CN105645942B - 一种具有核壳结构的硅酸盐陶瓷及其制备方法 - Google Patents
一种具有核壳结构的硅酸盐陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开的具有核壳结构的硅酸盐陶瓷,其核层结构为CaSiO3相、壳层结构为Ca(Mg,Al,Zn)(Si,Al)2O6相,制备过程如下:先以CaCO3和SiO2为原料,球磨混合后在1100~1200℃煅烧合成CaSiO3粉体,然后将CaSiO3粉体放入钙镁铝锌的硝酸盐与硅溶胶的去离子水溶液中,球磨共混后进行喷雾干燥,随后将干燥好的粉体进行预压成型,并在900~1100℃煅烧,冷却后再经冷等静压,在1250~1300℃烧结后即可获得本发明的硅酸盐陶瓷。本发明所采用的原材料来源广泛易得、制备工艺简单可控,利用烧结性能优异的Ca(Mg,Al,Zn)(Si,Al)2O6薄层对CaSiO3粉体进行包覆,可以在相对较低的温度下烧结后获得优良的介电性能。
Description
技术领域
本发明涉及一种硅酸盐陶瓷及其制备方法,属于材料科学技术领域。
背景技术
现代无线通讯技术对人类社会的发展起到了极大的推动作用。近年来,随着信息量的日益增大,对需要传送的信息容量以及传输速度要求越来越高。为解决低频段的拥挤并扩大频率资源,无线通信正朝更高频段的方向发展;相应的微波技术也向着更高频率,即向着毫米波和亚毫米波的方向发展。
目前,以高速传输数据并能传送图像与视频为特征的第四代(4G)移动通信系统已经得到广泛应用;在电视接收系统(TVRO,2-5 GHz)、直接广播系统(DBS,11-13 GHz)等民用领域,其频率使用范围已经超过了10 GHz;特别是在军事通信领域,由于雷达技术的高速发展,使得无线通讯的频率发展到了X波段(8.2-12.4 GHz)与K波段(12-40 GHz)。无线通信使用频率的提高,要求作为信息技术基本组成元素的电子元器件具有较高的自谐振中心频率(f 0 )。高的自谐振中心频率对应着低的介电常数(ε r )。低介电常数能减小材料与电极之间的交互耦合损耗,并提高电信号的传输速率;发展低介电常数(ε r ≤10)材料以满足高频和高速的要求,已成为当今电子材料如何适应高频应用的一个挑战。
硅酸盐系微波介质陶瓷也是目前应用最广的低介电常数材料之一,如MgO-SiO2系、ZnO-SiO2系、CaO-SiO2系等。Cheng等(J Alloy Comp, 2012, 513: 373-377)报道了Mg2SiO4陶瓷的介电常数为6-7,但发现该体系的烧结温度区间非常窄。Zou等(Jap J ApplPhy, 2006, 45: 4143-4145)研究发现,ZnO-SiO2即使在高温下也很难烧结致密,只有当SiO2过量时可细化晶粒、阻止晶粒的异常长大,可以获得介电常数为6.23,Q×f为52,500GHz,τ f 为-55.2ppm/℃的良好介电性能。Wang等(Ceram Int, 2008, 34: 1405-1408)发现,无论是采用传统的固相法还是溶胶-凝胶法,均无法获得致密结构的CaSiO3陶瓷,陶瓷在烧结后存在大量气孔,从而影响了CaSiO3陶瓷的微波介电性能。Sun等(Mat Sci Eng B,2007, 138: 46-50)通过Mg2+对Ca2+的取代,获得具有良好微波介电性能的CaMgSi2O6陶瓷;然而,其烧结温度局限在1290-1310℃之间。
从上述国内外研究结果可知,硅酸盐系微波介质陶瓷具有低的介电常数和良好的品质因数,但其烧成温度范围较窄,从而影响到微波器件产品的一致性。特别是CaSiO3陶瓷在烧结后即便存在大量气孔,但仍然具有良好的微波介电性能;因此,拓宽CaSiO3陶瓷的烧结温度范围、提高其烧结致密度,对提高硅酸盐陶瓷的微波介电性能具有重要意义。
发明内容
本发明的目的是提供一种具有核壳结构的硅酸盐陶瓷及其制备方法,通过核壳结构使该陶瓷具有较低的烧结温度、较宽的烧成温度范围以及优良的微波介电性能。
本发明的具有核壳结构的硅酸盐陶瓷,它的核层为CaSiO3相、壳层为Ca(Mg1-x- yAlxZny)(Si1-x/2Alx/2)2O6相,其中0.04 ≤ x ≤ 0.12,0 ≤ y ≤ 0.2,壳层物质与核层物质的摩尔比为0.001~0.1:1。
