CN110423118A - 一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料 - Google Patents
一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料 Download PDFInfo
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Abstract
本发明公开了一种热膨胀系数小、气孔率低、热震稳定性和耐磨性好，抗铜渣及铝渣和化学气体渗透性能优异，整体性良好、使用寿命长的SiC/Si3N4复合陶瓷材料及其制备方法。本发明原始料由多晶硅切片废液经过沉淀后的废渣，经过烘干、磨细，1100‑1300℃氮化处理，加入一定量的SiC作为补充原料，添加复合添加剂、水，进行浇注，常温养护，加温烘烤（200—300℃）后得到。本发明不仅拉长了多晶硅工业的生产链，而且也解决了耐火材料在有色金属冶炼工业中发展的瓶颈问题，并易于大规模工业推广使用和产业化。
Description
技术领域
本发明涉及奥斯麦特铜冶炼炉铜溜槽或熔铝炉用耐火材料，尤其涉及一种奥斯麦特铜冶炼炉铜溜槽或熔铝炉用一种工业废料生产的SiC/Si3N4复合陶瓷相结合防渗耐磨材料以其制备方法。
背景技术
奥斯麦特炉是一种基于物料中硫化物、金属组分、氧化铁及氧之间的高强度熔池熔炼系统，其核心技术浸没式喷枪顶吹技术（TSL）。 近年来 TSL 炼铜工艺日趋完善成熟,由于其具有高效、设备简单、操作容易、原料适应性强并能满足严格的环保要求等显著优点, 现已成为世界上先进的熔池熔炼炼铜工艺之一。目前国内外在奥斯麦特炉出铜溜槽工作层普遍使用的是镁铬砖，这种砖砌体在使用中普遍存在几方面的缺点；使用寿命短，效果差，一般一个星期使用寿命，铜液渣和水份侵蚀严重，耐火材料损耗严重，费用高；整体性差，由于铬元素的存在，极度污染空气；后期维护劳动强度大，需要人员多，人工费用极高。
近年来，随着我国多晶硅行业的迅速增长，多晶硅生产的工业副产品也急剧增多，由于投入过大及处理技术不过关，目前大多企业对于其采用方法是简单处理后深埋，严重污染了企业周边的环境。因此，研究适合我国多晶硅生产固废物的综合利用方法，将多晶硅生产的固废物“无害化”、“资源化”，一方面解决了多晶硅生产的污染问题，另一方面也为多晶硅生产提供了一个降低成本的途径，对国家的环境保护及可持续发展有着积极的意义，具有一定经济及社会效益。
发明内容
本发明目的是为了克服铜溜槽及熔铝炉用防渗浇注料使用寿命技术问题存在的不足，利用多晶硅切片的废液沉淀物作为原料，经过氮化处理，从而提供了一种热膨胀系数小、气孔率低、热震稳定性和耐磨性好，抗铜渣及铝渣和化学气体渗透性能优异，整体性良好、使用寿命长的SiC/Si3N4复合陶瓷材料及其制备方法。
为了实现上述目的，本发明采用的技术方案为：
这种利用多晶硅工业废料生产的铜溜槽用复合陶瓷相防渗耐磨材料,所用主坯体材料由多晶硅切片废液经过沉淀后的废渣，经过烘干、磨细，1100-1300℃氮化处理，加入一定量的SiC作为补充原料，添加复合添加剂、水，进行浇注，常温养护，加温烘烤（200—300℃）后就得到这种SiC/Si3N4复合陶瓷材料复合陶瓷材料。
本发明原始料的加入重量份数为： 经过氮化处理的多晶硅切片废液沉淀后的废渣料20—27份，SiC 60—67份，结合剂12—16份，外加复合添加剂，复合添加剂加入量为原始料总重量的 12 — 16 %； 外加水，水加入量为原始料总重量的5—10%。
其中经过氮化处理的多晶硅切片废液沉淀后的废渣料其粒度分布在1—0mm、≤0.088mm；
其中SiC的粒度分布在 15—5mm、5—3mm、3—1mm的粒度区间。
其中所述结合剂为硅微粉和a- A12O3微粉中的一种或两种以及两种以上的混合。
