CN116396076A - 一种导电铌酸锂靶材的制备方法 - Google Patents
一种导电铌酸锂靶材的制备方法 Download PDFInfo
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- 229910002804 graphite Inorganic materials 0.000 claims description 30
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims description 4
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Abstract
本发明公开了一种导电铌酸锂靶材的制备方法,涉及溅射靶材领域,旨在提供一种铌酸锂靶材,其技术方案要点是:S1:配置C粉、Nb2O5粉末、Li2CO3粉末;S2:将粉末称重后加入到去离子水中形成浆液,进行砂磨破碎,离心喷雾造粒;S3:进行预烧结;S4:将预烧后的还原粉末与Li2CO3粉末称重后加入到去离子水中形成浆液,进行砂磨破碎,进行离心喷雾造粒;S5:对造粒后的粉末再次进行预烧结,得到还原粉末;S6:破碎后筛分;S7:预压,进行烧结;S8:真空退火;S9:退火完成后进行机加工完成产品所需要求。本发明的一种导电铌酸锂靶材的制备方法可制备出高致密度、高纯度、细晶、近化学计量比的铌酸锂导电靶材。
Description
技术领域
本发明涉及磁控溅射靶材领域,更具体地说,它涉及一种导电铌酸锂靶材的制备方法。
背景技术
铌酸锂薄膜在室温下具有高离子电导率、高电子电阻率、高的可见光透过性,且化学稳定性好,可用于全固态电致变色器件中的离子导电层(电解质层)。制备铌酸锂薄膜通常采用磁控溅射或用脉冲激光沉积技术,这就需要高性能的铌酸锂溅射靶材。铌酸锂溅射靶材分为铌酸锂单晶溅射靶材和铌酸锂陶瓷溅射靶材,前者生产周期长、成本高,后者制备工艺简单,成本较低,有利于全固态电致变色器件的成本控制。但对于铌酸锂陶瓷溅射靶材,要求其化学组分均一、晶粒细小且尺寸均匀、致密度高、纯度高。铌酸锂陶瓷溅射靶材的制备方法一般有激光辐照法、固相烧结法。
多年来,铌酸锂(LiNbO3)以单晶形式被广泛研究和应用。有关铌酸锂陶瓷的研究报道却很少。主要原因是铌酸锂陶瓷的制备工艺的每个步骤都存在相当难度。具体表现在烧结时Li的挥发、矫顽场和极化温度高等。此外,铌酸锂陶瓷的制备主要是采用传统的固相反应烧结法,烧结周期长、无法实时监控。随着近年来对无铅压电陶瓷的强烈需求,铌酸锂陶瓷优良的铁电性能受到广泛关注。
现有技术中,不论通过激光辐照法还是固相烧结法,为了制备致密度高的铌酸锂陶瓷溅射靶材,都需要加入聚乙烯醇,聚乙烯醇高温热解,部分碳元素会残留在铌酸锂陶瓷溅射靶材中,会在铌酸锂陶瓷溅射靶材中引入碳杂质,导致其纯度下降,且聚乙烯醇热解造成环境污染。因此,制备化学组分均一、晶粒细小且尺寸均匀、致密度高以及纯度高的铌酸锂陶瓷溅射靶材是本领域技术人员迫切需要解决的问题,这些问题严重制约铌酸锂陶瓷溅射靶材及铌酸锂薄膜技术领域的发展。
发明内容
针对现有技术存在的不足,本发明的目的在于提供一种导电铌酸锂靶材的制备方法,可制备出高致密度、高纯度、细晶、近化学计量比的铌酸锂导电靶材。
本发明的上述技术目的是通过以下技术方案得以实现的:一种导电铌酸锂靶材的制备方法,包括以下步骤:
S1:按照化学计量比配置C粉、Nb2O5粉末、Li2CO3粉末;
S2:将质量分数0.1%-0.4%的C粉及Nb2O5粉末称重后加入到去离子水中形成浆液,所述浆液固含量10%-40%;然后加入到砂磨机中进行砂磨破碎,砂磨结束后所得粉体细度0.3-0.5μm;对砂磨后的浆液进行离心喷雾造粒;
S3:对造粒后的粉末进行预烧结,使其原位反应得到还原粉末;
S4:将预烧后的还原粉末与计量比的Li2CO3粉末称重后加入到去离子水中形成浆液,所述浆液固含量10%-40%,然后加入到砂磨机中进行砂磨破碎,砂磨结束后所得粉体细度0.3-0.5μm;对砂磨后的浆液进行离心喷雾造粒;
