CN114773042A - 一种石英陶瓷的制备工艺 - Google Patents

一种石英陶瓷的制备工艺 Download PDF

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CN114773042A
CN114773042A CN202210292951.5A CN202210292951A CN114773042A CN 114773042 A CN114773042 A CN 114773042A CN 202210292951 A CN202210292951 A CN 202210292951A CN 114773042 A CN114773042 A CN 114773042A
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quartz
temperature
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梁文华
蔡喜来
张琳悦
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Comrolla Co ltd
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Abstract

本发明公开了一种石英陶瓷的制备工艺,由以下重量份的组分制备而成:硅微粉80~110份、碳酸钡10~15份、二硼化钛7~16份、氮化铝12~15份、氮化硼11~13份、氧化锆1~5份、氮化硅4~8份、陶瓷粉3~8份、碳化硅5~8份、碳酸氢钠1~4份、三氧化二锑2~5份、结合剂2~7份、加强纤维丝3~8份、石英涂层3~8份。本发明在陶瓷产品的表面缠绕连接了由玻璃纤维和石墨纤维组成的加强纤维丝,且在加强纤维丝的内外侧分别涂刷石英涂层,加强耐磨性能和抗腐蚀性能,进一步加强对石英陶瓷表面的保护能力,在石英陶瓷产品破碎后加强纤维丝会对碎片起到粘连的效果,避免碎片飞出,同时还方便对碎片进行收集。

Description

一种石英陶瓷的制备工艺
技术领域
本发明涉及石英陶瓷制备技术领域,更具体为一种石英陶瓷的制备工艺。
背景技术
熔融石英陶瓷是一种以熔融石英为原料,采用陶瓷生产工艺制成的熔融石英材料,熔融石英陶瓷的制备方法有许多,注凝成型由于其近净尺寸生产、可成型复杂形状的制品,已经成为了制备复杂陶瓷制品的新途径,具体工艺过程主要分为料浆制备、固化脱模、干燥排胶、烧结制品四个部分,烧结制品时需要对烧结后的产品进行检验和喷淋清洗。
目前,现有的石英陶瓷产品在使用过程中容易发生碎裂的现象,石英陶瓷产品碎裂后形成多个小碎块,碎块飞出后易对人员造成伤害,同时还不便于对碎块进行清理。为此,需要设计一个新的方案给予改进。
发明内容
本发明的目的在于提供一种石英陶瓷的制备工艺,解决了背景技术中所提出的问题,满足实际使用需求。
为实现上述目的,本发明提供如下技术方案:一种石英陶瓷的制备工艺,由以下重量份的组分制备而成:
硅微粉80~110份、碳酸钡10~15份、二硼化钛7~16份、氮化铝12~15份、氮化硼11~13份、氧化锆1~5份、氮化硅4~8份、陶瓷粉3~8份、碳化硅5~8份、碳酸氢钠1~4份、三氧化二锑2~5份、结合剂2~7份、加强纤维丝3~8份、石英涂层3~8份。
作为本发明的一种优选实施方式,包括如下步骤:
