CN116639970A - 一种钙锶铝氧系列陶瓷靶材的制备方法 - Google Patents
一种钙锶铝氧系列陶瓷靶材的制备方法 Download PDFInfo
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- -1 calcium strontium aluminum oxygen series Chemical class 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000013077 target material Substances 0.000 title abstract description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 48
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 35
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- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 14
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- KDYIRGWWWUGPCM-UHFFFAOYSA-N aluminum calcium strontium oxygen(2-) Chemical class [O-2].[Ca+2].[Sr+2].[Al+3] KDYIRGWWWUGPCM-UHFFFAOYSA-N 0.000 claims abstract description 7
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Abstract
本发明公开一种钙锶铝氧系列陶瓷靶材的制备方法，将硝酸锶(四水硝酸钙)、九水硝酸铝、柠檬酸溶于去离子水溶剂中，其中，柠檬酸作为络合剂，乙二醇为分散剂，放置在恒温磁力搅拌器上，加热搅拌形成湿凝胶，放入干燥箱烘干；最后将凝胶研磨，预烧处理得到纳米粉体；将纳米粉体研磨并对其进行压片处理，再进行二次烧结即得锶钙铝氧系列陶瓷靶材。本发明采用溶剂凝胶法保证了各组分在分子级别的混合，得到的陶瓷靶材致密度好，成分、晶粒尺寸均一，此外，本法工艺简单，重复性好，选用的化学试剂价格低廉易得。
Description
技术领域
本发明涉及一种钙锶铝氧系列陶瓷靶材的制备方法，属于功能陶瓷技术领域。
背景技术
钙锶铝氧系列陶瓷是一种多用途的化合物：在陶瓷领域可以制备透明陶瓷；在纳米柔性薄膜领域可做为水溶性材料用于制备各种独立式薄膜，方便薄膜衬底剥离而不损伤薄膜；在建筑领域，其粉体可以用于水泥材料，提高水泥材料质量；在钢铁行业可用于耐火浇筑材料，在预防放射性领域用于制备辐射屏蔽混凝土的粘结材料。在发光材料领域用来作为荧光发光材料使用，在不需要任何掺杂的条件下能够激发出红色荧光，它的长效红色荧光能力可以用来有效消除交流电驱动发光二极管的发光闪烁问题；氧化物红色荧光粉在制备白色发光二极管上具有成本低廉，发光效率高，热发光稳定，易合成等的优势。
现有的钙锶铝氧系列陶瓷是通过固相法制备得到，固相法制备的陶瓷往往晶粒尺寸不均匀，致密度低，成相不纯，容易出现杂质，从而对后续应用造成不利影响。本发明提出的钙锶铝氧系列陶瓷靶材，采用溶胶凝胶方法，配合精细的烧结制度，克服以上制备过程中粉体均匀性差、块体致密度低、成相不纯等问题。
发明内容