S5:对造粒后的粉末再次进行预烧结,使其原位反应得到还原粉末;
S6:将最终预烧结的还原粉末经过破碎后筛分得到10-25μm的预烧粉末;
S7:将预烧粉末按照产品尺寸计算出所需重量后装入热压石墨模具中,将石墨模具置于真空热压炉的压头正下方,对模具进行预压,然后设定烧结参数进行烧结;
S8:将烧结后的毛坯靶放入真空退火炉中进行真空退火;
S9:退火完成后进行机加工完成产品所需要求。
本发明进一步设置为:在S1步骤中,C粉规格为D50=1-10μm,纯度≥99.99%,片状形貌;Nb2O5粉末规格为D50=5-15μm、纯度≥99.99%、不规则形貌;Li2CO3粉末规格为D50=10-25μm、纯度≥99.99%、不规则形貌。
本发明进一步设置为:在S2步骤中,砂磨破碎时的砂磨转速为1000-2500r/min,砂磨时间1-3h;球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球的一种或多种,装载量为筒体容积的1/3-1/2。
本发明进一步设置为:在S2步骤中,离心喷雾造粒时进风口温度200-300℃、出风口温度90-150℃、雾化盘转速8000-12000r/min、塔体负压为-30--60KPa。
本发明进一步设置为:在S2步骤中,离心喷雾造粒的造粒粘结剂为PVA、PVC、乙基纤维素其中的一种或多种,增塑剂为聚乙二醇或二酸二辛酯,消泡剂为正辛醇或硅基溶液;所述粘结剂的质量百分比为0.5%-1.5%、增塑剂的质量百分比为0.1%-0.5%、消泡剂的质量百分比0.1%-0.5%。
本发明进一步设置为:在S3步骤中,还原温度为900℃-1200℃,烧结气氛为真空或Ar气。
本发明进一步设置为:在S5步骤中,还原温度为500℃-700℃、烧结气氛为真空或Ar气。
本发明进一步设置为:在S4步骤中,所述砂磨破碎的转速为1000-2500r/min,砂磨时间1-3h,球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球的一种或多种,装载量为筒体容积的1/3-1/2。
本发明进一步设置为:在S7步骤中,装模时首先在底部及内部四周垫石墨纸,将粉末分次加入到石墨腔内,每加一层均需使粉末平整,然后再放石墨纸,且石墨模具及石墨纸均需均匀喷涂六方氮化硼脱模剂。
本发明进一步设置为:在S7步骤中,烧结过程包括:将炉体抽真空至100Pa以下,先以5-10℃/min升温至200-300℃并保温1-4h;然后以3-8℃/min升温至500-750℃,保温0.5-4h;再以3-5℃/min升温速率升至800℃-1000℃,然后按照升温速率计算升至高温的时间,以0.5-4MPa/min升压至15-40MPa,使高温和高压同时达到;保温结束后,关闭加热,压力按照1-5MPa/min的速度进行撤压至0MPa;待温度降至室温后将模具取出进行脱模操作。
综上所述,本发明具有以下有益效果:
1、采用C粉末、Nb2O5粉末及Li2CO3粉末作为铌酸锂靶材的原材料,原材料易于获得、价格相对低廉;
2、采用原位烧结反应的方法将Nb2O5粉末预还原,形成缺氧Nb的氧化物,且反应过后C生产CO2挥发,无残留;
3、将预还原的Nb2O5粉末同Li2CO3粉末再次原位烧结反应,形成LiNbO3-x缺氧靶材,由于靶材缺氧,因此在通电时有自由电子移动,因此靶材可以导电,可采用直流磁控溅射靶机进行打靶镀膜,提高生产效率,降低生产成本;
4、采用真空热压的方式对粉末进行固相烧结,并对烧成的毛坯靶进行真空退火处理,可制备出高致密度、高纯度、细晶、近化学计量比的铌酸锂导电靶材。
附图说明
图1为本发明的制备工艺流程图;
图2为装模示意图。
具体实施方式
下面结合附图和实施例,对本发明进行详细描述。
本发明提供一种高品质磁控溅射用导电铌酸锂靶材的制备方法,其工艺流程图参照图1所示,包括以下步骤:
按照化学计量比配置C粉(D50=1-10μm、纯度≥99.99%、片状形貌)、Nb2O5粉末(D50=5-15μm、纯度≥99.99%、不规则形貌)、Li2CO3粉末(D50=10-25μm、纯度≥99.99%、不规则形貌)。本发明的优势在于在C源的引入可以得到缺氧的LiNbO3-x,使得靶材本身导电,且采用真空热压的方式得到致密度高、纯度高、晶粒细小的产品。
将质量分数0.1%-0.4%的C粉及Nb2O5粉末称重后加入到去离子水中形成浆液,浆液固含量10%-40%;通过吸料管加入到砂磨机中进行砂磨破碎,砂磨转速为1000 -2500r/min、砂磨时间1-3h、球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球,装载量为筒体容积的1/3-1/2;砂磨结束后所得粉体细度0.3-0.5μm。
对砂磨后的浆液进行离心喷雾造粒,离心喷雾造粒进风口温度200-300℃,出风口温度90-150℃,雾化盘转速8000-12000r/min,塔体负压为-30~-60KPa;造粒粘结剂为PVA、PVC、乙基纤维素等,增塑剂为聚乙二醇、二酸二辛酯,消泡剂为正辛醇、硅基溶液,粘结剂含量(质量比)为0.5%-1.5%、增塑剂含量(质量比)为0.1%-0.5%、消泡剂(质量比)含量为0.1%-0.5%。
对造粒后的粉末进行预烧结,使其原位反应得到还原粉末,其中还原温度为900℃-1200℃,烧结气氛为真空(真空度<10-2Pa)或Ar气。
将预烧后的C粉+T2O5粉末与计量比的Li2CO3粉末称重后加入到去离子水中形成浆液,浆液固含量10%-40%;通过吸料管加入到砂磨机中进行砂磨破碎,砂磨转速为1000-2500r/min、砂磨时间1-3h、球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球,装载量为筒体容积的1/3-1/2;砂磨结束后所得粉体细度0.3-0.5μm。
对砂磨后的浆液进行离心喷雾造粒,离心喷雾造粒进风口温度200-300℃,出风口温度90-150℃,雾化盘转速8000-12000r/min,塔体负压为-30~-60KPa;造粒粘结剂为PVA、PVC、乙基纤维素等,增塑剂为聚乙二醇、二酸二辛酯,消泡剂为正辛醇、硅基溶液,粘结剂的质量百分数为0.5%-1.5%、增塑剂的质量百分数为0.1%-0.5%、消泡剂的质量百分数为0.1%-0.5%。
对造粒后的粉末再次进行预烧结,使其原位反应得到还原粉末,还原温度为500-700℃、烧结气氛为真空(真空度<10-2Pa)或Ar气。
将最终预烧结的粉末经过破碎后筛分得到10-25μm的粉末。
将预烧粉末按照产品尺寸计算出所需重量后装入热压石墨模具中,装模如附图2所示,装模时首先在底部及内部四周垫石墨纸,将粉末分次加入到石墨腔内,每加一层均需使粉末平整,然后再放石墨纸,且石墨模具及石墨纸均需均匀喷涂六方氮化硼脱模剂。
将石墨模具置于真空热压炉的压头正下方,并对模具进行预压0.5-2MPa,设定烧结参数;首先,将炉体抽真空至100Pa以下,先以5-10℃/min升温至200-300℃并保温1-4h;然后以3-8℃/min升温至500-750℃,保温0.5-4h;再以3℃/min-5℃/min升温速率升至800℃-1000℃然后按照升温速率计算升至高温的时间,以0.5-4MPa/min升压至15-40MPa,使高温和高压同时达到;保温结束后,关闭加热,压力按照1-5MPa/min的速度进行撤压至0MPa,待温度降至室温后将模具取出进行脱模操作。
对烧结的毛坯靶进行简单的处理,去掉表面的石墨纸,然后放入真空退火炉中进行真空退火:首先,将炉体抽真空至100Pa以下,以1-5℃/min升温至300-500℃并保温2-8h进行退火,保温结束后随炉冷却至室温后取出产品,并对毛坯进行各种机加工至所需产品要求。
实施例1
将质量分数0.2%、D50=2μm的C粉及剩余D50=10μm的Nb2O5粉末称重后加入到去离子水中形成浆液,浆液固含量20%;通过吸料管加入到砂磨机中进行砂磨破碎,砂磨转速为2000r/min、砂磨时间2h、球磨介质为0.3mm:0.5mm=1:1的氧化锆球、装载量为筒体容积的1/3;砂磨结束后所得粉体细度0.5μm。
