CN113896516B - 一种石英陶瓷辊的制备方法 - Google Patents

一种石英陶瓷辊的制备方法 Download PDF

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CN113896516B
CN113896516B CN202111315617.9A CN202111315617A CN113896516B CN 113896516 B CN113896516 B CN 113896516B CN 202111315617 A CN202111315617 A CN 202111315617A CN 113896516 B CN113896516 B CN 113896516B
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吕金虎
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Lianyungang Sunlight Quartz Ceramics Co ltd
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Abstract

本发明属于石英陶瓷领域,具体实际一种石英陶瓷辊的制备方法,包括:将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液;将混合料加入至粘稠液中恒温超声2‑5h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;将预制品形成初步烧结3‑5h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品;将镀膜预烧品静置20‑30min,然后升温烘干,烧结30‑40h,逐步降温得到毛坯料,经打磨得到成品。本发明制得的石英陶瓷辊道具有高密度,高强度,低膨胀系数,表面光滑细腻等优点。

Description

一种石英陶瓷辊的制备方法
技术领域
本发明属于石英陶瓷领域,具体实际一种石英陶瓷辊的制备方法。
背景技术
石英陶瓷是以熔融石英为原料,具有热膨胀系数小、热稳定性好、电绝缘性好、耐化学侵蚀性好等特点,广泛用于陶瓷辊、陶瓷平板、陶瓷闸板砖、铸钢用水口、冲头、坩埚、炉体、搅拌棒、料盆、旋转管、焦炉炉门等产品。目前的石英陶瓷产品的工艺较为复杂,且成本较高,同时产品极易因冷热均匀度不佳,造成应力裂纹与缺陷。
发明内容
针对现有技术中的问题,本发明提供一种石英陶瓷辊的制备方法,制得的石英陶瓷辊道具有高密度,高强度,低膨胀系数,表面光滑细腻等优点。
为实现以上技术目的,本发明的技术方案是:
一种石英陶瓷辊的制备方法,包括如下步骤:
步骤1,将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;所述混合料的质量配比如下:熔融石英粉40-70份、纳米氧化铝20-30份、氢氧化铝细粉10-15份,所述熔融石英粉由2-10μm石英粉和20-30微米石英粉组成,且两者的质量比为2:4-7;所述搅拌速度为500-1500r/min,进一步的,所述搅拌采用湿法搅拌,且溶剂采用无水乙醇或无水乙醚,搅拌结束后过滤并90-100℃烘干;
步骤2,将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液,所述聚乙烯醇、聚乙二醇、硅胶、乙醇水溶液的质量配比为1:1:2-3:4-7,所述乙醇水溶液中的乙醇的体积占比为30-40%;低温超声的温度为20-40℃,超声频率为50-80kHz;
