下该材质升液管可连续运行60天以上。钛酸铝陶瓷不仅具有较高的熔点(1860℃)、较低的热膨胀系数(α≤2.0×10-6)和优良的抗热震性，且具有与铝等许多有色金属熔体不润湿的特性, 成为制备铸铝用升液管材质之一。但钛酸铝在750~1300℃之间易于分解为α-Al2O3和金红石型TiO2，导致材料力学和抗热震性能降低，制品破坏。
发明内容
本发明目的是提供一种碳化硅-石墨升液管及其制备方法，使其能代替目前普遍应用的陶瓷质升液管例如氮化硅结合碳化硅和钛酸铝陶瓷升液管。
本发明为完成上述目的采用如下技术方案：
一种碳化硅-石墨升液管，所述升液管的原料包括有主相材料和基质部份；所述的主相材料为碳化硅和石墨，所述的基质部份为金属硅粉、碳化硼和硼玻璃粉；升液管的原料组成及质量百分比为：
碳化硅：30%~40%； 粒度 2~1mm，
10%~20% 1~0mm，；
石墨： 15%~25%； 595#，
金属硅粉：5%~10% ≤1000目，
碳化硼：5%~10% ≤1000目，
硼玻璃粉：10%~20% ≤1000目；
所述的升液管还外加有作为结合剂的酚醛树脂粉和作为溶剂的糠醛，酚醛树脂粉和糠醛加入量分别为上述原料总重量的3%~6%、4%~7%；酚醛树脂粉，固含量≥80%，游离酚≤8%硼玻璃粉的成分为：钾长石25%～30%；叶蜡石12%～17% ；硼砂47%～53%；硅石5%～11%，将上述物料装入振动球磨罐中进行充分混合，混磨时间5~15h，混合细粉的粒度≤1000目。
利用所述的一种碳化硅-石墨升液管进行制备的方法，其特征在于：先将钾长石、叶蜡石、硼砂、硅石按比例加入振动球磨灌中进入预混获得硼玻璃粉，然后将碳化硅、石墨、金属硅粉、硼玻璃粉、酚醛树脂粉按照比例加入到高速造粒机混料罐中，高速旋转10~30min；然后将糠醛加入高速造粒机混料罐中继续高速混炼10~20min，再低速混炼5min出料；坯料须进行料过筛，筛子孔径尺寸<3mm；将坯料干燥后并控制挥发份后装入升液管压制模具中在等静压机中液压成型，成型的坯体在氮气氛下进行热处理，形成了碳化硅-石墨高抗热震高致密性升液管。
物料挥发份控制在0.8%~1.2%。
物料烘拷温度≤70℃。
成型压力不低于100MP，保压时间≥2min。热处理温度950℃~1250℃，升温速度1℃/分 ，保温时间5h；热处理气氛为氮气，氮气纯度≥99.9999%，炉内氮气压力≥0.1MPa；保温时间结束后，在600℃以上控制炉内降温速率≤1℃/分。
升液管的成型方式为等静压，液压介质为油或是水，成型用胶套材质为聚氨酯或是人造橡胶。
本发明提出的一种碳化硅-石墨升液管及其制备方法，利用低膨胀性原料碳化硅、石墨作为所制备升液管的主相材料，同时热处理后的结合相为树脂残碳，因而热震性能好。为了满足升液管的气密性要求，必须先获取高致密性生坯，而酚醛树脂粉是极好的塑性结合剂，通过控制合适的加入量和控制合适的挥发份，在高压下生坯气孔率可以控制在2%以下；在热处理过程中，无法通过烧结来降低材料气孔率，同时，所采用的结合剂是有机物，会有一部份烧失，造成了气孔率的提高，我们采用能够促进酚醛树脂残碳的糠醛作为溶剂，糠醛在混料器中可以与酚醛树脂反应，增加了其支链，进而获得较高的残碳，从而获得高致密熟坯；为了进一步提高材料的抗氧化性和致密性，还需适当添加金属硅粉、硼玻璃粉；因为上述超细粉，会在树脂碳化完成后的温度范围内呈现熔融状态能够填充其间隙，从而提高材料的致密度；该方法制备的升液管不但可以满足铸造过程中的热震条件和气密性要求（显气孔率3%以下），并且成本较低，可以大面积推广，具有很好的经济效益。
具体实施方式
实施例1
碳化硅和石墨为主要原料，其中粒度2~1mm碳化硅：30%，粒度1~0mm碳化硅20%，石墨含量18%，并添6%金属硅粉，6%碳化硼，20%硼玻璃粉（硼玻璃制备方法：钾长石25%、叶蜡石15% 、硼砂50%、硅石10%，在振动球磨罐中预混10h，料球比例：1:2）。固态树脂粉作为结合剂，溶剂为糠醛，加入量分别为上述原料总量的4%和5%，经高速混料机混练，60℃烘干后得到坯料挥发份0.9%，并于MPa等静压成型，最后在氮气氛保护处理炉中进行热处理，N2含量大于99.999vol%，以1℃/min升温至950℃，保温300min以1℃/min降温至600℃。热处理后材料的显气孔率为2.6%，材料的常高温强度分别18MPa和14MPa。1100℃水冷热震4次后残余强度为10MPa。
实施例2
