CN115073141A - 一种单相近零热膨胀材料及其制备方法和应用 - Google Patents
一种单相近零热膨胀材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种单相近零热膨胀材料及其制备方法和应用,属于无机非金属材料技术领域,本发明的单相近零热膨胀材料的化学式为Cd4‑yMyAl6O12XO4,属于纯铝方钠石笼结构,其中,M为Fe,Zn,Mg,Hg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba中的任意一种,X为S或Mo,y的取值范围为0‑2。本发明的单相近零热膨胀材料同时具备宽近零膨胀温区、化学/热力学稳定和可紫外透过性,在10K‑1400K可以稳定存在,没有相变或分解发生,其中,Cd4Al6O12SO4在10‑868K的温度区间内,使用X射线衍射技术测得的本征线性热膨胀系数为0.09×10‑6/K,具有非常高的应用前景。
Description
技术领域
本发明涉及无机非金属材料技术领域,特别涉及一种单相近零热膨胀材料及其制备方法和应用。
背景技术
热胀冷缩,是自然界绝大多数材料所具备的基本性质。对于工作环境温度剧烈波动或敏感的设备或器件,材料热膨胀产生的热应力常会导致其性能的降低、信号失真,波束变形,结构破坏等。传统上,通过增加外部控温装置或设计复杂的结构或填充复合物来进行热效应的补偿,这不仅使得整个器件复杂性增加,提高了使用成本,也降低了系统可靠性。随着航天技术、高功率高精密激光技术、燃料电池正负极,高性能催化剂等现代高新技术的发展,急需克服热效应对其性能的约束,这急需发现新型的高热稳定性的材料来满足目前技术的需求。
近十余年主流的消除材料热效应的方法主要有三种:(1)基于Turner模型Levin模型等,将正、负热膨胀材料进行机械混合,通过调节正负热膨胀材料的比例实现近零膨胀(|热膨胀系数|<2×10-6/K ,如锂铝硅酸盐微晶玻璃,ZrW2O8基,A2M3O12基陶瓷多相混合的近零热膨胀材料等。但机械混合法会因不同材料的界面接触,产生局部的热应力,降低近零膨胀复合材料的力/热学及机械性能。
(2)在负热膨胀材料里进行化学掺杂,通过调节掺杂元素的含量得到近零膨胀材料,如以ZrMo2O8为母体,用Sn部分替换Zr,得到的Zr0.4Sn0.6Mo2O8这一近零热膨胀材料。然而,化学掺杂法则受限于负热膨胀材料通常具备的开放式骨架,制备过程通常存在以下难以解决的问题:(a)相变或分解,如ZrW2O8只在1105℃-1257℃范围内稳态存在,但低于该温度范围时,ZrW2O8具有转化为稳态的ZrO2和WO3,因此,其需要在高温下快速退火才可能保持其负热膨胀性能。ZrV2O7常温下为正膨胀材料,100℃以上才转变为负热膨胀材料;(b)反应物挥发导致制备不稳定,如MgZrF6,ScF3,A2Mo3O12等在合成温度附近,反应物存在严重的挥发,这使得每次实验结果的可重复性较低;(c)受限于母体材料本身的热膨胀性质,新材料的近零热膨胀温区较窄,如Fe[Co(CN)6],Mn3Cu0.5Ge0.5N,TbCo1.9Fe0.1等,其近零热膨胀温区几乎都在室温之下()。
(3)通过结构设计/探索,合成出的单一相的近零热膨胀材料如TaO2F,K6Cd3(C3N3O3)4,FeNi36,Zn4B6O13·[Zn8(SiO4)(m-BDC)6]n等,而这几种材料的近零膨胀温区也较窄,在室温附近。
因此,需要研究一种同时具备宽近零膨胀温区,化学和热力学稳定,可紫外透过的单相近零热膨胀材料。
发明内容
本发明的目的在于全部或部分解决上述消除材料热效应方法中存在的技术问题,提供一种化学式为Cd4-yMyAl6O12XO4的单相近零热膨胀材料及其制备方法和应用,同时具备宽的近零膨胀温区、化学/热力学稳定和可紫外透过性,在10K-1400K可以稳定存在,没有相变或分解发生,具有非常高的应用前景。
为实现上述目的,本发明采用下述技术方案:
本发明提供一种单相近零热膨胀材料,其化学式为Cd4-yMyAl6O12XO4,为纯铝方钠石笼结构,其中,M为Fe,Zn,Hg,Mg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba中的任意一种,X为S或Mo,y的取值范围为0-2。