步骤3,将混合料加入至粘稠液中恒温超声2-5h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;所述混合料与粘稠液的质量比为10-15:3,恒温超声的温度为80-90℃,超声频率为70-80kHz,所述浇铸成型采用边浇铸边震动的方法,且浇铸的温度为100-110℃,直至表面呈半干状态,所述加压的压力为100-120MPa,温度为100-120℃,时间为20-30h,晾干采用自然晾干,时间为20-30h;
步骤4,将预制品形成初步烧结3-5h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品,所述初步烧结的温度为300-400℃,升温速度为10-30℃/min,所述三氯甲基硅烷乙醚液中的三氯甲基硅烷浓度为100-150g/L,超声浸泡的温度为10-20℃,超声频率为50-80kHz,所述烘干温度为40-50℃;
步骤5,将镀膜预烧品静置20-30min,然后升温烘干,烧结30-40h,逐步降温得到毛坯料,经打磨得到成品,所述静置环境为水蒸气与氮气的混合氛围,且水蒸气的体积占比为10-12%,温度为60-80℃,所述升温烘干的温度为200-400℃,时间为2-5h,所述烧结温度为1150-1200℃。
进一步的,氢氧化铝自身属于耐热剂,在高温极易形成氧化铝,且在氧化铝转变过程中,自身材料的脆性会形成一定的变化,不仅造成内部结构的孔隙增大,而且会增加陶瓷的内部脆性,为解决这一问题,所述氢氧化铝细粉采用包裹型氢氧化铝,且所述包裹型氢氧化铝细粉的制备方法,包括如下步骤:a1,将乙烯基三乙氧基硅烷加入至乙醚中溶解,然后缓慢加入乙基纤维素搅拌均匀,形成粘稠液;所述乙烯基三乙氧基硅烷与乙醚的质量比为10:13-17,所述乙基纤维素的加入量是乙烯基三乙氧基硅烷的200-400%;a2,将粘稠液造粒烘干得到粘稠半干细粉,造粒烘干的温度为50-70℃;a3,将异丙醇铝加入至异丙醇内搅拌均匀,然后喷雾沉降至粘稠半干细粉表面,得到镀膜细粉;所述异丙醇铝与异丙醇的质量比为4:2-3,所述喷雾沉降的温度为80-90℃;此时的喷雾将异丙醇与异丙醇铝分离开,此时异丙醇铝自身沉降并沉积在粘稠半干细粉表面,基于细粉的粘稠性与半干特性,异丙醇铝沉降在细粉表面且不会向内渗透,达到良好的包覆效果;a4,将镀膜细粉静置20-30min,恒温烘干得到包裹型氢氧化铝细粉,所述静置环境为水蒸气与氮气混合气体,且水蒸气的体积占比为5-8%,所述烘干温度为80-90℃;该方法利用乙烯基三乙氧基硅烷的粘稠液态特性,配合乙基纤维素自身的固体常态形成粘稠半干的细粉颗粒,同时利用气态沉降将异丙醇铝形成表面包裹沉降,达到表面包裹效果,半干且粘稠的细粉不会被异丙醇铝细粉渗透,即,异丙醇铝只能够形成表面包裹的效果,当异丙醇铝转化为氢氧化铝时,整个颗粒转化为氢氧化铝包裹状态。在使用过程中,随着稳定的升高,氢氧化铝受热转化为活性氧化铝,同时表面形成自身的介孔结构,该介孔结构的内侧形成表面活性羟基,与受热状态的乙烯基三乙氧基硅烷形成键连效果,达到内部连接性,保证了内部的氧化铝内部收到硅氧框架的支撑与连接,解决了氧化铝转变过程中的脆化问题,保证整个产品的内部稳定性。与此同时,后续的超声浸泡过程中,三氯甲基硅烷通过预烧品表面的缝隙进入内部,与活性氧化铝和乙烯基三乙氧基硅烷形成连接,并在静置过程中形成内部的硅烷网络结构,确保缝隙内的稳定框架结构,大大提升了稳定性。