对砂磨后的浆液进行离心喷雾造粒,离心喷雾造粒进风口温度300℃,出风口温度120℃,雾化盘转速11000r/min,塔体负压为-40KPa;所述造粒粘结剂为PVA,增塑剂为聚乙二醇,消泡剂为正辛醇,所述粘结剂含量为0.5%,增塑剂含量为0.2%,消泡剂含量为0.1%。
对造粒后的粉末进行预烧结,使其原位反应得到还原粉末,所述还原温度为1050℃、烧结气氛为真空(真空度<10-2Pa)。
将预烧后的C粉+T2O5粉末与近计量比的D50=15μm的Li2CO3粉末称重后加入到去离子水中形成浆液,浆液固含量15%;通过吸料管加入到砂磨机中进行砂磨破碎,砂磨转速为2500r/min,砂磨时间3h,球磨介质为0.3mm:0.5mm=1:2的氧化锆球,装载量为筒体容积的1/2;砂磨结束后所得粉体细度0.3μm。
对砂磨后的浆液进行离心喷雾造粒,所述离心喷雾造粒进风口温度300℃、出风口温度120℃、雾化盘转速11000r/min、塔体负压为-40KPa;所述造粒粘结剂为PVA,增塑剂为聚乙二醇,消泡剂为正辛醇;所述粘结剂质量含量为0.5%,增塑剂质量含量为0.2%,消泡剂质量含量为0.1%。
对造粒后的粉末再次进行预烧结,使其原位反应得到还原粉末,所述还原温度为650℃、烧结气氛为真空(真空度<10-2Pa)。
将最终预烧结的粉末经过破碎后筛分得到10μm的粉末。
将预烧粉末按照产品尺寸计算出所需重量后装入热压石墨模具中,装模时首先在底部及内部四周垫石墨纸,将粉末分次加入到石墨腔内,每加一层均需使粉末平整,然后再放石墨纸,且石墨模具及石墨纸均需均匀喷涂六方氮化硼脱模剂。
将石墨模具置于真空热压炉的压头正下方,并对模具进行预压0.5Mpa,设定烧结参数:首先,将炉体抽真空至100Pa以下,先以5℃/min升温至250℃并保温1h;然后以3℃/min升温至650℃,保温3h,最后以2℃/min升温至900℃,保温4h;然后按照升温速率计算升至高温的时间,以0.5MPa/min升压至40MPa,使高温和高压同时达到;保温结束后,关闭加热,压力按照1MPa/min的速度进行撤压至0MPa。待温度降至室温后将模具取出进行脱模操作。
对烧结的毛坯靶进行简单的处理,去掉表面的石墨纸,然后放入真空退火炉中进行真空退火:首先,将炉体抽真空至100Pa以下,以1℃/min升温至450℃并保温8h进行退火,保温结束后随炉冷却至室温后取出产品,并对毛坯进行各种机加工至所需产品要求。
实施例2
实施例2基本同实施例1相同,不用之处在于:粉末预烧气氛为Ar气。
对比例1
对比例1的粉末砂磨、造粒及预烧步骤同实施例1相同,不同之处在于最终预烧后的粉末再次进行砂磨造粒;对造粒粉末进行成型操作,成型方式分为两步进:第一步:采用液压机进行模压成型,成型压力为200MPa、保压时间10min;第二步:将模压成型的素坯进行包套密封,抽真空后进行冷等静压,压力为150MPa、保压时间20min。经过两步成型的素坯具有一定的强度,首先对素坯进行机加工至所需形状(按照烧结收缩率留余量)。对加工后的素坯进行无压烧结,烧结气氛为采用Ar气保护,所述烧结温度为1100℃、升温速率2℃/min、保温时间4h;烧结完成后以5℃/min的降温速率降至室温,取出毛坯后进行各种机加工。
对实施例1、实施例2以及对比例1进行性能测试获得如下表1数据:
表1性能测试结果:
致密度/% | 平均晶粒尺寸/μm | 电阻率/Ω.cm | |
实施例1 | 95.3 | 48 | 5.4*10-4 |
实施例2 | 94.9 | 52 | 4.7*10-4 |
对比例1 | 86.7 | 104 | 6.9*10-3 |
以上所述仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种导电铌酸锂靶材的制备方法,其特征在于,包括以下步骤:
S1:按照化学计量比配置C粉、Nb2O5粉末、Li2CO3粉末;
S2:将质量分数0.1%-0.4%的C粉及Nb2O5粉末称重后加入到去离子水中形成浆液,所述浆液固含量10%-40%;然后加入到砂磨机中进行砂磨破碎,砂磨结束后所得粉体细度0.3-0.5μm;对砂磨后的浆液进行离心喷雾造粒;