(1)制备加强纤维丝:以玻璃纤维和碳纤维做为原料,将碳纤维以微波聚焦方式对其进行超快速高温石墨化制程,以每min加热速度10~100℃将碳纤维温度提高到石墨化温度1400~3000℃,并在0.5~10min内进行快速石墨化制程,形成具有高模数特性的石墨纤维,在玻璃纤维表面涂刷粘合剂,并将其与石墨纤维缠绕粘合,制成加强纤维丝;
(2)石英涂层:熔融石英、低温石英、氮化硅、硅、氢氧化钡、氧化锆和粘结剂置于混料机中进行混合10~40min,制成石英涂层;
(3)制备石英硅微粉:
选取高纯度硅粉浸入研磨液,将浸液后的硅粉送到研磨机进行研磨,控制研磨机的进料和出料速度均衡,保持研磨时间为2~4h;
经第一级研磨机研磨后的粉体送至纳米级超细磨机进行研磨,研磨时间为2~5h,研磨后送振动筛进行筛分,粒度低于1.5微米的出料送入高速搅拌机;
将超细熔融石英硅微粉送入高速搅拌机,调高速搅拌机的转速为750~900转/分,搅拌时间以硅微粉自然升温至95℃时,此时将配方量的活性液送入高速搅拌机,继续高速搅拌30~60min,使活性液与硅微粉充分混合,当温度达到150℃时,停止搅拌,让其自然降温至常温,得到石英硅微粉;
(4)制备石英陶瓷:
S1:按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑,加入高压均质机中混合均匀,充分球磨,得到混合料,并置入反应釜;
S2:将惰性气体充入反应釜,反应釜中加入结合剂,搅拌15~20min后,升温至120~150℃,保温反应40~60min;
S3:将步骤(S2)的在烘箱内先进行低温干燥,低温干燥温度设为25~30℃,干燥时间设为2~3h;然后进行高温干燥,高温干燥温度设为120~140℃,空气湿度设为25~35%RH,干燥时间设为4.5~5.5h;
S4:将步骤(S3)中干燥后的胚体置于煅烧炉内进行煅烧,煅烧炉内先采用升温速率为2℃/min的升温速率缓慢升至350℃,然后采用升温速率为20~30℃/min的升温速率进行快速升温,升温至1100~1200℃时,在此温度下烧结1.5~2.5h,再采用45~50℃/min的降温速率进行快速降温,并降温至室温,待冷却后即可得到石英陶瓷胚
S5:在石英陶瓷表面涂刷石英涂层,放入烘干机中烘干2~2.5h,温度设为150~170℃,将加强纤维丝均匀的缠绕在石英陶瓷的表面,缠绕完成后在石英陶瓷及加强纤维丝的表面再涂刷一层石英涂层,放入烘干机中烘干2~2.5h,温度设为150~170℃,待其冷却即可得到石英陶瓷产品。
作为本发明的一种优选实施方式,所述结合剂由1:0.6:0.8的乙酸乙酯、水性树脂聚丙烯酰胺、聚乙二醇组成。
作为本发明的一种优选实施方式,所述加强纤维丝呈丝线状,且缠绕在石英陶瓷表面的加强纤维丝为整根不间断,其直径为30μm。
作为本发明的一种优选实施方式,所述石英涂层的厚度为300~400μm。
作为本发明的一种优选实施方式,所述步骤(2)中的熔融石英、低温石英、氮化硅比例为0.12~2:0.05~0.5:0.08~0.5,氢氧化钡质量含量为10~1000ppm,氧化锆质量含量为10~1000ppm。
与现有技术相比,本发明的有益效果如下:
本发明,在陶瓷产品的表面缠绕连接了由玻璃纤维和石墨纤维组成的加强纤维丝,且在加强纤维丝的内外侧分别涂刷石英涂层,加强耐磨性能和抗腐蚀性能,进一步加强对石英陶瓷表面的保护能力,在石英陶瓷产品破碎后加强纤维丝会对碎片起到粘连的效果,避免碎片飞出,同时还方便对碎片进行收集。