优选地,其化学式为Cd4Al6O12SO4,其室温下的单胞参数为9.10206埃,空间群为I- 43m属于立方晶系,具备各项同性的热力学和光学性质;在10-868K的温度区间内,使用X射线衍射技术测得的本征线性热膨胀系数为0.09×10-6/K;在波长280 nm到2500nm的范围内,具有90%以上的光透过率。
优选地,其化学式为Cd2Fe2Al6O12SO4,Cd2Zn2Al6O12SO4,Cd2Mg2Al6O12SO4,Cd2Hg2Al6O12SO4,Cd2Cu2Al6O12SO4,Cd2Ni2Al6O12SO4,Cd2Co2Al6O12SO4,Cd2Pb2Al6O12SO4,Cd2Mn2Al6O12SO4,Cd2Ca2Al6O12SO4,Cd2Sr2Al6O12SO4和Cd2Ba2Al6O12SO4中的任意一种,属于立方晶系,具备各项同性的热力学和光学性质。
优选地,其化学式为Cd2Fe2Al6O12MoO4,Cd2Zn2Al6O12MoO4,Cd2Mg2Al6O12MoO4,Cd2Hg2Al6O12MoO4,Cd2Cu2Al6O12MoO4,Cd2Ni2Al6O12MoO4,Cd2Co2Al6O12MoO4,Cd2Pb2Al6O12MoO4,Cd2Mn2Al6O12MoO4,Cd2Ca2Al6O12MoO4,Cd2Sr2Al6O12MoO4和Cd2Ba2Al6O12MoO4中的任意一种,属于立方晶系,具备各项同性的热力学和光学性质。
本发明还提供一种如上所述的单相近零热膨胀材料的制备方法,包括以下步骤:
S1:将含有Cd,M,Al以及X6+的化合物按比例称重后充分研磨混合,在200~300℃下保温0.5~2天后,冷却至0~40℃,得到混合物I;
S2:将混合物I继续研磨混合后,在400~500℃下保温0.5~3天后,冷却至0~40℃,得到混合物II;
S3:将混合物II继续研磨混合后,在600~800℃下保温0.5~3天后,冷却至0~40℃,得到混合物III;
S4:将混合物III继续研磨混合后,在700~900℃下保温0.5~3天后,冷却至0~40℃,得到混合物IV;
S5:将混合物IV继续研磨混合后,在900~1000℃下保温1~5天后,冷却至0~40℃,得到Cd4-yMyAl6O12XO4多晶原料V。
本发明还提供一种近零热膨胀陶瓷器件,采用如上所述的单相近零热膨胀材料制备而成。
优选地,所述器件为长方体器件,高×宽×长的尺寸为3×4×8 mm,所述器件在170-773K的温度范围的平均热膨胀系数为1.5×10-6/K。
本发明还提供一种如上所述的近零热膨胀陶瓷器件的制备方法,采用放电等离子烧结技术制备,包括以下步骤:
S1:以水为介质,采用使用行星式球磨机充分研磨Cd4-yMyAl6O12XO4多晶原料,之后在70~200℃下干燥0.5-2天后得到多晶粉料;
S2:称取一定量的所述多晶粉料,将其放入石墨模具,两端用石墨压头压住,放入放电等离子烧结炉中;
S3:使用机械泵抽除等离子烧结炉内的空气,使其真空度降到10 Pa,然后设置升温程序:10分钟从27℃升温到770 ℃,五分钟从770 ℃升温到800 ℃;在烧结压力25MPa、烧结温度800 ℃下烧结1分钟,再降到室温;
S4:关闭真空系统,取出陶瓷毛坯,使用线切割加工成形,得到近零热膨胀陶瓷器件。
本发明还提供一种如上所述的单相近零热膨胀材料在催化剂载体中的应用。
本发明还提供一种如上所述的单相近零热膨胀材料在荧光粉中的应用。
本发明还提供一种如上所述的近零热膨胀陶瓷器件在发动机配件中的应用。
本发明还提供一种如上所述的近零热膨胀陶瓷器件在电池电极中的应用。
本发明还提供一种如上所述的近零热膨胀陶瓷器件在光学支架和镜头中的应用。
本发明还提供一种如上所述的近零热膨胀陶瓷器件在电子线路板基底中的应用。
上述技术方案,具备下述有益效果:
(1)现有应用广泛的多相各项同性近零热膨胀材料如锂铝硅酸盐微晶玻璃,ZrW2O8基陶瓷,A2M3O12基陶瓷等,在温度波动时,这些材料的相界面处会存在局部热应力造成的微裂纹,影响器件性能。而本发明的单相近零热膨胀材料Cd4-yMyAl6O12XO4为单一相,不存在相界面接触造成的热应力。
