CN106145906A - 一种低温烧结环保陶瓷材料及其制备工艺 - Google Patents

一种低温烧结环保陶瓷材料及其制备工艺 Download PDF

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CN106145906A
CN106145906A CN201610524116.4A CN201610524116A CN106145906A CN 106145906 A CN106145906 A CN 106145906A CN 201610524116 A CN201610524116 A CN 201610524116A CN 106145906 A CN106145906 A CN 106145906A
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赵岚
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Zhejiang Industry and Trade Vocational College
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Abstract

本发明公开了一种低温烧结环保陶瓷材料及其制备工艺,将制备原料混合料经高能球磨,得到的陶瓷原料粉体进行微波水热,反应后经洗涤、干燥、研磨,得到复合粉体;添加粘结剂进行造粒处理;将造粒品经高压成型;将得到的成型品放入电炉中,经预烧后,得预烧体;将预烧体经烧结后,自然冷却至室温,即得。本发明制备的低温烧结环保陶瓷材料具有优良特性,制备工艺大大提高陶瓷材料制备和使用过程中的环保水平。

Description

一种低温烧结环保陶瓷材料及其制备工艺
技术领域
本发明涉及陶瓷领域,具体涉及一种低温烧结环保陶瓷材料及其制备工艺。
背景技术
陶瓷材料是一类非常重要的无机非金属材料,具有耐摩擦、抗腐蚀、高强度、超硬度等突出优点,在建筑建材、电力设施方面有广泛且重要的应用。随着陶瓷材料应用范围的不断扩大,人们在充分利用陶瓷材料优点的同时,也发现陶瓷材料有很多方面容易对环境造成严重的污染和破坏,从而意识到环保陶瓷材料的重要性。
目前陶瓷材料的制备工艺主要是通过粉体烧结制备而成。陶瓷制备过程中,各种细小的粉体颗粒随风飞扬飘散,既对操作人员呼吸系统造成伤害,也容易造成空气污染,并且高温烧结过程耗费了大量的化石能源,排出的“三废”也会对环境造成破坏。由此可见,提高能量利用效率,降低陶瓷的烧结温度,制备低温烧结环保陶瓷是非常必要的。
中国专利CN 201510955856.9公开了一种低温烧结陶瓷材料及制备方法。该陶瓷材料按重量份由如下成分组成:高岭土55-68份,氮化铝氧化铝混合材料19-31份,硅烷偶联剂7-17份,氧化钛1.5份,云母1-3份,氧化镧0.5份和/或氧化钇0.5份。但是该专利通过添加稀土氧化物来改善陶瓷材料的半导体光电性能,而未从环保应用层面对传统陶瓷材料进行改善和提高。
中国专利CN 201410365589.5公开了一种低温烧结陶瓷介质材料,包括下列重量份数的物质:瓷石31-47份,碳酸钠11-17.9份,聚乙烯醇10-25份,二氧化硅5.7-13.6份,绢云母12-34份,合成橡胶11-54份,乙酰丙酮铈1-11份,聚碳硅烷4-9份,二氧化锰3-15份,疏水改性的纳米级氧化硅5.7-18.4份,丁基橡胶3-14份。但是该专利中添加了很高含量的合成橡胶、聚碳硅烷、丁基橡胶等高分子化合物,在进行烧结时发生分解,导致陶瓷材料化学组成产生不利变化,结构强度大大下降,影响陶瓷材料的使用性能和环保水平。
因此需要发明一种低温烧结环保陶瓷,在不影响传统陶瓷材料优良特性的基础上,大大提高陶瓷材料制备和使用过程中的环保水平。
发明内容
本发明针对上述问题,提供一种低温烧结环保陶瓷材料及其制备工艺。