S3:对造粒后的粉末进行预烧结,使其原位反应得到还原粉末;
S4:将预烧后的还原粉末与计量比的Li2CO3粉末称重后加入到去离子水中形成浆液,所述浆液固含量10%-40%,然后加入到砂磨机中进行砂磨破碎,砂磨结束后所得粉体细度0.3-0.5μm;对砂磨后的浆液进行离心喷雾造粒;
S5:对造粒后的粉末再次进行预烧结,使其原位反应得到还原粉末;
S6:将最终预烧结的还原粉末经过破碎后筛分得到10-25μm的预烧粉末;
S7:将预烧粉末按照产品尺寸计算出所需重量后装入热压石墨模具中,将石墨模具置于真空热压炉的压头正下方,对模具进行预压,然后设定烧结参数进行烧结;
S8:将烧结后的毛坯靶放入真空退火炉中进行真空退火;
S9:退火完成后进行机加工完成产品所需要求。
2.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S1步骤中,C粉规格为D50=1-10μm,纯度≥99.99%,片状形貌;Nb2O5粉末规格为D50=5-15μm、纯度≥99.99%、不规则形貌;Li2CO3粉末规格为D50=10-25μm、纯度≥99.99%、不规则形貌。
3.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S2步骤中,砂磨破碎时的砂磨转速为1000-2500r/min,砂磨时间1-3h;球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球的一种或多种,装载量为筒体容积的1/3-1/2。
4.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S2步骤中,离心喷雾造粒时进风口温度200-300℃、出风口温度90-150℃、雾化盘转速8000-12000r/min、塔体负压为-30--60KPa。
5.根据权利要求1或4所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S2步骤中,离心喷雾造粒的造粒粘结剂为PVA、PVC、乙基纤维素其中的一种或多种,增塑剂为聚乙二醇或二酸二辛酯,消泡剂为正辛醇或硅基溶液。
6.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S3步骤中,还原温度为900℃-1200℃,烧结气氛为真空或Ar气。
7.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S5步骤中,还原温度为500℃-700℃、烧结气氛为真空或Ar气。
8.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S4步骤中,所述砂磨破碎的转速为1000-2500r/min,砂磨时间1-3h,球磨介质为0.3mm、0.5mm、1mm、2mm的氧化锆球的一种或多种,装载量为筒体容积的1/3-1/2。
9.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S7步骤中,装模时首先在底部及内部四周垫石墨纸,将粉末分次加入到石墨腔内,每加一层均需使粉末平整,然后再放石墨纸,且石墨模具及石墨纸均需均匀喷涂六方氮化硼脱模剂。
10.根据权利要求1所述的一种导电铌酸锂靶材的制备方法,其特征在于:在S7步骤中,烧结过程包括:将炉体抽真空至100Pa以下,先以5-10℃/min升温至200-300℃并保温1-4h;然后以3-8℃/min升温至500-750℃,保温0.5-4h,再以3 -5℃/min升温速率升至800℃-1000℃;然后按照升温速率计算升至高温的时间,以0.5-4MPa/min升压至15-40MPa,使高温和高压同时达到;保温结束后,关闭加热,压力按照1-5MPa/min的速度进行撤压至0MPa;待温度降至室温后将模具取出进行脱模操作。
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