(2)现有应用广泛的单相各项同性近零热膨胀材料FeNi36,Zn4B6O13Mn3Cu0.5Ge0.5N,TbCo1.9Fe0.1等,其近零热膨胀温区均在室温附近,最高温区的FeNi36也仅有393K (120℃)。而本发明的Cd4Al6O12SO4近零热膨胀区间为10K-868K,跨过了室温的约束,而且制备的陶瓷器件,使用热膨胀仪测试后发现,其也可以在170-773K保持近零膨胀特性,这是许多单相近零热膨胀材料所不具备的。
(3)现有应用广泛的单相各项同性近零热膨胀材料MgZrF6,Sc0.85Fe0.15F3等,其反应物在合成过程中存在较为严重的挥发,这会降低每次实验结果的可重复性。本发明的单相各项同性近零热膨胀材料Cd4-yMyAl6O12SO4在合成温度区间具有良好的稳定性,挥发少,不分解,制备流程简单可靠,重复性高。目前已制备近百批Cd4Al6O12SO4多晶粉料,通过X射线衍射确定了这些原料均具有相同的空间群,原位XRD及同步热分析确定了Cd4Al6O12SO4在10 K到1083K之间没有相变,不发生分解,均保持I-43m空间群。
(4)本发明的单相近零热膨胀材料Cd4-yMyAl6O12SO4具有铝方纳石笼结构。其中阳离子Cd位于方纳石笼内部,可以部分被Fe,Zn,Hg,Mg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba替代,掺杂浓度在0-2之间。根据实际需要,可以制备不同热膨胀系数,不同化学性质的近零热膨胀材料,如Cd3.9Sr0.1Al6O12SO4的近零膨胀温区为10-750K,可以满足特定工况/部件对热膨胀系数的需要;如Cd3.9Mn0.1Al6O12SO4具备高热稳定性的发光性能,可以作为优异的荧光粉;Cd3.9Ni0.1Al6O12SO4具备高热稳定性同时拥有磁性,可作为优异的特殊功能部件;Cd3.9Co0.1Al6O12SO4具备高热稳定性同时拥有催化能力,可以作为热稳定性良好的催化剂。
(5)现有具备紫外透过窗口的单相近零热膨胀材料有Zn4B6O13和K6Cd3(C3N3O3)4等,它们的近零热膨胀温区均在室温之下,应用场景有限。优选的,本发明的单相近零热膨胀材料Cd4Al6O12SO4,在波长280 nm到2500nm的范围内具有90%以上的光透过率(具有较好的深紫外透过能力)的同时,在10-868K之间均具有优异的近零膨胀特性,能够广泛用于光学,光纤等领域。
(6)本发明的单相近零热膨胀材料Cd4-yMyAl6O12XO4属于立方晶系,具备各项同性的热力学和光学性质,可用作催化剂和荧光粉材料;利于器件锻造和光学信号的处理,可制备成陶瓷器件,进而广泛应用于发动机配件,电极,光学支架,电子线路板基底等领域中。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对本发明实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面所描述的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为本发明单相近零热膨胀材料Cd4Al6O12SO4的XRD分析,其中(a)为300K时Cd4Al6O12SO4的XRD图谱,(b)为基于变温XRD,使用Rietveld拟合得到的单胞参数随温度的变化图;
图2为本发明单相近零热膨胀材料Cd4Al6O12SO4采用紫外可见近红外分光光度计测定的透过光谱曲线;
图3为本发明单相近零热膨胀材料Cd4Al6O12SO4的TG-DSC曲线,测试气氛为N2气环境;
图4为本发明一实施例的Cd4Al6O12SO4近零热膨胀陶瓷器件的实物照片;
图5为本发明一实施例的Cd4Al6O12SO4近零热膨胀陶瓷器件的热膨胀系数曲线图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中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它实施例,都属于本发明保护的范围。