具体实施方式
下面将结合本发明的实施例对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一
一种石英陶瓷的制备工艺,由以下重量份的组分制备而成:
硅微粉85份、碳酸钡13份、二硼化钛12份、氮化铝13份、氮化硼12份、氧化锆4份、氮化硅6份、陶瓷粉6份、碳化硅6份、碳酸氢钠2份、三氧化二锑3份、结合剂3份、加强纤维丝6份、石英涂层4份。
进一步改进地,包括如下步骤:
(1)制备加强纤维丝:以玻璃纤维和碳纤维做为原料,将碳纤维以微波聚焦方式对其进行超快速高温石墨化制程,以每min加热速度60℃将碳纤维温度提高到石墨化温度1800℃,并在7min内进行快速石墨化制程,形成具有高模数特性的石墨纤维,在玻璃纤维表面涂刷粘合剂,并将其与石墨纤维缠绕粘合,制成加强纤维丝;
(2)石英涂层:熔融石英、低温石英、氮化硅、硅、氢氧化钡、氧化锆和粘结剂置于混料机中进行混合25min,制成石英涂层;
(3)制备石英硅微粉:
选取高纯度硅粉浸入研磨液,将浸液后的硅粉送到研磨机进行研磨,控制研磨机的进料和出料速度均衡,保持研磨时间为3h;
经第一级研磨机研磨后的粉体送至纳米级超细磨机进行研磨,研磨时间为3h,研磨后送振动筛进行筛分,粒度低于1.5微米的出料送入高速搅拌机;
将超细熔融石英硅微粉送入高速搅拌机,调高速搅拌机的转速为800转/分,搅拌时间以硅微粉自然升温至95℃时,此时将配方量的活性液送入高速搅拌机,继续高速搅拌40min,使活性液与硅微粉充分混合,当温度达到150℃时,停止搅拌,让其自然降温至常温,得到石英硅微粉;
(4)制备石英陶瓷:
S1:按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑,加入高压均质机中混合均匀,充分球磨,得到混合料,并置入反应釜;
S2:将惰性气体充入反应釜,反应釜中加入结合剂,搅拌17min后,升温至130℃,保温反应30min;
S3:将步骤(S2)的在烘箱内先进行低温干燥,低温干燥温度设为27℃,干燥时间设为2h;然后进行高温干燥,高温干燥温度设为130℃,空气湿度设为30%RH,干燥时间设为4.5~5.5h;
S4:将步骤(S3)中干燥后的胚体置于煅烧炉内进行煅烧,煅烧炉内先采用升温速率为2℃/min的升温速率缓慢升至350℃,然后采用升温速率为20~30℃/min的升温速率进行快速升温,升温至1100℃时,在此温度下烧结2h,再采用45℃/min的降温速率进行快速降温,并降温至室温,待冷却后即可得到石英陶瓷胚
S5:在石英陶瓷表面涂刷石英涂层,放入烘干机中烘干2.2h,温度设为160℃,将加强纤维丝均匀的缠绕在石英陶瓷的表面,缠绕完成后在石英陶瓷及加强纤维丝的表面再涂刷一层石英涂层,放入烘干机中烘干2.2h,温度设为160℃,待其冷却即可得到石英陶瓷产品。
进一步改进地,结合剂由1:0.6:0.8的乙酸乙酯、水性树脂聚丙烯酰胺、聚乙二醇组成。
进一步改进地,加强纤维丝呈丝线状,且缠绕在石英陶瓷表面的加强纤维丝为整根不间断,其直径为30μm。
进一步改进地,石英涂层的厚度为350μm。
进一步改进地,步骤(2)中的熔融石英、低温石英、氮化硅比例为1.12:0.25:0.28,氢氧化钡质量含量为500ppm,氧化锆质量含量为500ppm。