进一步的,所述硅胶采用复合硅胶,具体采用纳米胶基硅胶,常规硅胶一般采用含水硅酸凝胶固定化得到,内部具有良好的多孔性,自身机械性变差,针对这一问题,将纳米胶结合至硅胶内,形成复合硅胶体系,利用纳米胶自身直径在200nm以下的三维网状聚合物,能够将孔隙封堵化,减少内部孔穴,且自身的化学键连接,提升了硅胶的稳定性;所述纳米胶基硅胶的制备方法,包括:b1,将将硅胶颗粒加入至无水乙醇中超声清洗,并恒温烘干得到洁净的硅胶颗粒,所述超声清洗的温度为10-20℃,超声频率为50-70kHz,恒温烘干的温度为150-180℃;b2,将硅胶颗粒放入反应釜中,通入氯化氢气体静置20-30min,得到活化硅胶颗粒,所述反应釜内的氛围为水蒸气占比为3-5%的空气氛围,所述氯化氢的通入速度为5-10mL/min;b3,将纳米胶加入至无水乙醚中搅拌均匀得到悬浊液,然后将悬浊液喷淋至活化硅胶颗粒表面,经烘干与振荡筛滤得到纳米胶基硅胶颗粒,所述纳米胶与无水乙醚的质量比为1:10-14,所述喷淋速度为10-30mL/min,所述喷淋中的活化硅胶颗粒放置在反应釜中段,确保喷淋液完全渗透至底部排出,所述烘干温度为30-50℃;在该步骤中,纳米胶在无水乙醚中形成溶解,并在喷淋处理过程中充分渗透至硅胶颗粒多孔内,纳米胶受到吸附性的作用,停留在硅胶颗粒内;b4,将纳米级硅胶颗粒放置到反应釜内静置1-2h,然后取出烘干,反复2-10次,得到纳米胶基硅胶。纳米胶能够对硅胶自身的结构多孔性形成补助效果,同时,纳米胶遇水膨胀过程中形成向外延伸,并与聚乙烯醇和聚乙二醇形成连接,达到稳定的共粘体系;硅胶本身属于硅氧结构,能够与石英等材料形成同质互连,大大提升陶瓷辊的自身结构特点。
从以上描述可以看出,本发明具备以下优点:
1.本发明解决了现有石英陶瓷辊的缺陷,利用三氯甲基硅烷作为填补液形成硅氧支撑体系,减少应力裂纹与缺陷,提升了产品质量。
2.本发明利用氢氧化铝转化为活性氧化铝,配合高温条件下的洋槐,转化为硅酸铝,结构更为稳固。
3.本发明利用酸钠氯甲基硅烷配合不同粒径的石英粉和硅胶,形成稳定的硅氧体系,同时缝隙内的硅氧框架支撑,有效的提升了石英陶瓷的力学强度。
4.本发明利用不同粒径的石英粉来减少陶瓷孔隙,提升致密性,配合三氯甲基硅烷的缝隙填补,减少整体的孔隙,提高致密性,且表面包裹有硅氧结构,保证表面的光滑细腻,径向跳动小;于此同时可以调整石英陶瓷的密度来调整介电常数性能。
5.本发明利用氧化铝作为填充材料,能够在内部形成热量的局部均匀散布,减少局部温度的影响。
具体实施方式
结合实施例详细说明本发明的一个具体实施例,但不对本发明的权利要求做任何限定。
实施例1
一种石英陶瓷辊的制备方法,包括如下步骤:
步骤1,将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;所述混合料的质量配比如下:熔融石英粉40份、纳米氧化铝20份、氢氧化铝细粉10份,所述熔融石英粉由2-10μm石英粉和20-30微米石英粉组成,且两者的质量比为1:2;所述搅拌速度为500r/min,进一步的,所述搅拌采用湿法搅拌,且溶剂采用无水乙醇,搅拌结束后过滤并90℃烘干;
步骤2,将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液,所述聚乙烯醇、聚乙二醇、硅胶、乙醇水溶液的质量配比为1:1:2:4,所述乙醇水溶液中的乙醇的体积占比为30%;低温超声的温度为20℃,超声频率为50kHz;
步骤3,将混合料加入至粘稠液中恒温超声2h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;所述混合料与粘稠液的质量比为10:3,恒温超声的温度为80℃,超声频率为70kHz,所述浇铸成型采用边浇铸边震动的方法,且浇铸的温度为100℃,直至表面呈半干状态,所述加压的压力为100MPa,温度为100℃,时间为20h,晾干采用自然晾干,时间为20h;