本发明解决上述问题所采用的技术方案是:一种低温烧结环保陶瓷材料的制备工艺,包括以下步骤:
步骤S1,混料:将制备所述低温烧结陶瓷的原料Al2O3、SiO2、CaO、CoO、MgO、WO3、MoO3、Si3N4混合而成的混合料,投入行星式高能球磨机中,采用乙醇作为球磨介质,其中混合料、乙醇、研磨球的添加质量比为1:(0.8~1.2):(1.8~2.5),经高能球磨4h~8h,所得浆料经干燥研磨后,过200目~300目筛,得到陶瓷原料粉体;
步骤S2,微波水热处理:将得到的陶瓷原料粉体按照60g~100g:1L的添加比例加入水,在160℃~190℃的温度条件下进行微波水热反应60min~150min,反应后经洗涤、干燥、研磨,得到复合粉体;
步骤S3,造粒:将得到的复合粉体添加其自身重量的0.5%~1%的粘结剂,进行造粒处理,过60目~100目筛,截取中间的粉体颗粒,得到造粒品;
步骤S4,成型:将造粒品经高压成型,得到成型品;
步骤S5,预烧:将成型品放入高温箱式电炉中,以3℃/min~6℃/min的升温速率升温至350℃~400℃,保温2h~4h,再以5℃/min~8℃/min的降温速率降温至95℃~105℃,再自然冷却至室温,取出,得预烧体;
步骤S6,烧结:将预烧体以3℃/min~6℃/min的升温速率升温至900℃~960℃,保温3h~6h,再以5℃/min~8℃/min的降温速率降温至450℃~500℃,保温1h~1.5h,再以8℃/min~12℃/min的降温速率降温至200℃~250℃,保温1h~3h,自然冷却至室温,即得所制低温烧结陶瓷。
进一步地,步骤S1中,制备低温烧结陶瓷的原料及其重量百分数为:Al2O3、50份~70份,SiO2、20份~35份,CaO、15份~20份,CoO、10份~15份,MgO、5份~8份,WO3、5份~10份,MoO3、3份~5份,Si3N4、3份~5份。
进一步地,步骤S1中,高能球磨的转速为800r/min~900r/min。
进一步地,步骤S2中,微波水热反应时的反应压力为0.5MPa~1.6MPa。
进一步地,步骤S2中,洗涤具体为:采用去离子水和乙醇进行离心洗涤3次~5次。
进一步地,步骤S2中,干燥具体为:在60℃~70℃的温度条件下进行干燥处理6h~18h。
进一步地,步骤S3中,粘结剂为聚乙烯醇。
更进一步地,聚乙烯醇的质量分数为4%~8%。
进一步地,步骤S4中,高压成型的压力为35MPa~50MPa。
本发明的另一发明目的,在于提供一种低温烧结环保陶瓷材料,采用上述制备工艺制备而成。
本发明的优点是:
1.本发明制备的陶瓷材料具有良好的环保性能;
2.本发明采用的陶瓷制备工艺,采用先水热、造粒、预烧、烧结的制备工艺,有效地降低了陶瓷的烧结温度,大幅降低能耗损失,降低陶瓷生产成本;
3.本发明制备的低温烧结环保陶瓷具有优秀的低吸水率和高抗冲击韧性,并且无甲醛等有毒有害物质释放,具有优秀的环保性能。
具体实施方式
以下对本发明的实施例进行详细说明,但是本发明可以由权利要求限定和覆盖的多种不同方式实施。
实施例1
一种低温烧结环保陶瓷材料的制备工艺,包括以下步骤:
步骤S1,混料:将制备所述低温烧结陶瓷的原料Al2O3、50份,SiO2、20份,CaO、15份,CoO、10份,MgO、5份,WO3、5份,MoO3、3份,Si3N4、3份混合而成的混合料,投入行星式高能球磨机中,采用乙醇作为球磨介质,其中混合料、乙醇、研磨球的添加质量比为1:0.8:1.8,在转速为800r/min的条件下,经高能球磨4h,所得浆料经干燥研磨后,过200目筛,得到陶瓷原料粉体;
步骤S2,微波水热处理:将得到的陶瓷原料粉体按照60g:1L的添加比例加入水,在160℃的温度条件下进行微波水热反应60min,反应后采用去离子水和乙醇对反应产物进行离心洗涤3次~5次,然后在60℃的温度条件下进行干燥处理6h,研磨,得到复合粉体;其中微波水热反应时的反应压力为0.5MPa;