本发明提供一种单相近零热膨胀材料,其化学式为Cd4-yMyAl6O12XO4,属于纯铝方钠石笼结构,其中,M为Fe,Zn,Hg,Mg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba中的任意一种, X为S或Mo,y的取值范围为0-2。
优选的,以单相近零热膨胀材料Cd4Al6O12SO4例,其为铝方钠石笼结构,其室温下的单胞参数为9.10206埃,从图1中(a)可以看出,其空间群为I-43m属于立方晶系,具备各项同性的热力学和光学性质。从图1中(b)可以看出,测试Cd4Al6O12SO4在10-660K、660-868K两个温度区间拟合的平均线性热膨胀系数分别为-0.05×10-6/K,0.76×10-6/K;即在10-868K的温度区间内,使用X射线衍射技术测得的本征线性热膨胀系数为0.09×10-6/K。从图2中可以看出,Cd4Al6O12SO4在波长280 nm到2500nm的范围内,具有90%以上的光透过率。从图3中可以看出,Cd4Al6O12SO4在较宽的温度区间10-1400K内具有良好的物理、化学稳定性,不挥发,不分解。
单相近零热膨胀材料Cd4Al6O12SO4具有方钠石笼结构,其中的Cd离子位于铝方钠石笼的内部,由于笼内具有较大的空隙,所以Cd离子可被部分其它阳离子部分替代,因此可以进行化学掺杂Cd位点得到一系列Cd4-yMyAl6O12XO4化合物,掺杂元素M为Fe,Zn,Hg,Mg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba中的任意一种, 且掺杂元素的比例可以在0-2之间根据实际需要进行调整。此外位于方纳石笼中心的S也可以被Mo全部取代得到Cd4Al6O12MoO4,且这些化合物也会具备优异的近零热膨胀特性。结合M化学掺杂元素的其它性质如Fe或Co的磁性和催化性,Mn的荧光性能等,在温度波动场合具有潜在的应用。例如,单相近零热膨胀材料Cd3.9Mn0.1Al6O12SO4,具备优异的近零热膨胀特性,还是具备高热稳定性性能的荧光粉。
本发明提供如上所述的Cd4-yMyAl6O12XO4单相近零热膨胀材料的制备方法,包括以下步骤:
S1:将含有Cd,M,Al以及X6+的化合物按比例称重后充分研磨混合,在200~300℃下保温0.5~2天后,冷却至0~40℃,得到混合物I;
S2:将混合物I继续研磨混合后,在400~500℃下保温0.5~3天后,冷却至0~40℃,得到混合物II;
S3:将混合物II继续研磨混合后,在600~800℃下保温0.5~3天后,冷却至0~40℃,得到混合物III;
S4:将混合物III继续研磨混合后,在700~900℃下保温0.5~3天后,冷却至0~40℃,得到混合物IV;
S5:将混合物IV继续研磨混合后,在900~1000℃下保温1~5天后,冷却至0~40℃,得到Cd4-yMyAl6O12XO4多晶原料V。
本发明还提供一种近零热膨胀陶瓷器件,采用上述的Cd4-yMyAl6O12XO4单相近零热膨胀材料制备而成。在一优选实施例中,如图4所示,所述器件为长方体器件,高×宽×长的尺寸为3×4×8 mm,所述器件在170-773K的温度范围的平均热膨胀系数为1.5×10-6/K。
本发明还提供上述Cd4-yMyAl6O12XO4近零热膨胀陶瓷器件的制备方法,采用放电等离子烧结技术制备,包括以下步骤:
S1:以水为介质,采用使用行星式球磨机充分研磨Cd4-yMyAl6O12XO4多晶原料,之后在70~200℃下干燥0.5-2天后得到多晶粉料;
S2:称取一定量的所述多晶粉料,将其放入石墨模具,两端用石墨压头压住,放入放电等离子烧结炉中;
S3:使用机械泵抽除等离子烧结炉内的空气,使其真空度降到10 Pa,然后设置升温程序:10分钟从27℃升温到770 ℃,五分钟从770 ℃升温到800 ℃;在烧结压力25MPa、烧结温度800 ℃下烧结1分钟,再降到室温;
S4:关闭真空系统,取出陶瓷毛坯,使用线切割加工成形,得到近零热膨胀陶瓷器件。
本发明提供一种如上所述的近零热膨胀多晶粉料材料在催化剂中的应用。
本发明提供一种如上所述的近零热膨胀多晶粉料材料在荧光粉中的应用。