本实施例,在陶瓷产品的表面缠绕连接了由玻璃纤维和石墨纤维组成的加强纤维丝,且在加强纤维丝的内外侧分别涂刷石英涂层,加强耐磨性能和抗腐蚀性能,进一步加强对石英陶瓷表面的保护能力,在石英陶瓷产品破碎后加强纤维丝会对碎片起到粘连的效果,避免碎片飞出,同时还方便对碎片进行收集。
实施例二
一种石英陶瓷的制备工艺,由以下重量份的组分制备而成:
硅微粉80份、碳酸钡10份、二硼化钛7份、氮化铝12份、氮化硼11份、氧化锆1份、氮化硅4份、陶瓷粉3份、碳化硅5份、碳酸氢钠1份、三氧化二锑2份、结合剂2份、加强纤维丝3份、石英涂层3份。
进一步改进地,包括如下步骤:
(1)制备加强纤维丝:以玻璃纤维和碳纤维做为原料,将碳纤维以微波聚焦方式对其进行超快速高温石墨化制程,以每min加热速度10℃将碳纤维温度提高到石墨化温度1400℃,并在0.5min内进行快速石墨化制程,形成具有高模数特性的石墨纤维,在玻璃纤维表面涂刷粘合剂,并将其与石墨纤维缠绕粘合,制成加强纤维丝;
(2)石英涂层:熔融石英、低温石英、氮化硅、硅、氢氧化钡、氧化锆和粘结剂置于混料机中进行混合10min,制成石英涂层;
(3)制备石英硅微粉:
选取高纯度硅粉浸入研磨液,将浸液后的硅粉送到研磨机进行研磨,控制研磨机的进料和出料速度均衡,保持研磨时间为2h;
经第一级研磨机研磨后的粉体送至纳米级超细磨机进行研磨,研磨时间为2h,研磨后送振动筛进行筛分,粒度低于1.5微米的出料送入高速搅拌机;
将超细熔融石英硅微粉送入高速搅拌机,调高速搅拌机的转速为750转/分,搅拌时间以硅微粉自然升温至95℃时,此时将配方量的活性液送入高速搅拌机,继续高速搅拌30min,使活性液与硅微粉充分混合,当温度达到150℃时,停止搅拌,让其自然降温至常温,得到石英硅微粉;
(4)制备石英陶瓷:
S1:按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑,加入高压均质机中混合均匀,充分球磨,得到混合料,并置入反应釜;
S2:将惰性气体充入反应釜,反应釜中加入结合剂,搅拌15min后,升温至120℃,保温反应40min;
S3:将步骤(S2)的在烘箱内先进行低温干燥,低温干燥温度设为25℃,干燥时间设为2h;然后进行高温干燥,高温干燥温度设为120℃,空气湿度设为25%RH,干燥时间设为4.5h;
S4:将步骤(S3)中干燥后的胚体置于煅烧炉内进行煅烧,煅烧炉内先采用升温速率为2℃/min的升温速率缓慢升至350℃,然后采用升温速率为20℃/min的升温速率进行快速升温,升温至1100℃时,在此温度下烧结1.5h,再采用45℃/min的降温速率进行快速降温,并降温至室温,待冷却后即可得到石英陶瓷胚
S5:在石英陶瓷表面涂刷石英涂层,放入烘干机中烘干2h,温度设为150℃,将加强纤维丝均匀的缠绕在石英陶瓷的表面,缠绕完成后在石英陶瓷及加强纤维丝的表面再涂刷一层石英涂层,放入烘干机中烘干2h,温度设为150℃,待其冷却即可得到石英陶瓷产品。
进一步改进地,结合剂由1:0.6:0.8的乙酸乙酯、水性树脂聚丙烯酰胺、聚乙二醇组成。
进一步改进地,加强纤维丝呈丝线状,且缠绕在石英陶瓷表面的加强纤维丝为整根不间断,其直径为30μm。
进一步改进地,石英涂层的厚度为300μm。
进一步改进地,步骤(2)中的熔融石英、低温石英、氮化硅比例为0.12:0.05:0.08,氢氧化钡质量含量为200ppm,氧化锆质量含量为200ppm。
