CN114133219A - 电子烟用氧化锆复合的高温多孔陶瓷及其制备方法 - Google Patents
电子烟用氧化锆复合的高温多孔陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开一种电子烟用氧化锆复合的高温多孔陶瓷及其制备方法,具体步骤包括:将350‑375重量份D50粒径为30‑70μm的氧化铝、25‑50重量份D50粒径为1‑3μm的氧化锆、80‑120重量份D50粒径为30‑50μm的玉米淀粉、40‑60重量份的玻璃粉、1‑5重量份的硬脂酸和100‑150重量份的石蜡进行球磨,得到混合料;将60‑100重量份的聚丙烯加入密炼机中,分5次加入混合料,进行密炼、破碎、注射成型、排胶烧结,得到电子烟用氧化锆复合的高温多孔陶瓷。本发明采用氧化铝‑氧化锆体系制备多孔陶瓷,基于氧化铝‑氧化锆高温下不固溶,通过氧化锆陶瓷弥散分布在氧化铝颗粒之间,高温下抑制氧化铝晶粒间晶界的迁移,抑制晶粒长大,从而实现了孔隙率≥50%,孔径大于20微米,抗压强度≥500N的多孔陶瓷雾化芯。
Description
技术领域
本发明涉及电子烟技术领域,尤其涉及一种电子烟用氧化锆复合的高温多孔陶瓷及其制备方法。
背景技术
根据烧结温度的不同,电子烟的雾化芯主要有两种类型,一种是以低温玻璃粉为粘接剂在600-700℃烧结而成低温多孔陶瓷,另外一种是在1200℃以上高温烧结而成的多孔陶瓷。对低温多孔陶瓷而言,陶瓷颗粒之间的结合主要依靠低温玻璃粉的粘结作用,结合强度较低,使用过程中伴随着陶瓷基体受热热胀冷缩及气体流动影响,容易出现掉粉现象,有吸入人体肺部的风险,这是不可接受的。而高温烧结陶瓷主要依靠基体颗粒之间的晶界强度结合,结合强度高,极大的避免了掉粉的风险,这是高温多孔陶瓷的主要优势。然而,烧结本身就是消灭孔隙以达到致密化的过程,所以高温烧结多孔陶瓷在制备过程中相比低温多孔陶瓷容易出现烧结收缩率过大,孔隙率低,孔径较小的问题,这是高温多空陶瓷目前亟待解决的技术难点。
发明内容
本发明的目的是针对现有技术中的不足,提供一种电子烟用氧化锆复合的高温多孔陶瓷及其制备方法,以大尺寸氧化铝陶瓷颗粒为基体材料,氧化锆为晶界迁移抑制剂,基于氧化铝-氧化锆高温下不固溶,互不扩散,不形成化合物的基本原理,旨在通过氧化锆陶瓷弥散分布在氧化铝颗粒之间,高温下抑制氧化铝晶粒间晶界的迁移,抑制晶粒长大,从而获得一种具有高孔隙率,大孔径的多孔陶瓷制备方法。
为实现上述目的,本发明所提供的技术方案是:一种电子烟用氧化锆复合的高温多孔陶瓷,包含如下组分:氧化铝350-375重量份、氧化锆25-50重量份、玉米淀粉80-120重量份、玻璃粉40-60重量份、聚丙烯60-100重量份、石蜡100-150重量份、硬脂酸1-5重量份。
优选地,所述氧化铝的D50粒径为30-70μm。
优选地,所述氧化锆的D50粒径为1-3μm。
优选地,所述玉米淀粉的D50粒径为30-50μm。
上述的电子烟用氧化锆复合的高温多孔陶瓷的制备方法,包括以下步骤:
(1)将氧化铝、氧化锆、玉米淀粉、玻璃粉、硬脂酸和石蜡按比例称量,加入滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径为1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
本发明的有益效果为:
1、本发明采用氧化铝-氧化锆体系制备多孔陶瓷,基于氧化铝-氧化锆高温下不固溶,不形成化合物的基本原理,通过氧化锆弥散分布在氧化铝颗粒之间,高温下抑制氧化铝晶粒间晶界的迁移,抑制晶粒长大,从而实现了孔隙率≥50%,孔径大于20微米,抗压强度≥500N的多孔陶瓷雾化芯。
2、采用注射成型工艺保证了雾化芯制备工艺的稳定性和尺寸一致性。
3、雾化芯陶瓷组成材材料种类较少,且为常见工业原料,来源稳定,质量可靠。
具体实施方式
为了进一步理解本发明,下面结合实施例对本发明优选实施方案进行描述,但是应当理解,这些描述只是为进一步说明本发明的特征和优点,而不是对本发明权利要求的限制。
本发明所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
实施例1
(1)称取350重量份D50粒径为50μm的氧化铝、50重量份D50粒径为2μm的氧化锆、100重量份D50粒径为30μm的玉米淀粉、50重量份的玻璃粉、3重量份的硬脂酸和120重量份的石蜡并置于滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将80重量份的聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中进行排胶烧结,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
实施例2
(1)称取375重量份D50粒径为30μm的氧化铝、25重量份D50粒径为3μm的氧化锆、80重量份D50粒径为40μm的玉米淀粉、40重量份的玻璃粉、1重量份的硬脂酸和100重量份的石蜡并置于滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将60重量份的聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中进行排胶烧结,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
实施例3