其中所述硅微粉的SiO2含量大于92%，粒度小于5μm。
其中所述a- A12O3粉的粒度小于5μm ，A12O3含量大于98%。
加入这种结合剂的目的是硅微粉和a- A12O3微粉可以渗入到本发明的原料颗粒的缝隙中，达到依靠微粉的活性来促进材料坯体在较低温度下充分烧结，这是一种新型的活化烧结工艺；并且，有一些超微小粉粒渗入到后续工艺所生成的SiC与Si3N4交织的网状晶相结构的复合陶瓷相中，不仅粘附在陶瓷晶相体结构表面上，形成牢固的骨架作用，显著提高最终产品的强度；另外更是有一些超微小粉粒渗入陶瓷晶相烧结层的空隙中，起到二次防护的作用，从而提高足够防渗透和耐侵蚀性能。
所述的复合添加剂为羧甲基纤维素钠、聚丙烯酸钠、糊精中的一种或两种以及两种以上的组合。
本发明，一种利用多晶硅工业废料生产的铜溜槽用复合陶瓷相防渗耐磨材料的制备方法为：
步骤一、先把多晶硅工业废料沉淀物烘干，磨细后，放入氮化炉（N2气氛保护炉）在1100-1300℃保温24小时进行氮化处理，得到经过氮化处理的废渣料，氮化处理后的废渣料包括，氮化硅含量55-65%，碳化硅含量15-25%；
步骤二、取经过氮化处理的废渣料重量份数20—27份、 碳化硅原料重量份数60—67份、结合剂重量份数12—16份，放入强制搅拌机预混10-15min，将混合好的料加入水，水加入量为原始料总重量的5—10%，复合添加剂加入量为原始料总重量的12 — 16 %；继续搅拌5-10min，将原料制成混凝土浆体；
步骤三、采用振动减压成型的成型方式，即将制成的混凝土浆体注入事先组装好的模具内，进行高频振动和真空处理，除去气泡；
步骤四、湿法保温养护，温度不低于5℃，待凝固成型后脱模；
步骤五、将脱出的素坯放在温度不低于5℃的环境中继续湿法养护；
步骤六、养护后，进行干燥烘干，烘干温度常温—300℃，时间大于24小时；得到本发明铜溜槽用复合陶瓷相防渗材料。
众所周知，氮化硅是一种高温陶瓷材料，硬度大、熔点高、化学性质稳定， 工业上常常采用纯Si和纯N2在1300度制取得到。因此，氮化硅的市场售价是较高的；在步骤一中，多晶硅工业废料沉淀物中硅粉在氮化处理中，形成了氮化硅，为后续工艺形成SiC/Si3N4交织的网状晶相结构的复合陶瓷相,提供了廉价的氮化硅来源。
其中把多晶硅工业废料沉淀物烘干，再磨细后，粒度分布在1—0mm、≤0.088mm；这样的粒度可以增加物料的比表面积，提高氮化率，使废料中游离的Si能有效的氮化成α-Si3N4相以及少量β-Si3N4相，有效提高原料的体积密度和强度。
本发明创新地使用了多晶硅行业所产生的废液经过沉淀后的废渣料为主料，多晶硅工业废料沉淀物中硅粉在本发明的氮化处理中，形成氮化硅，再加入一定量的SiC作为补充原料，再经过振动减压成型，以及一些特殊的养护方法，使本发明形成了SiC与Si3N4交织的立体网状晶相结构的复合陶瓷相，
本发明的有益效果是：
本发明选取的主要原料为多晶硅工业处理的废料，变废为宝，成本及其低廉，并通过合理的组份，特殊的工艺，制备出了有色金属冶炼用的高质量，高性能的耐火材料，不仅拉长了多晶硅工业的生产链，而且也解决了耐火材料在有色金属冶炼工业中发展的瓶颈问题，并易于大规模工业推广使用和产业化。
众所周知，有色金属冶炼有以下特征：（1)冶炼温度一般都较低；（2)熔融金属或金属氧化物的流动性和浸透能力很强；（3)熔渣和熔融金属的侵蚀性很强；（4)炉内温度变化较大。因此，目前有色金属冶炼所用的耐火材料，使用寿命短，效果差，一般一个星期使用寿命，铜液渣和水份侵蚀严重，耐火材料损耗严重，费用高。本发明则通过选择合适复合添加剂和复合结合剂及控制加入量，选择合适的工艺路线和参数，通过优化工业废料和碳化硅原料的化学组成，利用原料高温线膨胀率低，热震稳定性高以及耐磨性高，高温体积稳定和防渗性优异的特性机理，解决了由于有色金属渣渗透性强使得耐火材料使用性能下降的矛盾。