步骤S3,造粒:将得到的复合粉体添加其自身重量的0.5%的聚乙烯醇粘结剂,进行造粒处理,过60目筛,截取中间的粉体颗粒,得到造粒品;其中聚乙烯醇的质量分数为4%;
步骤S4,成型:将造粒品在压力为35MPa的条件下经高压成型,得到成型品;
步骤S5,预烧:将成型品放入高温箱式电炉中,以3℃/min的升温速率升温至350℃,保温2h,再以5℃/min的降温速率降温至95℃,再自然冷却至室温,取出,得预烧体;
步骤S6,烧结:将预烧体以3℃/min的升温速率升温至900℃,保温3h,再以5℃/min的降温速率降温至450℃,保温1h,再以8℃/min的降温速率降温至200℃,保温1h,自然冷却至室温,即得所制低温烧结陶瓷。
实施例2
一种低温烧结环保陶瓷材料的制备工艺,包括以下步骤:
步骤S1,混料:将制备所述低温烧结陶瓷的原料Al2O3、70份,SiO2、35份,CaO、20份,CoO、15份,MgO、8份,WO3、10份,MoO3、5份,Si3N4、5份混合而成的混合料,投入行星式高能球磨机中,采用乙醇作为球磨介质,其中混合料、乙醇、研磨球的添加质量比为1:1.2:2.5,在转速为900r/min的条件下,经高能球磨8h,所得浆料经干燥研磨后,过300目筛,得到陶瓷原料粉体;
步骤S2,微波水热处理:将得到的陶瓷原料粉体按照100g:1L的添加比例加入水,在190℃的温度条件下进行微波水热反应150min,反应后采用去离子水和乙醇对反应产物进行离心洗涤5次,然后在70℃的温度条件下进行干燥处理18h,研磨,得到复合粉体;其中微波水热反应时的反应压力为1.6MPa;
步骤S3,造粒:将得到的复合粉体添加其自身重量的1%的聚乙烯醇粘结剂,进行造粒处理,过100目筛,截取中间的粉体颗粒,得到造粒品;其中聚乙烯醇的质量分数为8%;
步骤S4,成型:将造粒品在压力为50MPa的条件下经高压成型,得到成型品;
步骤S5,预烧:将成型品放入高温箱式电炉中,以6℃/min的升温速率升温至400℃,保温4h,再以8℃/min的降温速率降温至105℃,再自然冷却至室温,取出,得预烧体;
步骤S6,烧结:将预烧体以6℃/min的升温速率升温至960℃,保温6h,再以8℃/min的降温速率降温至500℃,保温1.5h,再以12℃/min的降温速率降温至250℃,保温3h,自然冷却至室温,即得所制低温烧结陶瓷。
实施例3
一种低温烧结环保陶瓷材料的制备工艺,包括以下步骤:
步骤S1,混料:将制备所述低温烧结陶瓷的原料Al2O3、60份,SiO2、27份,CaO、17份,CoO、13份,MgO、6份,WO3、7份,MoO3、4份,Si3N4、4份混合而成的混合料,投入行星式高能球磨机中,采用乙醇作为球磨介质,其中混合料、乙醇、研磨球的添加质量比为1:1:2,在转速为850r/min的条件下,经高能球磨6h,所得浆料经干燥研磨后,过250目筛,得到陶瓷原料粉体;
步骤S2,微波水热处理:将得到的陶瓷原料粉体按照80g:1L的添加比例加入水,在180℃的温度条件下进行微波水热反应120min,反应后采用去离子水和乙醇对反应产物进行离心洗涤4次,然后在65℃的温度条件下进行干燥处理12h,研磨,得到复合粉体;其中微波水热反应时的反应压力为1.0MPa;
步骤S3,造粒:将得到的复合粉体添加其自身重量的0.7%的聚乙烯醇粘结剂,进行造粒处理,过80目筛,截取中间的粉体颗粒,得到造粒品;其中聚乙烯醇的质量分数为6%;
步骤S4,成型:将造粒品在压力为42MPa的条件下经高压成型,得到成型品;
步骤S5,预烧:将成型品放入高温箱式电炉中,以4.5℃/min的升温速率升温至370℃,保温3h,再以6℃/min的降温速率降温至100℃,再自然冷却至室温,取出,得预烧体;
步骤S6,烧结:将预烧体以4.5℃/min的升温速率升温至930℃,保温4.5h,再以6.5℃/min的降温速率降温至470℃,保温1.2h,再以10℃/min的降温速率降温至220℃,保温2h,自然冷却至室温,即得所制低温烧结陶瓷。
实验例1