本发明的具有核壳结构硅酸盐陶瓷的制备方法,包括以下步骤:
(1)称取相同摩尔数的CaCO3和SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合6~24小时;
(2)将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1100~1200 ℃的温度下煅烧2~4小时,冷却后获得主晶相为CaSiO3的陶瓷粉体;
(3)按壳层组成物中各元素的比例,将硝酸钙、硝酸镁、硝酸铝、硝酸锌以及硅溶胶同时溶解在去离子水中,使混合物在去离子水中的浓度为0.01~0.8 mol/l,搅拌混合均匀;
(4)将步骤(2)制得的陶瓷粉体与步骤(3)制得的溶液进行混合,然后放入球磨罐中,以氧化锆球为磨介,球磨混合4~8小时,随后将混合物进行喷雾干燥,除掉去离子水;
(5)将喷雾干燥后获得的粉体放入模具中,在30~40 MPa的压力下成型,然后升温到900~1100 ℃保温4~6小时,冷却后再放入等静压机中,在150~300 MPa下进行等静压;
(6)将等静压后的产物放在炉中,在1250~1300 ℃保温2~4小时,得到具有核壳结构的硅酸盐陶瓷。
本发明具有以下有益效果:以硅酸钙为核心、通过将镁、铝和锌元素固溶入硅酸钙晶体结构中形成壳层,从而获得以CaSiO3为核、Ca(Mg,Al,Zn)(Si,Al)2O6为壳的核壳结构;由于Ca(Mg,Al,Zn)(Si,Al)2O6具有较低的烧结温度和较宽的烧成温度范围,从而可在保证硅酸钙陶瓷良好介电性能的基础上,获得优异的烧结性能。
具体实施方式
下面结合实例对本发明作进一步描述。
实施例1:CaSiO3-0.1Ca(Mg0.8Al0.1Zn0.1)(Si0.95Al0.05)2O6(x=0.1,y=0.1)
称取1.0 mol的CaCO3和1.0 mol的SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合12小时;将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1150 ℃煅烧2小时,冷却后获得主晶相为CaSiO3的陶瓷粉体。
称取0.1 mol的硝酸钙、0.08 mol的硝酸镁、0.01 mol硝酸铝、0.01 mol硝酸锌以及0.19 mol的硅溶胶同时溶解在去离子水中,使混合溶液在去离子水中的浓度为0.8 mol/l,搅拌混合均匀。将合成的CaSiO3陶瓷粉体放入上述混合溶液中,并置于球磨罐中,以氧化锆球为磨介,球磨混合6小时,随后将混合物进行喷雾干燥,除掉去离子水。将喷雾干燥后获得的粉体放入模具中,在30 MPa的压力下成型,然后升温到1000 ℃保温4小时,冷却后再放入等静压机中,在200 MPa下进行等静压,然后放在高温炉中,升温至1250 ℃保温2小时,获得具有核壳结构的硅酸盐陶瓷。
实施例2:CaSiO3-0.001Ca(Mg0.68Al0.12Zn0.2)(Si0.94Al0.06)2O6(x=0.12,y=0.2)
称取1.0 mol的CaCO3和1.0 mol的SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合24小时;将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1200 ℃煅烧3小时,冷却后获得主晶相为CaSiO3的陶瓷粉体。
称取0.001 mol的硝酸钙、0.00068 mol的硝酸镁、0.00012 mol硝酸铝、0.0002mol硝酸锌以及0.00188 mol的硅溶胶同时溶解在去离子水中,使混合溶液在去离子水中的浓度为0.01 mol/l,搅拌混合均匀。将合成的CaSiO3陶瓷粉体放入上述混合溶液中,并置于球磨罐中,以氧化锆球为磨介,球磨混合4小时,随后将混合物进行喷雾干燥,除掉去离子水。将喷雾干燥后获得的粉体放入模具中,在40 MPa的压力下成型,然后升温到1100 ℃保温5小时,冷却后再放入等静压机中,在300 MPa下进行等静压,然后放在高温炉中,升温至1300 ℃保温3小时,获得具有核壳结构的硅酸盐陶瓷。