本发明提供一种如上所述的近零热膨胀陶瓷器件在发动机配件中的应用。
本发明提供一种如上所述的近零热膨胀陶瓷器件在电池电极中的应用。
本发明提供一种如上所述的近零热膨胀陶瓷器件在光学支架或镜头中的应用。
本发明提供一种如上所述的近零热膨胀陶瓷器件在电子线路板基底中的应用。
上述技术方案,具备下述有益效果:
(1)现有应用广泛的多相各项同性近零热膨胀材料如锂铝硅酸盐微晶玻璃,ZrW2O8基陶瓷,A2M3O12基陶瓷等,在温度波动时,这些材料的相界面处会存在局部热应力造成的微裂纹,影响器件性能。而本发明的单相近零热膨胀材料Cd4-yMyAl6O12XO4为单一相,不存在相界面接触造成的热应力。
(2)现有应用广泛的单相各项同性近零热膨胀材料FeNi36,Zn4B6O13Mn3Cu0.5Ge0.5N,TbCo1.9Fe0.1等,其近零热膨胀温区均在室温附近,最高温区的FeNi36也仅有393K (120℃)。而本发明的Cd4Al6O12SO4近零热膨胀区间为10K-868K,跨过了室温的约束,而且制备的陶瓷器件,使用热膨胀仪测试后发现,其也可以在170-773K保持近零膨胀特性,这是许多单相近零热膨胀材料所不具备的。
(3)现有应用广泛的单相各项同性近零热膨胀材料MgZrF6,Sc0.85Fe0.15F3等,其反应物在合成过程中存在较为严重的挥发,这会降低每次实验结果的可重复性。本发明的单相各项同性近零热膨胀材料Cd4-yMyAl6O12SO4在合成温度区间具有良好的稳定性,挥发少,不分解,制备流程简单可靠,重复性高。目前已制备近百批Cd4Al6O12SO4多晶粉料,通过X射线衍射确定了这些原料均具有相同的空间群,原位XRD及同步热分析确定了Cd4Al6O12SO4在10 K到1083K之间没有相变,不发生分解,均保持I-43m空间群。
(4)本发明的单相近零热膨胀材料Cd4-yMyAl6O12SO4具有铝方纳石笼结构。其中阳离子Cd位于方纳石笼内部,可以部分被Fe,Zn,Hg,Mg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba替代,掺杂浓度在0-2之间。根据实际需要,可以制备不同热膨胀系数,不同化学性质的近零热膨胀材料,如Cd3.9Sr0.1Al6O12SO4的近零膨胀温区为10-750K,可以满足特定工况/部件对热膨胀系数的需要;如Cd3.9Mn0.1Al6O12SO4具备高热稳定性的发光性能,可以作为优异的荧光粉;Cd3.9Ni0.1Al6O12SO4具备高热稳定性同时拥有磁性,可作为优异的特殊功能部件;Cd3.9Co0.1Al6O12SO4具备高热稳定性同时拥有催化能力,可以作为热稳定性良好的催化剂。
(5)现有具备紫外透过窗口的单相近零热膨胀材料有Zn4B6O13和K6Cd3(C3N3O3)4等,它们的近零热膨胀温区均在室温之下,应用场景有限。优选的,本发明的单相近零热膨胀材料Cd4Al6O12SO4,在波长280 nm到2500nm的范围内具有90%以上的光透过率(具有较好的深紫外透过能力)的同时,在10-868K之间均具有优异的近零膨胀特性,能够广泛用于光学,光纤等领域。
(6)本发明的单相近零热膨胀材料Cd4-yMyAl6O12XO4属于立方晶系,具备各项同性的热力学和光学性质,可用作催化剂和荧光粉材料;利于器件锻造和光学信号的处理,可制备成陶瓷器件,进而广泛应用于发动机配件,电极,光学支架,电子线路板基底等领域中。
以上仅为本发明的较佳实施例而已,仅具体描述了本发明的技术原理,这些描述只是为了解释本发明的原理,不能以任何方式解释为对本发明保护范围的限制。基于此处解释,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进,及本领域的技术人员不需要付出创造性的劳动即可联想到本发明的其他具体实施方式,均应包含在本发明的保护范围之内。
Claims (14)
1.一种单相近零热膨胀材料,其特征在于,其化学式为Cd4-yMyAl6O12XO4,为纯铝方钠石笼结构,其中,M为Fe,Zn,Mg,Hg,Cu,Ni,Co,Pb,Mn,Ca,Sr,和Ba中的任意一种,X为S或Mo,y的取值范围为0-2。