本发明的目的在于提供一种钙锶铝氧系列陶瓷靶材的制备方法，本发明采用溶胶凝胶方法实现在较少合成工艺，致密度好，晶粒大小合适的钙锶铝氧系列靶材，在1200～1450℃得到钙锶铝氧系列靶材，此外，本法重复性好，选用的化学试剂价格低廉易得。
本发明所述的钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤：
(1)将硝酸锶、九水硝酸铝、四水硝酸钙按钙锶铝氧系列的化学计量配比进行称量，在密闭空间称量，然后称量柠檬酸，柠檬酸与钙锶铝氧系列的金属阳离子的摩尔比为1:1；在密闭空间称量，防止气流干扰其他等外界因素影响实验结果。
(2)将步骤(1)所称量的原料先后溶于去离子水溶剂中，均匀搅拌，经过5～10min溶解后，加入一定比例的乙二醇溶剂作为分散剂，经过一段时间，搅拌均匀。
(3)将步骤(2)溶液进行搅拌加热一段时间，待溶剂蒸发形成胶体，将胶体置于干燥恒温烘箱中发泡得到凝胶。
(4)将步骤(3)中的凝胶充分磨碎，得到钙锶铝氧系列陶瓷粉体。
(5)对步骤(4)的钙锶铝氧系列陶瓷粉体放入箱式炉进行预烧处理，得到初次煅烧粉体。
(6)将步骤(5)中的初次煅烧粉体放入特定模具中，进行加压处理，制成钙锶铝氧系列陶瓷块体。
(7)将步骤(6)所得陶瓷块体进行二次煅烧，得到钙锶铝氧系列陶瓷靶材。
本发明所述步骤(1)称量误差控制在±0.0004g范围内，柠檬酸与钙锶铝氧系列的金属阳离子摩尔比为1:1。
本发明所述步骤(2)去离子水与乙二醇的体积比值为10:1～3:1，搅拌时间15～45min。
本发明所述步骤(3)中混合溶液的加热温度为80～100℃，加热时长为0.5～2h，凝胶干燥温度为50～100℃，干燥时长为12～24h。
本发明所述步骤(4)中研磨时间0.5～1h。
本发明所述步骤(5)中初次烧结温度为400～600℃，加热时长为2～8h。
本发明所述步骤(6)中称量粉体质量1.5～6g，选用模具规格20～30mm圆形模具，使用压片机3～4Mpa，加压时间20～30min。
本发明所述步骤(7)中二次煅烧温度为1200～1450℃，加热时长为2～12h。
本发明有益效果：
本发明所使用的原料价格低廉，容易获得。其次，重复性好，易于控制陶瓷质量；所使用的烧结温度低于氧化物熔点，便于节约能源；烧结时间短，利于提高生产率。制备得到的钙锶铝氧系列陶瓷靶材，可以用于透明陶瓷，采用本发明的方法制备得到的纳米级别的钙锶铝氧系列陶瓷靶材，质量良好、颗粒均匀，靶材致密度高。在柔性薄膜生长过程中，使用钙锶铝氧系列陶瓷靶材生长的薄膜，易于外延生长，均一性好，为后续方便衬底完全剥离而不损伤薄膜提供条件。使用钙锶铝氧系列陶瓷靶材制备水泥建筑材料，可以提高产品质量，提升耐用性，使用钙锶铝氧系列陶瓷靶材制备荧光粉具有成分均匀，合成相纯，在纳米尺度上颗粒大小均一等特点。
附图说明
图1为实施例1初次烧结粉体样品的XRD图；
图2为实施例1二次煅烧样品的XRD图；
图3为实施例1二次煅烧样品的SEM照片(10000倍)；
图4为实施例2初次烧结粉体样品的XRD图；
图5为实施例2二次煅烧样品的XRD图；
图6为实施例2二次煅烧样品的SEM照片(40000倍)；
图7为实施例3初次烧结粉体样品的XRD图；
图8为实施例3二次煅烧样品的XRD图；
图9为实施例3二次煅烧样品的SEM照片(1500倍)；
图10为实施例4初次烧结粉体样品的XRD图；
图11为实施例4二次煅烧样品的XRD图；
图12为实施例4二次煅烧样品的SEM照片(1500倍)。
具体实施方式
下面结合附图及具体实施例为本发明作进一步详细说明，但本发明的保护范围不限于所述内容。
实施例1