步骤4,将预制品形成初步烧结3h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品,所述初步烧结的温度为300℃,升温速度为10℃/min,所述三氯甲基硅烷乙醚液中的三氯甲基硅烷浓度为100g/L,超声浸泡的温度为10℃,超声频率为50kHz,所述烘干温度为40℃;
步骤5,将镀膜预烧品静置20min,然后升温烘干,烧结30h,逐步降温得到毛坯料,经打磨得到成品,所述静置环境为水蒸气与氮气的混合氛围,且水蒸气的体积占比为10%,温度为60℃,所述升温烘干的温度为200℃,时间为2h,所述烧结温度为1150℃。
其中,所述氢氧化铝细粉采用包裹型氢氧化铝,且所述包裹型氢氧化铝细粉的制备方法,包括如下步骤:a1,将乙烯基三乙氧基硅烷加入至乙醚中溶解,然后缓慢加入乙基纤维素搅拌均匀,形成粘稠液;所述乙烯基三乙氧基硅烷与乙醚的质量比为10:13,所述乙基纤维素的加入量是乙烯基三乙氧基硅烷的200%;a2,将粘稠液造粒烘干得到粘稠半干细粉,造粒烘干的温度为50℃;a3,将异丙醇铝加入至异丙醇内搅拌均匀,然后喷雾沉降至粘稠半干细粉表面,得到镀膜细粉;所述异丙醇铝与异丙醇的质量比为4:2,所述喷雾沉降的温度为80℃;a4,将镀膜细粉静置20min,恒温烘干得到包裹型氢氧化铝细粉,所述静置环境为水蒸气与氮气混合气体,且水蒸气的体积占比为5%,所述烘干温度为80℃。
其中,所述硅胶采用纳米胶基硅胶,所述纳米胶基硅胶的制备方法,包括:b1,将将硅胶颗粒加入至无水乙醇中超声清洗,并恒温烘干得到洁净的硅胶颗粒,所述超声清洗的温度为10℃,超声频率为50kHz,恒温烘干的温度为150℃;b2,将硅胶颗粒放入反应釜中,通入氯化氢气体静置20min,得到活化硅胶颗粒,所述反应釜内的氛围为水蒸气占比为3-5%的空气氛围,所述氯化氢的通入速度为5mL/min;b3,将纳米胶加入至无水乙醚中搅拌均匀得到悬浊液,然后将悬浊液喷淋至活化硅胶颗粒表面,经烘干与振荡筛滤得到纳米胶基硅胶颗粒,所述纳米胶与无水乙醚的质量比为1:10,所述喷淋速度为10mL/min,所述喷淋中的活化硅胶颗粒放置在反应釜中段,确保喷淋液完全渗透至底部排出,所述烘干温度为30℃;b4,将纳米级硅胶颗粒放置到反应釜内静置1h,然后取出烘干,反复2次,得到纳米胶基硅胶。
本实施例制备的石英陶瓷辊,直径公差为±0.5mm,径向跳动±0.08mm,摩擦系数为0.5,介电常数为2.33(1kHz),热膨胀系数为0.65×10-6/℃,常温耐压强度为118.1MPa,常温抗折强度为37.4MPa,体积密度为2.08g/cm3
实施例2
一种石英陶瓷辊的制备方法,包括如下步骤:
步骤1,将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;所述混合料的质量配比如下:熔融石英粉70份、纳米氧化铝30份、氢氧化铝细粉15份,所述熔融石英粉由2-10μm石英粉和30微米石英粉组成,且两者的质量比为2:7;所述搅拌速度为1500r/min,进一步的,所述搅拌采用湿法搅拌,且溶剂采用无水乙醚,搅拌结束后过滤并100℃烘干;
步骤2,将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液,所述聚乙烯醇、聚乙二醇、硅胶、乙醇水溶液的质量配比为1:1:3:7,所述乙醇水溶液中的乙醇的体积占比为40%;低温超声的温度为40℃,超声频率为80kHz;
步骤3,将混合料加入至粘稠液中恒温超声5h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;所述混合料与粘稠液的质量比为5:1,恒温超声的温度为90℃,超声频率为80kHz,所述浇铸成型采用边浇铸边震动的方法,且浇铸的温度为110℃,直至表面呈半干状态,所述加压的压力为120MPa,温度为120℃,时间为30h,晾干采用自然晾干,时间为30h;