实施例3:CaSiO3-0.05Ca(Mg0.76Al0.04Zn0.2)(Si0.98Al0.02)2O6(x=0.04,y=0.2)
称取1.0 mol的CaCO3和1.0 mol的SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合6小时;将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1100 ℃煅烧4小时,冷却后获得主晶相为CaSiO3的陶瓷粉体。
称取0.05 mol的硝酸钙、0.038 mol的硝酸镁、0.002 mol硝酸铝、0.01 mol硝酸锌以及0.098 mol的硅溶胶同时溶解在去离子水中,使混合溶液在去离子水中的浓度为0.3mol/l,搅拌混合均匀。将合成的CaSiO3陶瓷粉体放入上述混合溶液中,并置于球磨罐中,以氧化锆球为磨介,球磨混合8小时,随后将混合物进行喷雾干燥,除掉去离子水。将喷雾干燥后获得的粉体放入模具中,在35 MPa的压力下成型,然后升温到1050 ℃保温6小时,冷却后再放入等静压机中,在150 MPa下进行等静压,然后放在高温炉中,升温至1275 ℃保温4小时,获得具有核壳结构的硅酸盐陶瓷。
实施例4:CaSiO3-0.1Ca(Mg0.88Al0.12)(Si0.94Al0.06)2O6(x=0.12,y=0)
称取1.0 mol的CaCO3和1.0 mol的SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合24小时;将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1200 ℃煅烧2小时,冷却后获得主晶相为CaSiO3的陶瓷粉体。
称取0.1 mol的硝酸钙、0.088 mol的硝酸镁、0.012 mol硝酸铝以及0.188 mol的硅溶胶同时溶解在去离子水中,使混合溶液在去离子水中的浓度为0.5 mol/l,搅拌混合均匀。将合成的CaSiO3陶瓷粉体放入上述混合溶液中,并置于球磨罐中,以氧化锆球为磨介,球磨混合4小时,随后将混合物进行喷雾干燥,除掉去离子水。将喷雾干燥后获得的粉体放入模具中,在30 MPa的压力下成型,然后升温到1100 ℃保温4小时,冷却后再放入等静压机中,在300 MPa下进行等静压,然后放在高温炉中,升温至1300 ℃保温2小时,获得具有核壳结构的硅酸盐陶瓷。
Claims (2)
1.一种具有核壳结构的硅酸盐陶瓷,其特征在于它的核层为CaSiO3相、壳层为Ca(Mg1-x-yAlxZny)(Si1-x/2Alx/2)2O6相,其中0.04 ≤ x ≤ 0.12,0 ≤ y ≤ 0.2,壳层物质与核层物质的摩尔比为0.001~0.1:1。
2.制备权利要求1所述的具有核壳结构的硅酸盐陶瓷的方法,其特征在于包括下述步骤:
(1)称取相同摩尔数的CaCO3和SiO2放入球磨罐中,然后以无水乙醇为介质、氧化锆球为磨介,球磨混合6~24小时;
(2)将上述经过球磨混合的物质放入烘箱中干燥,除去无水乙醇,然后放入高铝坩埚中,在1100~1200 ℃的温度下煅烧2~4小时,冷却后获得主晶相为CaSiO3的陶瓷粉体;
(3)按壳层组成物中各元素的比例,将硝酸钙、硝酸镁、硝酸铝、硝酸锌以及硅溶胶同时溶解在去离子水中,使混合物在去离子水中的浓度为0.01~0.8 mol/l,搅拌混合均匀;
(4)将步骤(2)制得的陶瓷粉体与步骤(3)制得的溶液进行混合,然后放入球磨罐中,以氧化锆球为磨介,球磨混合4~8小时,随后将混合物进行喷雾干燥,除掉去离子水;
(5)将喷雾干燥后获得的粉体放入模具中,在30~40 MPa的压力下成型,然后升温到900~1100 ℃保温4~6小时,冷却后再放入等静压机中,在150~300 MPa下进行等静压;
(6)将等静压后的产物放在炉中,在1250~1300 ℃保温2~4小时,得到具有核壳结构的硅酸盐陶瓷。
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