本实施例所述溶胶凝胶法钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤:
(1)将硝酸锶、九水硝酸铝按Sr3Al2O6的化学计量配比进行称量，按柠檬酸与Sr3Al2O6的金属阳离子摩尔比为1:1的比例称取柠檬酸。
(2)将步骤(1)所称量的硝酸锶、九水硝酸铝、柠檬酸溶于去离子水溶剂中，同时用磁力搅拌器搅拌均匀，等固体原料溶解，得到透明溶液，经过10min搅拌后，然后加入一定量的乙二醇溶剂，去离子水与乙二醇溶剂的体积比值为5:1，搅拌15min，得到混合溶液。
(3)将步骤(2)所得混合溶液进行加热搅拌，加热时长为0.5h，加热温度为80℃，得到胶体，将胶体置于烘箱中脱水发泡得到干凝胶，干燥温度为100℃，干燥时长为12h，干燥气氛为常压、空气。
(4)将步骤(3)中的凝胶充分磨碎1h，得到Sr3Al2O6陶瓷粉体。
(5)对步骤(4)的Sr3Al2O6陶瓷粉体进行预烧处理，初次烧结温度为600℃，加热时长为8h，得到Sr3Al2O6初次煅烧粉体。
(6)将步骤(5)中的Sr3Al2O6初次煅烧粉体称量6g，放入30mm的圆形模具中，使用压片机在3Mpa的压力下，加压20min，形成Sr3Al2O6陶瓷靶材。
(7)将步骤(6)所得Sr3Al2O6陶瓷靶材放入箱式炉距离热电偶合适位置，其中二次煅烧温度为1300℃，加热时长12h，烧结气氛为常压、空气气氛，得到Sr3Al2O6陶瓷靶材。
本实施例制备得到的Sr3Al2O6陶瓷纳米粉体的预烧XRD图谱如图1所示，由图可以看出预烧粉体杂相较少。
本实施例制备得到的Sr3Al2O6陶瓷靶材的二次煅烧XRD图谱如图2所示，可以看出最终成相较纯。
本实施例二次煅烧制备得到的Sr3Al2O6陶瓷靶材的SEM照片如图3所示，可以看出陶瓷靶材颗粒均匀。
实施例2
本实施例所述溶胶凝胶法钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤:
(1)将九水硝酸铝、四水硝酸钙按Ca3Al2O6的化学计量配比进行称量，柠檬酸与Ca3Al2O6的金属阳离子摩尔比为1:1。
(2)将步骤(1)所称量的四水硝酸钙、九水硝酸铝、柠檬酸溶于去离子水溶剂中，同时用磁力搅拌器搅拌均匀，等固体原料溶解，得到透明溶液，经过10min搅拌后，然后加入一定量的乙二醇溶剂，去离子水与乙二醇溶剂的体积比值为5:1，搅拌30min，得到混合溶液。
(3)将步骤(2)所得混合溶液进行加热搅拌，加热时长为1h，加热温度为90℃，得到胶体，将胶体置于烘箱中脱水发泡得到干凝胶，干燥温度为90℃，干燥时长为24h，干燥气氛为常压、空气。
(4)将步骤(3)中的凝胶充分磨碎0.5h，得到Ca3Al2O6陶瓷粉体。
(5)对步骤(4)的Ca3Al2O6陶瓷粉体进行预烧处理，初次烧结温度为400℃，加热时长为2h，得到Ca3Al2O6初次煅烧粉体。
(6)将步骤(5)中的Ca3Al2O6初次煅烧粉体称量2g，放入20mm的圆形模具中，使用压片机在3Mpa的压力下，加压30min，形成Ca3Al2O6陶瓷块体。
(7)将步骤(6)所得Ca3Al2O6陶瓷块体放入箱式炉距离热电偶合适位置，其中二次煅烧温度为1350℃，加热时长为12h，烧结气氛为常压、空气气氛，得到Ca3Al2O6陶瓷靶材。
本实施例制备得到的Ca3Al2O6陶瓷纳米粉体的预烧XRD图谱如图4所示，由图可以看出预烧粉体杂相较少。
本实施例制备得到的Ca3Al2O6陶瓷靶材的二次煅烧XRD图谱如图5所示，可以看出成相较纯。
本实施例二次煅烧制备得到的Ca3Al2O6陶瓷靶材的SEM照片如图6所示，可以看出成相颗粒均匀。