步骤4,将预制品形成初步烧结5h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品,所述初步烧结的温度为400℃,升温速度为30℃/min,所述三氯甲基硅烷乙醚液中的三氯甲基硅烷浓度为150g/L,超声浸泡的温度为20℃,超声频率为80kHz,所述烘干温度为50℃;
步骤5,将镀膜预烧品静置30min,然后升温烘干,烧结40h,逐步降温得到毛坯料,经打磨得到成品,所述静置环境为水蒸气与氮气的混合氛围,且水蒸气的体积占比为12%,温度为80℃,所述升温烘干的温度为400℃,时间为5h,所述烧结温度为1200℃。
其中,所述氢氧化铝细粉采用包裹型氢氧化铝,且所述包裹型氢氧化铝细粉的制备方法,包括如下步骤:a1,将乙烯基三乙氧基硅烷加入至乙醚中溶解,然后缓慢加入乙基纤维素搅拌均匀,形成粘稠液;所述乙烯基三乙氧基硅烷与乙醚的质量比为10:17,所述乙基纤维素的加入量是乙烯基三乙氧基硅烷的400%;a2,将粘稠液造粒烘干得到粘稠半干细粉,造粒烘干的温度为70℃;a3,将异丙醇铝加入至异丙醇内搅拌均匀,然后喷雾沉降至粘稠半干细粉表面,得到镀膜细粉;所述异丙醇铝与异丙醇的质量比为4:3,所述喷雾沉降的温度为90℃;a4,将镀膜细粉静置30min,恒温烘干得到包裹型氢氧化铝细粉,所述静置环境为水蒸气与氮气混合气体,且水蒸气的体积占比为8%,所述烘干温度为90℃。
其中,所述硅胶采用纳米胶基硅胶,所述纳米胶基硅胶的制备方法,包括:b1,将将硅胶颗粒加入至无水乙醇中超声清洗,并恒温烘干得到洁净的硅胶颗粒,所述超声清洗的温度为20℃,超声频率为70kHz,恒温烘干的温度为180℃;b2,将硅胶颗粒放入反应釜中,通入氯化氢气体静置30min,得到活化硅胶颗粒,所述反应釜内的氛围为水蒸气占比为5%的空气氛围,所述氯化氢的通入速度为10mL/min;b3,将纳米胶加入至无水乙醚中搅拌均匀得到悬浊液,然后将悬浊液喷淋至活化硅胶颗粒表面,经烘干与振荡筛滤得到纳米胶基硅胶颗粒,所述纳米胶与无水乙醚的质量比为1:14,所述喷淋速度为30mL/min,所述喷淋中的活化硅胶颗粒放置在反应釜中段,确保喷淋液完全渗透至底部排出,所述烘干温度为50℃;b4,将纳米级硅胶颗粒放置到反应釜内静置2h,然后取出烘干,反复10次,得到纳米胶基硅胶。
本实施例制备的石英陶瓷辊,直径公差为±0.5mm,径向跳动±0.06mm,摩擦系数为0.6,介电常数为2.31(1kHz),热膨胀系数为0.63×10-6/℃,常温耐压强度为118.9MPa,常温抗折强度为37.6MPa,体积密度为2.10g/cm3
实施例3
一种石英陶瓷辊的制备方法,包括如下步骤:
步骤1,将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;所述混合料的质量配比如下:熔融石英粉60份、纳米氧化铝25份、氢氧化铝细粉12份,所述熔融石英粉由2-10μm石英粉和20-30微米石英粉组成,且两者的质量比为2:5;所述搅拌速度为1000r/min,进一步的,所述搅拌采用湿法搅拌,且溶剂采用无水乙醇,搅拌结束后过滤并95℃烘干;
步骤2,将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液,所述聚乙烯醇、聚乙二醇、硅胶、乙醇水溶液的质量配比为1:1:3:6,所述乙醇水溶液中的乙醇的体积占比为35%;低温超声的温度为30℃,超声频率为70kHz;