(1)称取360重量份D50粒径为70μm的氧化铝、40重量份D50粒径1μm的氧化锆、120重量份D50粒径为50μm的玉米淀粉、60重量份的玻璃粉、5重量份的硬脂酸和150重量份的石蜡并置于滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将100重量份的聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中进行排胶烧结,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
对比例1
(1)称取325重量份D50粒径为30μm的氧化铝、75重量份D50粒径为3μm的氧化锆、80重量份D50粒径为40μm的玉米淀粉、40重量份的玻璃粉、1重量份的硬脂酸和100重量份的石蜡并置于滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将60重量份的聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中进行排胶烧结,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
对比例2
(1)称取400重量份D50粒径为50μm的氧化铝、100重量份D50粒径为30μm的玉米淀粉、50重量份的玻璃粉、3重量份的硬脂酸和120重量份的石蜡并置于滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将80重量份的聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中进行排胶烧结,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
对实施例1-3和对比例1-2制备得到的电子烟用氧化锆复合的高温多孔陶瓷进行了如下测试:
孔径:采用压汞法对陶瓷块体进行孔径分布测试,参考国标GB/T21650.2-2008;
孔隙率:采用阿基米德排水法对块体陶瓷进行孔隙率测试,参考国标JIS R1634-1998
抗压强度:采用电子烟雾化芯强度测试仪对陶瓷块体进行抗压强度测试,加载速率为50mm/min,测量断裂时所承受的最大力。
表1为实施例1-3和对比例1-2所得电子烟用多孔陶瓷的孔径、孔隙率以及抗压强度的对应表。
表1
平均孔径/μm | 孔隙率/% | 抗压强度/N | |
实施例1 | 23 | 50 | 600 |
实施例2 | 26 | 56 | 500 |
实施例3 | 25 | 55 | 550 |
对比例1 | 28 | 58 | 200 |
对比例2 | 10 | 35 | 800 |
本发明采用氧化铝-氧化锆体系制备多孔陶瓷,基于氧化铝-氧化锆高温下不固溶,不形成化合物的基本原理,通过氧化锆陶瓷弥散分布在氧化铝颗粒之间,高温下抑制氧化铝晶粒间晶界的迁移,抑制晶粒长大,采用注射成型工艺保证了雾化芯制备工艺的稳定性和尺寸一致性,从而实现了孔隙率≥50%,孔径大于20微米,抗压强度≥500N的多孔陶瓷雾化芯。
根据上述说明书的揭示,本发明所属领域的技术人员还可以对上述实施方式进行适当的变更和修改。因此,本发明并不局限于上面揭示和描述的具体实施方式,对本发明的一些修改和变更也应当落入本发明的权利要求的保护范围内。此外,尽管本说明书中使用了一些特定的术语,但这些术语只是为了方便说明,并不对本发明构成任何限制。
Claims (5)
1.一种电子烟用氧化锆复合的高温多孔陶瓷,其特征在于:包含如下组分:氧化铝350-375重量份、氧化锆25-50重量份、玉米淀粉80-120重量份、玻璃粉40-60重量份、聚丙烯60-100重量份、石蜡100-150重量份、硬脂酸1-5重量份。
2.根据权利要求1所述的电子烟用氧化锆复合的高温多孔陶瓷,其特征在于:所述氧化铝的D50粒径为30-70μm。
3.根据权利要求1所述的电子烟用氧化锆复合的高温多孔陶瓷,其特征在于:所述氧化锆的D50粒径为1-3μm。
4.根据权利要求1所述的电子烟用氧化锆复合的高温多孔陶瓷,其特征在于:所述玉米淀粉的D50粒径为30-50μm。
5.一种根据权利要求1-4任意一项所述的电子烟用氧化锆复合的高温多孔陶瓷的制备方法,其特征在于:包括以下步骤:
(1)将氧化铝、氧化锆、玉米淀粉、玻璃粉、硬脂酸和石蜡按比例称量,加入滚筒球磨机中,再加入直径为10mm的氧化铝球磨珠,球料比为2:1,球磨机转速为100r/min,球磨12h,得到混合料;
(2)将聚丙烯加入密炼机中,温度200℃,转速40r/min,搅拌30min后将密炼机温度降低至180℃,转速30r/min,分5次加入混合料,每次间隔30min;待混合料加入完毕,转速调为20r/min,继续密炼1h,得到混炼料;
(3)将冷却后的混炼料放入颚式破碎机进行破碎,得到粒径为1cm的颗粒物;
(4)将颗粒物在注射成型机中进行注射成型,注射机储料仓温度从注射喷口到喂料加注端为五段式梯度设置依次为190-170-150-130-100℃,注射压力为60bar,注射后保压时间为2s,得到生坯;
(5)将生坯进行放入烧结炉中,按下述过程进行排胶烧结:50min升到120℃,在120℃保温60min;180min从120℃升到280℃,在280℃保温120min;180min从280℃升到390℃,在390℃保温100min;120min从390℃升到500℃,然后100min从500℃升到1250℃,在1250℃保温30min,之后随炉冷却,得到电子烟用氧化锆复合的高温多孔陶瓷。
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