本实施例,在陶瓷产品的表面缠绕连接了由玻璃纤维和石墨纤维组成的加强纤维丝,且在加强纤维丝的内外侧分别涂刷石英涂层,加强耐磨性能和抗腐蚀性能,进一步加强对石英陶瓷表面的保护能力,在石英陶瓷产品破碎后加强纤维丝会对碎片起到粘连的效果,避免碎片飞出,同时还方便对碎片进行收集。
实施例三
一种石英陶瓷的制备工艺,由以下重量份的组分制备而成:
硅微粉110份、碳酸钡15份、二硼化钛16份、氮化铝15份、氮化硼13份、氧化锆5份、氮化硅8份、陶瓷粉8份、碳化硅8份、碳酸氢钠4份、三氧化二锑5份、结合剂7份、石英涂层8份。
进一步改进地,包括如下步骤:
(1)石英涂层:熔融石英、低温石英、氮化硅、硅、氢氧化钡、氧化锆和粘结剂置于混料机中进行混合40min,制成石英涂层;
(2)制备石英硅微粉:
选取高纯度硅粉浸入研磨液,将浸液后的硅粉送到研磨机进行研磨,控制研磨机的进料和出料速度均衡,保持研磨时间为4h;
经第一级研磨机研磨后的粉体送至纳米级超细磨机进行研磨,研磨时间为5h,研磨后送振动筛进行筛分,粒度低于1.5微米的出料送入高速搅拌机;
将超细熔融石英硅微粉送入高速搅拌机,调高速搅拌机的转速为900转/分,搅拌时间以硅微粉自然升温至95℃时,此时将配方量的活性液送入高速搅拌机,继续高速搅拌60min,使活性液与硅微粉充分混合,当温度达到150℃时,停止搅拌,让其自然降温至常温,得到石英硅微粉;
(3)制备石英陶瓷:
S1:按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑,加入高压均质机中混合均匀,充分球磨,得到混合料,并置入反应釜;
S2:将惰性气体充入反应釜,反应釜中加入结合剂,搅拌20min后,升温至150℃,保温反应60min;
S3:将步骤(S2)的在烘箱内先进行低温干燥,低温干燥温度设为30℃,干燥时间设为3h;然后进行高温干燥,高温干燥温度设为140℃,空气湿度设为35%RH,干燥时间设为5.5h;
S4:将步骤(S3)中干燥后的胚体置于煅烧炉内进行煅烧,煅烧炉内先采用升温速率为2℃/min的升温速率缓慢升至350℃,然后采用升温速率为30℃/min的升温速率进行快速升温,升温至1200℃时,在此温度下烧结2.5h,再采用50℃/min的降温速率进行快速降温,并降温至室温,待冷却后即可得到石英陶瓷胚
S5:在石英陶瓷表面涂刷石英涂层,放入烘干机中烘干2.5h,温度设为170℃,完成后在石英陶瓷表面再涂刷一层石英涂层,放入烘干机中烘干2.5h,温度设为170℃,待其冷却即可得到石英陶瓷产品。
进一步改进地,结合剂由1:0.6:0.8的乙酸乙酯、水性树脂聚丙烯酰胺、聚乙二醇组成。
进一步改进地,石英涂层的厚度为400μm。
进一步改进地,步骤(2)中的熔融石英、低温石英、氮化硅比例为2:0.5:0.5,氢氧化钡质量含量为800ppm,氧化锆质量含量为800ppm。
本实施例,在陶瓷产品的表面未缠绕加强纤维丝,其结构强度较实施例一和实施例二的陶瓷产品低,且破碎后产生的碎片易飞出,不易收集和清理。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (6)

1.一种石英陶瓷的制备工艺,其特征在于:由以下重量份的组分制备而成:
硅微粉80~110份、碳酸钡10~15份、二硼化钛7~16份、氮化铝12~15份、氮化硼11~13份、氧化锆1~5份、氮化硅4~8份、陶瓷粉3~8份、碳化硅5~8份、碳酸氢钠1~4份、三氧化二锑2~5份、结合剂2~7份、加强纤维丝3~8份、石英涂层3~8份。