本发明利用了活化烧结机制，达到了较低温烧成高强度防渗材料的目的，节能环保。
本发明中多晶硅废料的原料经过氮化处理，由于有氮化硅以及碳化硅作为主要成分，使其具备高强、防渗的性能。采用振动减压成型方式和特定的烧成工艺大大降低了制品的气孔率，提高了强度和制品的成品率以及质量稳定性，使制品具有使用温度高、寿命长、强度高、耐磨性强、热线膨胀率低、热震稳定性和抗渗透侵蚀优异等特性优点。
本发明利用合理的颗粒级配，所用各种原料和结合剂具有多种不同粒度区间，堆积密度大，产品强度高、耐磨性能好，使用寿命长，保证了此材料能长期在炼铜、铝冶炼环境中使用，满足了用户的使用要求。
本发明制成预制件，代替了传统的镁铬砖和浇注料，不仅与炉体结合更紧密，施工灵活，维修便捷，更是进一步提高了制品的强度和保温性以及制品的耐磨性和抗渗透侵蚀性能。
这种复合陶瓷材料制造方法简单易行，有利于产业化生产制造，并且保证了此材料能长期在有色冶炼环境中使用，满足了用户的使用要求。解决了有色冶炼炉长寿命、环保节能、高产稳产工艺的迫切需求，特别是解决了出渣口、溜槽等部位使用寿命低，环境污染严重，保温效果差的问题；大大延长了奥斯麦特炉和其他有色冶炼炉寿命，环保节能，符合国家产业环保政策，对我国有色行业的发展具有深远意义。将会在环保和经济领域发挥巨大潜能。本发明为高级耐磨防渗耐火材料，寿命高，施工维护非常便捷，大大降低劳动强度，改善冶炼环境污染，提高奥斯迈麦炉和其他有色冶炼炉的利用率，提高效益。
本产品利用活化烧结机制，通过选择合适复合添加剂并控制加入量，选择合适的工艺路线和参数，研制出强度高、保温性好、耐磨性强、热震稳定性和抗渗透侵蚀优异的高性能新型耐火材料的性能指标如下：
。
具体实施方式
下面结合实施例进一步说明本发明的方案。
实施例1
一种利用多晶硅工业废料生产的铜溜槽用复合陶瓷相防渗耐磨材料的制备方法为：
步骤一、先把多晶硅工业废料沉淀物烘干，磨细后，放入氮化炉（N2气氛保护炉）在1100℃保温24小时进行氮化处理，得到经过氮化处理的废渣料，氮化处理后的废渣料包括，氮化硅含量55%，碳化硅含量15%；
步骤二、取经过氮化处理的废渣料重量份数20份、 碳化硅原料重量份数67份、结合剂重量份数13份，放入强制搅拌机预混10-15min，将混合好的料加入水，水加入量为原始料总重量的5%，复合添加剂加入量为原始料总重量的16 %；继续搅拌5-10min，将原料制成混凝土浆体；
步骤三、采用振动减压成型的成型方式，即将制成的混凝土浆体注入事先组装好的模具内，进行高频振动和真空处理，除去气泡；
步骤四、湿法保温养护，温度不低于5℃，待凝固成型后脱模；
步骤五、将脱出的素坯放在温度不低于5℃的环境中继续湿法养护；
步骤六、养护后，进行干燥烘干，烘干温度为常温，时间28小时；得到本发明铜溜槽用复合陶瓷相防渗材料。
本实施例的主要性能指标
实施例2
一种利用多晶硅工业废料生产的铜溜槽用复合陶瓷相防渗耐磨材料的制备方法为：
步骤一、先把多晶硅工业废料沉淀物烘干，磨细后，放入氮化炉（N2气氛保护炉）在1300℃保温24小时进行氮化处理，得到经过氮化处理的废渣料，氮化处理后的废渣料包括，氮化硅含量65%，碳化硅含量20%；
步骤二、取经过氮化处理的废渣料重量份数22份、 碳化硅原料重量份数66份、结合剂重量份数12份，放入强制搅拌机预混10-15min，将混合好的料加入水，水加入量为原始料总重量的8%，复合添加剂加入量为原始料总重量的12 %；继续搅拌5-10min，将原料制成混凝土浆体；
步骤三、采用振动减压成型的成型方式，即将制成的混凝土浆体注入事先组装好的模具内，进行高频振动和真空处理，除去气泡；
步骤四、湿法保温养护，温度不低于5℃，待凝固成型后脱模；
步骤五、将脱出的素坯放在温度不低于5℃的环境中继续湿法养护；
步骤六、养护后，进行干燥烘干，烘干温度300℃，时间26小时；得到本发明铜溜槽用复合陶瓷相防渗材料。