步骤3,将混合料加入至粘稠液中恒温超声4h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;所述混合料与粘稠液的质量比为13:3,恒温超声的温度为85℃,超声频率为75kHz,所述浇铸成型采用边浇铸边震动的方法,且浇铸的温度为105℃,直至表面呈半干状态,所述加压的压力为110MPa,温度为110℃,时间为25h,晾干采用自然晾干,时间为25h;
步骤4,将预制品形成初步烧结4h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品,所述初步烧结的温度为350℃,升温速度为20℃/min,所述三氯甲基硅烷乙醚液中的三氯甲基硅烷浓度为130g/L,超声浸泡的温度为15℃,超声频率为70kHz,所述烘干温度为45℃;
步骤5,将镀膜预烧品静置25min,然后升温烘干,烧结35h,逐步降温得到毛坯料,经打磨得到成品,所述静置环境为水蒸气与氮气的混合氛围,且水蒸气的体积占比为11%,温度为70℃,所述升温烘干的温度为300℃,时间为4h,所述烧结温度为1200℃。
其中,所述氢氧化铝细粉采用包裹型氢氧化铝,且所述包裹型氢氧化铝细粉的制备方法,包括如下步骤:a1,将乙烯基三乙氧基硅烷加入至乙醚中溶解,然后缓慢加入乙基纤维素搅拌均匀,形成粘稠液;所述乙烯基三乙氧基硅烷与乙醚的质量比为10:16,所述乙基纤维素的加入量是乙烯基三乙氧基硅烷的300%;a2,将粘稠液造粒烘干得到粘稠半干细粉,造粒烘干的温度为60℃;a3,将异丙醇铝加入至异丙醇内搅拌均匀,然后喷雾沉降至粘稠半干细粉表面,得到镀膜细粉;所述异丙醇铝与异丙醇的质量比为4:3,所述喷雾沉降的温度为85℃;a4,将镀膜细粉静置25min,恒温烘干得到包裹型氢氧化铝细粉,所述静置环境为水蒸气与氮气混合气体,且水蒸气的体积占比为7%,所述烘干温度为85℃。
其中,所述硅胶采用纳米胶基硅胶,所述纳米胶基硅胶的制备方法,包括:b1,将将硅胶颗粒加入至无水乙醇中超声清洗,并恒温烘干得到洁净的硅胶颗粒,所述超声清洗的温度为15℃,超声频率为60kHz,恒温烘干的温度为170℃;b2,将硅胶颗粒放入反应釜中,通入氯化氢气体静置20-30min,得到活化硅胶颗粒,所述反应釜内的氛围为水蒸气占比为4%的空气氛围,所述氯化氢的通入速度为8mL/min;b3,将纳米胶加入至无水乙醚中搅拌均匀得到悬浊液,然后将悬浊液喷淋至活化硅胶颗粒表面,经烘干与振荡筛滤得到纳米胶基硅胶颗粒,所述纳米胶与无水乙醚的质量比为1:12,所述喷淋速度为20mL/min,所述喷淋中的活化硅胶颗粒放置在反应釜中段,确保喷淋液完全渗透至底部排出,所述烘干温度为40℃;b4,将纳米级硅胶颗粒放置到反应釜内静置2h,然后取出烘干,反复8次,得到纳米胶基硅胶。
本实施例制备的石英陶瓷辊,直径公差为±0.4mm,径向跳动±0.07mm,摩擦系数为0.5,介电常数为2.32(1kHz),热膨胀系数为0.65×10-6/℃,常温耐压强度为118.0MPa,常温抗折强度为37.5MPa,体积密度为2.09g/cm3
可以理解的是,以上关于本发明的具体描述,仅用于说明本发明而并非受限于本发明实施例所描述的技术方案。本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换,以达到相同的技术效果;只要满足使用需要,都在本发明的保护范围之内。

Claims (9)

1.一种石英陶瓷辊的制备方法,其特征在于:包括如下步骤:
步骤1,将不同粒径的熔融石英粉、纳米氧化铝、氢氧化铝细粉颗粒加入至搅拌机中搅拌均匀,形成混合料;
步骤2,将聚乙烯醇、聚乙二醇、硅胶加入至乙醇水溶液中,低温超声至完全分散,得到粘稠液;