2.根据权利要求1所述的单相近零热膨胀材料,其特征在于,其化学式为Cd4Al6O12SO4,其室温下的单胞参数为9.10206埃,空间群为I-43m属于立方晶系,具备各项同性的热力学和光学性质;在10-868K的温度区间内,使用X射线衍射技术测得的本征线性热膨胀系数为0.09×10-6/K;在波长280 nm到2500nm的范围内,具有90%以上的光透过率。
3.根据权利要求1所述的单相近零热膨胀材料,其特征在于,其化学式为Cd2Fe2Al6O12SO4,Cd2Zn2Al6O12SO4,Cd2Mg2Al6O12SO4,Cd2Hg2Al6O12SO4,Cd2Cu2Al6O12SO4,Cd2Ni2Al6O12SO4,Cd2Co2Al6O12SO4,Cd2Pb2Al6O12SO4,Cd2Mn2Al6O12SO4,Cd2Ca2Al6O12SO4,Cd2Sr2Al6O12SO4和Cd2Ba2Al6O12SO4中的任意一种,属于立方晶系,具备各项同性的热力学和光学性质。
4.根据权利要求1所述的单相近零热膨胀材料,其特征在于,其化学式为Cd2Fe2Al6O12MoO4,Cd2Zn2Al6O12MoO4,Cd2Mg2Al6O12MoO4,Cd2Hg2Al6O12MoO4,Cd2Cu2Al6O12MoO4,Cd2Ni2Al6O12MoO4,Cd2Co2Al6O12MoO4,Cd2Pb2Al6O12MoO4,Cd2Mn2Al6O12MoO4,Cd2Ca2Al6O12MoO4,Cd2Sr2Al6O12MoO4和Cd2Ba2Al6O12MoO4中的任意一种,属于立方晶系,具备各项同性的热力学和光学性质。
5.一种如权利要求1所述的单相近零热膨胀材料的制备方法,其特征在于,包括以下步骤:
S1:将含有Cd,M,Al以及X6+的化合物按比例称重后充分研磨混合,在200~300℃下保温0.5~2天后,冷却至0~40℃,得到混合物I;
S2:将混合物I继续研磨混合后,在400~500℃下保温0.5~3天后,冷却至0~40℃,得到混合物II;
S3:将混合物II继续研磨混合后,在600~800℃下保温0.5~3天后,冷却至0~40℃,得到混合物III;
S4:将混合物III继续研磨混合后,在700~900℃下保温0.5~3天后,冷却至0~40℃,得到混合物IV;
S5:将混合物IV继续研磨混合后,在900~1000℃下保温1~5天后,冷却至0~40℃,得到Cd4-yMyAl6O12XO4多晶原料V。
6.一种近零热膨胀陶瓷器件,其特征在于,采用权利要求1所述的单相近零热膨胀材料制备而成。
7.根据权利要求6所述的近零热膨胀陶瓷器件,其特征在于,所述器件为长方体器件,高×宽×长的尺寸为3×4×8 mm,所述器件在170-773K的温度范围的平均热膨胀系数为1.5×10-6/K。
8.一种如权利要求6或7所述的近零热膨胀陶瓷器件的制备方法,其特征在于,采用放电等离子烧结技术制备,包括以下步骤:
S1:以水为介质,采用使用行星式球磨机充分研磨Cd4-yMyAl6O12XO4多晶原料,之后在70~200℃下干燥0.5-2天后得到多晶粉料;
S2:称取一定量的所述多晶粉料,将其放入石墨模具,两端用石墨压头压住,放入放电等离子烧结炉中;
S3:使用机械泵抽除等离子烧结炉内的空气,使其真空度降到10 Pa,然后设置升温程序:10分钟从27℃升温到770 ℃,五分钟从770 ℃升温到800 ℃;在烧结压力25MPa、烧结温度800 ℃下烧结1分钟,再降到室温;
S4:关闭真空系统,取出陶瓷毛坯,使用线切割加工成形,得到近零热膨胀陶瓷器件。
9.一种如权利要求1所述的单相近零热膨胀材料在催化剂载体中的应用。
10.一种如权利要求1所述的单相近零热膨胀材料在荧光粉中的应用。
11.一种如权利要求6或7所述的近零热膨胀陶瓷器件在发动机配件中的应用。
12.一种如权利要求6或7所述的近零热膨胀陶瓷器件在电池电极中的应用。
13.一种如权利要求6或7所述的近零热膨胀陶瓷器件在光学支架或镜头中的应用。
14.一种如权利要求6或7所述的近零热膨胀陶瓷器件在电子线路板基底中的应用。
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