主要的性能指标
实施例3
一种利用多晶硅工业废料生产的铜溜槽用复合陶瓷相防渗耐磨材料的制备方法为：
步骤一、先把多晶硅工业废料沉淀物烘干，磨细后，放入氮化炉（N2气氛保护炉）在1100-1300℃保温24小时进行氮化处理，得到经过氮化处理的废渣料，氮化处理后的废渣料包括，氮化硅含量55-65%，碳化硅含量15-25%；
步骤二、取经过氮化处理的废渣料重量份数24份、 碳化硅原料重量份数60份、结合剂重量份数16份，放入强制搅拌机预混10-15min，将混合好的料加入水，水加入量为原始料总重量的10%，复合添加剂加入量为原始料总重量的16 %；继续搅拌5-10min，将原料制成混凝土浆体；
步骤三、采用振动减压成型的成型方式，即将制成的混凝土浆体注入事先组装好的模具内，进行高频振动和真空处理，除去气泡；
步骤四、湿法保温养护，温度不低于5℃，待凝固成型后脱模；
步骤五、将脱出的素坯放在温度不低于5℃的环境中继续湿法养护；
步骤六、养护后，进行干燥烘干，烘干温度200℃，时间30小时；得到本发明铜溜槽用复合陶瓷相防渗材料。
主要的性能指标
Claims (6)
1.一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料，其特征在于：原始料的加入重量份数为： 经过氮化处理的多晶硅切片废液沉淀后的废渣料20—27份，SiC 60—67份，结合剂12—16份，外加复合添加剂，复合添加剂加入量为原始料总重量的 12 — 16%； 外加水，水加入量为原始料总重量的5—10%。
2.根据权利要求1所述的一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料，其特征在于：经过氮化处理的多晶硅切片废液沉淀后的废渣料其粒度分布在1—0mm、≤0.088mm。
3.根据权利要求1所述的一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料，其特征在于：结合剂为硅微粉和a- A12O3微粉中的一种或两种以及两种以上的混合。
4.根据权利要求1所述的一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料，其特征在于：硅微粉的SiO2含量大于92%，粒度小于5μm。
5.根据权利要求1所述的一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料，其特征在于： a- A12O3粉的粒度小于5μm ，A12O3含量大于98%。
6.根据权利要求1所述的一种用多晶硅废料生产的铜溜槽用复合陶瓷相防渗耐磨材料的制备方法，其特征在于：步骤一、先把多晶硅工业废料沉淀物烘干，磨细后，放入氮化炉在1100-1300℃保温24小时进行氮化处理，得到经过氮化处理的废渣料，氮化处理后的废渣料包括，氮化硅含量55-65%，碳化硅含量15-25%；步骤二、取经过氮化处理的废渣料重量份数20—27份、 碳化硅原料重量份数60—67份、结合剂重量份数12—16份，放入强制搅拌机预混10-15min，将混合好的料加入水，水加入量为原始料总重量的5—10%，复合添加剂加入量为原始料总重量的12 — 16 %；继续搅拌5-10min，将原料制成混凝土浆体；步骤三、采用振动减压成型的成型方式，即将制成的混凝土浆体注入事先组装好的模具内，进行高频振动和真空处理，除去气泡；步骤四、湿法保温养护，温度不低于5℃，待凝固成型后脱模；步骤五、将脱出的素坯放在温度不低于5℃的环境中继续湿法养护；步骤六、养护后，进行干燥烘干，烘干温度常温—300℃，时间大于24小时；得到本发明铜溜槽用复合陶瓷相防渗材料。
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