步骤3,将混合料加入至粘稠液中恒温超声2-5h,然后放入模具中浇铸成型并加压,脱模晾干得到预制品;
步骤4,将预制品形成初步烧结3-5h,得到预烧品,然后超声浸泡至三氯甲基硅烷乙醚液中,取出烘干得到镀膜预烧品;
步骤5,将镀膜预烧品静置20-30min,然后升温烘干,烧结30-40h,逐步降温得到毛坯料,经打磨得到成品;
所述步骤1中的混合料的质量配比如下:熔融石英粉40-70份、纳米氧化铝20-30份、氢氧化铝细粉10-15份;
所述氢氧化铝细粉采用包裹型氢氧化铝,且所述包裹型氢氧化铝细粉的制备方法,包括如下步骤:a1,将乙烯基三乙氧基硅烷加入至乙醚中溶解,然后缓慢加入乙基纤维素搅拌均匀,形成粘稠液;所述乙烯基三乙氧基硅烷与乙醚的质量比为10:13-17,所述乙基纤维素的加入量是乙烯基三乙氧基硅烷的200-400%;a2,将粘稠液造粒烘干得到粘稠半干细粉,造粒烘干的温度为50-70℃;a3,将异丙醇铝加入至异丙醇内搅拌均匀,然后喷雾沉降至粘稠半干细粉表面,得到镀膜细粉;所述异丙醇铝与异丙醇的质量比为4:2-3,所述喷雾沉降的温度为80-90℃;a4,将镀膜细粉静置20-30min,恒温烘干得到包裹型氢氧化铝细粉,所述静置环境为水蒸气与氮气混合气体,且水蒸气的体积占比为5-8%,所述烘干温度为80-90℃。
2.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述熔融石英粉由2-10μm石英粉和20-30微米石英粉组成,且两者的质量比为2:4-7。
3.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述搅拌速度为500-1500r/min,所述搅拌采用湿法搅拌,且溶剂采用无水乙醇或无水乙醚,搅拌结束后过滤并90-100℃烘干。
4.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤2中的聚乙烯醇、聚乙二醇、硅胶、乙醇水溶液的质量配比为1:1:2-3:4-7,所述乙醇水溶液中的乙醇的体积占比为30-40%;低温超声的温度为20-40℃,超声频率为50-80kHz。
5.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤3中的混合料与粘稠液的质量比为10-15:3,恒温超声的温度为80-90℃,超声频率为70-80kHz,所述浇铸成型采用边浇铸边震动的方法,且浇铸的温度为100-110℃,直至表面呈半干状态,所述加压的压力为100-120MPa,温度为100-120℃,时间为20-30h,晾干采用自然晾干,时间为20-30h。
6.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤4中的初步烧结的温度为300-400℃,升温速度为10-30℃/min。
7.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤4中的三氯甲基硅烷乙醚液中的三氯甲基硅烷浓度为100-150g/L,超声浸泡的温度为10-20℃,超声频率为50-80kHz,所述烘干温度为40-50℃。
8.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤5中的静置环境为水蒸气与氮气的混合氛围,且水蒸气的体积占比为10-12%,温度为60-80℃。
9.根据权利要求1所述的石英陶瓷辊的制备方法,其特征在于:所述步骤5中的升温烘干的温度为200-400℃,时间为2-5h,所述烧结温度为1150-1200℃。
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