实施例3
本实施例所述溶胶凝胶法钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤:
(1)将硝酸锶、四水硝酸钙、九水硝酸铝按Sr2CaAl2O6的化学计量配比进行称量，柠檬酸与Sr2CaAl2O6的金属阳离子摩尔比为1:1。
(2)将步骤(1)所称量的四水硝酸钙、九水硝酸铝、柠檬酸溶于去离子水溶剂中，同时用磁力搅拌器搅拌均匀，等固体原料溶解，得到透明溶液，经过10min搅拌后，然后加入一定量的乙二醇溶剂，去离子水与乙二醇溶剂的体积比值为5:1，搅拌30min，得到混合溶液。
(3)将步骤(2)所得混合溶液进行加热搅拌，加热时长为1h，加热温度为90℃，得到胶体，将胶体置于烘箱中脱水发泡得到干凝胶，干燥温度为90℃，干燥时长为24h，干燥气氛为常压、空气。
(4)将步骤(3)中的凝胶充分磨碎0.5h，得到Sr2CaAl2O6陶瓷粉体。
(5)对步骤(4)的Sr2CaAl2O6陶瓷粉体进行预烧处理，初次烧结温度为400℃，加热时长为2h，得到Sr2CaAl2O6初次煅烧粉体。
(6)将步骤(5)中的Sr2CaAl2O6初次煅烧粉体称量2g，放入20mm的圆形模具中，使用压片机在3Mpa的压力下，加压30min，形成Sr2CaAl2O6陶瓷块体。
(7)将步骤(6)所得Sr2CaAl2O6陶瓷块体放入箱式炉距离热电偶合适位置，其中二次煅烧温度为1400℃，加热时长为12h，烧结气氛为常压、空气气氛，得到Sr2CaAl2O6陶瓷靶材。
本实施例初次烧结粉体样品制备得到的Sr2CaAl2O6陶瓷纳米粉体的XRD图谱如图7所示，可以看出最终成相较纯。
本实施例二次煅烧制备得到的Sr2CaAl2O6陶瓷靶材的XRD图谱如图8所示，可以看出成相较纯。
本实施例制备得到的Sr2CaAl2O6陶瓷靶材的SEM照片如图9所示，可以看出陶瓷靶材颗粒均匀。
实施例4
本实施例所述溶胶凝胶法钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤:
(1)将硝酸锶、四水硝酸钙、九水硝酸铝按SrCa2Al2O6的化学计量配比进行称量，柠檬酸与SrCa2Al2O6的金属阳离子摩尔比为1:1。
(2)将步骤(1)所称量的四水硝酸钙、九水硝酸铝、柠檬酸溶于去离子水溶剂中，同时用磁力搅拌器搅拌均匀，等固体原料溶解，得到透明溶液，经过10min搅拌后，然后加入一定量的乙二醇溶剂，去离子水与乙二醇溶剂的体积比值为5:1，搅拌30min，得到混合溶液。
(3)将步骤(2)所得混合溶液进行加热搅拌，加热时长为1h，加热温度为90℃，得到胶体，将胶体置于烘箱中脱水发泡得到干凝胶，干燥温度为90℃，干燥时长为24h，干燥气氛为常压、空气。
(4)将步骤(3)中的凝胶充分磨碎0.5h，得到SrCa2Al2O6陶瓷粉体。
(5)对步骤(4)的SrCa2Al2O6陶瓷粉体进行预烧处理，初次烧结温度为400℃，加热时长为2h，得到SrCa2Al2O6初次煅烧粉体。
(6)将步骤(5)中的SrCa2Al2O6初次煅烧粉体称量2g，放入20mm的圆形模具中，使用压片机在3Mpa的压力下，加压30min，形成SrCa2Al2O6陶瓷块体。
(7)将步骤(6)所得SrCa2Al2O6陶瓷块体放入箱式炉距离热电偶合适位置，其中二次煅烧温度为1400℃，加热时长为12h，烧结气氛为常压、空气气氛，得到SrCa2Al2O6陶瓷靶材。
本实施例中二次烧结的温度为1400℃，其他步骤及参数与实施例3相同。