碳化硅和石墨为主要原料，其中粒度2~1mm碳化硅：33%，粒度1~0mm碳化硅20%，石墨含量15%，并添6%金属硅粉，10%碳化硼，16%硼玻璃粉（硼玻璃制备方法：钾长石30%、叶蜡石10% 、硼砂50%、硅石10%，在振动球磨罐中预混10h，料球比例：1:2）。固态树脂粉作为结合剂，溶剂为糠醛，加入量分别为上述原料总量的3%和4%，经高速混料机混练，65℃烘干后得到坯料挥发份0.8%，并于120MPa等静压成型，最后在氮气氛保护处理炉中进行热处理，N2含量大于99.999vol%，以1℃/min升温至1150℃，保温300min以1℃/min降温至600℃。热处理后材料的显气孔率为2.5%，材料的常高温强度分别20MPa和13MPa。1100℃水冷热震4次后残余强度为7.4MPa。
实施例3
碳化硅和石墨为主要原料，其中粒度2~1mm碳化硅：33%，粒度1~0mm碳化硅10%，石墨含量25%，并添6%金属硅粉，10%碳化硼，16%硼玻璃粉（硼玻璃制备方法：钾长石26%、叶蜡石17% 、硼砂52%、硅石5%，在振动球磨罐中预混10h，料球比例：1:2）。固态树脂粉作为结合剂，溶剂为糠醛，加入量分别为上述原料总量的6%和7%，经高速混料机混练，70℃烘干后得到坯料挥发份1.2%，并于120MPa等静压成型，最后在氮气氛保护处理炉中进行热处理，N2含量大于99.999vol%，以1℃/min升温至1150℃，保温300min以1℃/min降温至600℃。热处理后材料的显气孔率为2.0%，材料的常高温强度分别23MPa和12MPa。1100℃水冷热震4次后残余强度为8.6MPa。
实施例4
碳化硅和石墨为主要原料，其中粒度2~1mm碳化硅：40%，粒度1~0mm碳化硅15%，石墨含量20%，并添6%金属硅粉，7%碳化硼，12%硼玻璃粉（硼玻璃制备方法：钾长石22%、叶蜡石15% 、硼砂53%、硅石10%，在振动球磨罐中预混10h，料球比例：1:2）。固态树脂粉作为结合剂，溶剂为糠醛，加入量分别为上述原料总量的5%和6%，经高速混料机混练，65℃烘干后得到坯料挥发份1.0%，并于120MPa等静压成型，最后在氮气氛保护处理炉中进行热处理，N2含量大于99.999vol%，以1℃/min升温至1150℃，保温300min以1℃/min降温至600℃。热处理后材料的显气孔率为2.1%，材料的常高温强度分别20MPa和13MPa。1100℃水冷热震4次后残余强度为7MPa。

Claims (3)

1.一种碳化硅-石墨升液管的制备方法，其特征在于：升液管的原料包括有主相材料和基质部份；所述的主相材料为碳化硅和石墨，所述的基质部份为金属硅粉、碳化硼和硼玻璃粉；升液管的主相材料和基质组成及质量百分比为：
碳化硅：30%~40%； 粒度 2~1mm，
10%~20% 1~0mm；
石墨：15%~25%； 595#，
金属硅粉：5%~10% ≤1000目，
碳化硼：5%~10% ≤1000目，
硼玻璃粉：10%~20% ≤1000目；
所述的升液管还外加有作为结合剂的酚醛树脂粉和作为溶剂的糠醛，酚醛树脂粉和糠醛加入量分别为上述原料总重量的3%~6%、4%~7%；酚醛树脂粉，固含量≥80%，游离酚≤8%；硼玻璃粉的成分为：钾长石25%～30%；叶蜡石12%～17% ；硼砂47%～53%；硅石5%～11%，将上述物料装入振动球磨罐中进行充分混合，混磨时间5~15h，混合细粉的粒度≤1000目；制备方法的具体步骤如下：先将钾长石、叶蜡石、硼砂、硅石按比例加入振动球磨灌中进入预混获得硼玻璃粉，然后将碳化硅、石墨、金属硅粉、硼玻璃粉、酚醛树脂粉按照比例加入到高速混料器中进行预混，然后将糠醛加入高速混料器中进行湿混得到坯料，将坯料干燥后并控制挥发份后装入升液管压制模具中在等静压机中液压成型，成型的坯体在氮气氛下进行热处理，形成了碳化硅-石墨高抗热震高致密性升液管。
2.如权利要求1所述的一种碳化硅-石墨升液管的制备方法，其特征在于：物料挥发份控制在0.8%~1.2%。
3.如权利要求1所述的一种碳化硅-石墨升液管的制备方法，其特征在于：成型压力不低于100MP，保压时间≥2min， 热处理温度950℃~1250℃，升温速度1℃/分，保温时间5h，热处理气氛为氮气，氮气纯度≥99.9999%，炉内氮气压力≥0.1MPa， 保温时间结束后，在600℃以上控制炉内降温速率≤1℃/分。
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