对实施例1~6所制的低温烧结环保陶瓷材料的性能进行测试,测试结果如表1所示。其中吸水率根据GB/T3299-2011测试。抗冲击韧性根据GB4742-1984测试。铅、镉溶出量根据GB/T3534-2002测试。
表1陶瓷材料性能测试结果
项目 吸水率 抗冲击韧性 铅溶出量 镉溶出量
实施例1所制的陶瓷 0.06% 0.62J/cm2 0.1mg/L 0.005mg/L
实施例2所制的陶瓷 0.05% 0.61J/cm2 0.05mg/L 0.005mg/L
实施例3所制的陶瓷 0.02% 0.65J/cm2 0.02mg/L 0.002mg/L
以上仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。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 (10)

1.一种低温烧结环保陶瓷材料的制备工艺,其特征在于,包括以下步骤:
步骤S1,混料:将制备所述低温烧结陶瓷的原料Al2O3、SiO2、CaO、CoO、MgO、WO3、MoO3、Si3N4混合而成的混合料,投入行星式高能球磨机中,采用乙醇作为球磨介质,其中混合料、乙醇、研磨球的添加质量比为1:(0.8~1.2):(1.8~2.5),经高能球磨4h~8h,所得浆料经干燥研磨后,过200目~300目筛,得到陶瓷原料粉体;
步骤S2,微波水热处理:将得到的陶瓷原料粉体按照60g~100g:1L的添加比例加入水,在160℃~190℃的温度条件下进行微波水热反应60min~150min,反应后经洗涤、干燥、研磨,得到复合粉体;
步骤S3,造粒:将得到的复合粉体添加其自身重量的0.5%~1%的粘结剂,进行造粒处理,过60目~100目筛,截取中间的粉体颗粒,得到造粒品;
步骤S4,成型:将造粒品经高压成型,得到成型品;
步骤S5,预烧:将成型品放入高温箱式电炉中,以3℃/min~6℃/min的升温速率升温至350℃~400℃,保温2h~4h,再以5℃/min~8℃/min的降温速率降温至95℃~105℃,再自然冷却至室温,取出,得预烧体;
步骤S6,烧结:将预烧体以3℃/min~6℃/min的升温速率升温至900℃~960℃,保温3h~6h,再以5℃/min~8℃/min的降温速率降温至450℃~500℃,保温1h~1.5h,再以8℃/min~12℃/min的降温速率降温至200℃~250℃,保温1h~3h,自然冷却至室温,即得所制低温烧结陶瓷。
2.根据权利要求1所述的制备工艺,其特征在于,步骤S1中,制备所述低温烧结陶瓷的原料及其重量百分数为:Al2O3、50份~70份,SiO2、20份~35份,CaO、15份~20份,CoO、10份~15份,MgO、5份~8份,WO3、5份~10份,MoO3、3份~5份,Si3N4、3份~5份。
3.根据权利要求1所述的制备工艺,其特征在于,步骤S1中,所述高能球磨的转速为800r/min~900r/min。
4.根据权利要求1所述的制备工艺,其特征在于,步骤S2中,所述微波水热反应时的反应压力为0.5MPa~1.6MPa。
5.根据权利要求1所述的制备工艺,其特征在于,步骤S2中,所述洗涤具体为:采用去离子水和乙醇进行离心洗涤3次~5次。
6.根据权利要求1所述的制备工艺,其特征在于,步骤S2中,所述干燥具体为:在60℃~70℃的温度条件下进行干燥处理6h~18h。
7.根据权利要求1所述的制备工艺,其特征在于,步骤S3中,所述粘结剂为聚乙烯醇。
8.根据权利要求7所述的制备工艺,其特征在于,所述聚乙烯醇的质量分数为4%~8%。
9.根据权利要求1所述的制备工艺,其特征在于,步骤S4中,所述高压成型的压力为35MPa~50MPa。
10.一种低温烧结环保陶瓷材料,其特征在于,采用权利要求1~9中任一项所述的制备工艺制备而成。
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