2.根据权利要求1所述的一种石英陶瓷的制备工艺,其特征在于:包括如下步骤:
(1)制备加强纤维丝:以玻璃纤维和碳纤维做为原料,将碳纤维以微波聚焦方式对其进行超快速高温石墨化制程,以每min加热速度10~100℃将碳纤维温度提高到石墨化温度1400~3000℃,并在0.5~10min内进行快速石墨化制程,形成具有高模数特性的石墨纤维,在玻璃纤维表面涂刷粘合剂,并将其与石墨纤维缠绕粘合,制成加强纤维丝;
(2)石英涂层:熔融石英、低温石英、氮化硅、硅、氢氧化钡、氧化锆和粘结剂置于混料机中进行混合10~40min,制成石英涂层;
(3)制备石英硅微粉:
选取高纯度硅粉浸入研磨液,将浸液后的硅粉送到研磨机进行研磨,控制研磨机的进料和出料速度均衡,保持研磨时间为2~4h;
经第一级研磨机研磨后的粉体送至纳米级超细磨机进行研磨,研磨时间为2~5h,研磨后送振动筛进行筛分,粒度低于1.5微米的出料送入高速搅拌机;
将超细熔融石英硅微粉送入高速搅拌机,调高速搅拌机的转速为750~900转/分,搅拌时间以硅微粉自然升温至95℃时,此时将配方量的活性液送入高速搅拌机,继续高速搅拌30~60min,使活性液与硅微粉充分混合,当温度达到150℃时,停止搅拌,让其自然降温至常温,得到石英硅微粉;
(4)制备石英陶瓷:
S1:按照配方重量份称取硅微粉、碳酸钡、二硼化钛、氮化铝、氮化硼、氧化锆、氮化硅、陶瓷粉、碳化硅、碳酸氢钠、三氧化二锑,加入高压均质机中混合均匀,充分球磨,得到混合料,并置入反应釜;
S2:将惰性气体充入反应釜,反应釜中加入结合剂,搅拌15~20min后,升温至120~150℃,保温反应40~60min;
S3:将步骤(S2)的在烘箱内先进行低温干燥,低温干燥温度设为25~30℃,干燥时间设为2~3h;然后进行高温干燥,高温干燥温度设为120~140℃,空气湿度设为25~35%RH,干燥时间设为4.5~5.5h;
S4:将步骤(S3)中干燥后的胚体置于煅烧炉内进行煅烧,煅烧炉内先采用升温速率为2℃/min的升温速率缓慢升至350℃,然后采用升温速率为20~30℃/min的升温速率进行快速升温,升温至1100~1200℃时,在此温度下烧结1.5~2.5h,再采用45~50℃/min的降温速率进行快速降温,并降温至室温,待冷却后即可得到石英陶瓷胚
S5:在石英陶瓷表面涂刷石英涂层,放入烘干机中烘干2~2.5h,温度设为150~170℃,将加强纤维丝均匀的缠绕在石英陶瓷的表面,缠绕完成后在石英陶瓷及加强纤维丝的表面再涂刷一层石英涂层,放入烘干机中烘干2~2.5h,温度设为150~170℃,待其冷却即可得到石英陶瓷产品。
3.根据权利要求1所述的一种石英陶瓷的制备工艺,其特征在于:所述结合剂由1:0.6:0.8的乙酸乙酯、水性树脂聚丙烯酰胺、聚乙二醇组成。
4.根据权利要求2所述的一种石英陶瓷的制备工艺,其特征在于:所述加强纤维丝呈丝线状,且缠绕在石英陶瓷表面的加强纤维丝为整根不间断,其直径为30μm。
5.根据权利要求2所述的一种石英陶瓷的制备工艺,其特征在于:所述石英涂层的厚度为300~400μm。
6.根据权利要求2所述的一种石英陶瓷的制备工艺,其特征在于:步骤(2)中的熔融石英、低温石英、氮化硅比例为0.12~2:0.05~0.5:0.08~0.5,氢氧化钡质量含量为10~1000ppm,氧化锆质量含量为10~1000ppm。
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