本实施例初次烧结粉体样品制备得到的SrCa2Al2O6陶瓷纳米粉体的XRD图谱如图10所示，由图可以看出预烧粉体杂相较少。
本实施例二次煅烧制备得到的SrCa2Al2O6陶瓷靶材的XRD图谱如图11所示，由图可以看出成相较纯。
本实施例制备得到的SrCa2Al2O6陶瓷靶材的SEM照片如图12所示，由图可以看出陶瓷靶材颗粒均匀。
对比实施例1
本实施例所述固相法钙锶铝氧系列陶瓷靶材的制备方法，具体包括以下步骤:
(1)将碳酸锶、碳酸钙、氧化铝按SrCa2Al2O6的化学计量配比进行称量。
(2)将步骤(1)所称量的碳酸锶、氧化铝混合，然后将混合物在球磨机中均匀化12小时。
(3)将步骤(2)所得混合物取出，放入清洁的研钵中，添加粘结剂，研磨30min使粘合剂充分混合。
(4)将步骤(3)中的混合物称量6g，放入30mm的圆形模具中，使用压片机在3Mpa的压力下，加压20min，形成SrCa2Al2O6陶瓷靶材。
(5)将步骤(4)所得SrCa2Al2O6陶瓷靶材放入箱式炉距离热电偶合适位置，其中煅烧温度为1400℃，加热时长12h，烧结气氛为常压、空气气氛，得到SrCa2Al2O6陶瓷靶材。
本实施例制备得到的SrCa2Al2O6陶瓷杂相较多，成相不纯，陶瓷靶材颗粒不均匀，致密性差，短时间陶瓷靶材容易风化成粉末，不利于后续的实际应用。
Claims (7)
1.一种钙锶铝氧系列陶瓷靶材的制备方法，其特征在于，具体包括以下步骤：
(1)将硝酸锶、九水硝酸铝、四水硝酸钙按钙锶铝氧系列的化学计量配比进行称量，在密闭空间称量，然后称量柠檬酸，柠檬酸与钙锶铝氧系列的金属阳离子的摩尔比为1:1；
(2)将步骤(1)所称量的原料先后溶于去离子水溶剂中，均匀搅拌，完全溶解后，加入乙二醇溶剂作为分散剂，搅拌均匀；
(3)将步骤(2)溶液进行搅拌加热一段时间，待溶剂蒸发形成胶体，将胶体置于干燥恒温烘箱中发泡得到凝胶；
(4)将步骤(3)中的凝胶充分磨碎，得到钙锶铝氧系列陶瓷粉体；
(5)对步骤(4)的钙锶铝氧系列陶瓷粉体放入箱式炉进行预烧处理，得到初次煅烧粉体；
(6)将步骤(5)中的初次煅烧粉体放入特定模具中，进行加压处理，制成钙锶铝氧系列陶瓷块体；
(7)将步骤(6)所得陶瓷块体放入箱式炉中进行二次煅烧，得到钙锶铝氧系列陶瓷靶材。
2.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：步骤(2)中去离子水与乙二醇的体积比值为10:1～3:1，搅拌时间15～45min。
3.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：所述步骤(3)中混合溶液的加热温度为80～100℃，加热时长为0.5～2h，凝胶干燥温度为50～100℃，干燥时长为12～24h。
4.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：所述步骤(4)中研磨时间0.5～1h。
5.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：所述步骤(5)中初次烧结温度为400～600℃，加热时长为2～8h。
6.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：所述步骤(6)中压片机的压力为3～4Mpa，加压时间20～30min。
7.根据权利要求1所述钙锶铝氧系列陶瓷靶材的制备方法，其特征在于：所述步骤(7)中二次煅烧温度为1200～1450℃，加热时长为2～12h。
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