CN105801101A - 一种Co：ZnAl2O4透明陶瓷及其制备方法和应用 - Google Patents

一种Co：ZnAl2O4透明陶瓷及其制备方法和应用 Download PDF

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CN105801101A
CN105801101A CN201610126935.3A CN201610126935A CN105801101A CN 105801101 A CN105801101 A CN 105801101A CN 201610126935 A CN201610126935 A CN 201610126935A CN 105801101 A CN105801101 A CN 105801101A
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付萍
王子颖
王戈明
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Tianjin Institute of Advanced Equipment of Tsinghua University
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Abstract

本发明提供一种Co:ZnAl2O4透明陶瓷，其化学组成为(Zn1‑xCox)Al2O4，其中0.0005≤x≤0.002，该透明陶瓷可用于固体激光器被动Q开关，其制备方法包括：将5‑20份NH4Al(SO4)2·12H2O、5‑20份ZnSO4·7H2O、1‑5份Co(NO3)·6H2O、5‑20份去离子水混合均匀后放入马弗炉内，在1100‑1400℃烧结1‑6h得(Zn1‑xCox)Al2O4纳米粉体，所述纳米粉体与0.1‑5份TEOS、乙醇溶剂混合均匀后经研磨、干压成型、冷等静压处理得陶瓷坯体，所述陶瓷坯体在1200‑1400℃烧结5‑30min，即得。该透明陶瓷具有优异的光学性能、物化性能、高低温稳定性以及比透明微晶玻璃更好的抗热震性和抗激光破坏性，其在被动调Q开关技术中具有良好的性能。

Description

一种Co:ZnAl2O4透明陶瓷及其制备方法和应用
技术领域
本发明涉及透明陶瓷技术领域，具体涉及一种Co:ZnAl2O4透明陶瓷及其制备方法和应用。
背景技术
掺铒激光玻璃发射的1.54μm激光，由于具有高的大气透过能力和极好的人眼安全特性，在激光测距、光通信以及医疗等领域具有广泛的应用。其中的大多数应用，均需要高峰值功率的纳米级脉冲，即需要实现调Q。被动调Q具有操作简单、高效稳定，成本较低等优点。良好的被动调Q可饱和吸收材料应具有如下性能：在激光波段具有较短的驰豫时间，较大的基态吸收截面和较小的激发态吸收截面，同时具有稳定的物化性能、良好的导热性、抗激光损伤性以及稳定的高低温特性等。
用于固体激光器的被动调Q技术是通过在谐振腔内插入可饱和吸收体材料来实现调Q运转的。目前，被动调Q技术的材料主要有有机染料、色心晶体及透明微晶玻璃等。其中，有机染料热稳定性差、易退化，导致输出的调Q脉冲极不稳定；色心晶体易褪色；掺Co2+离子的晶体(如Y3Al5Ol2，MgAl2O4和LaMgAl11O19等)制备难度大、掺杂不易均匀、成本高；掺Co2+离子的透明微晶玻璃需要在高温下熔制，制备工艺过程困难，较难获得很好的光学均匀性和较低的光学损耗。此外，包含玻璃的微晶玻璃其抗热震性和抗激光破坏性有一定的局限性，限制了其应用。
最近几年发展起来的ZnAl2O4及MgAl2O4等透明陶瓷，由于其优异的热学和力学性能、高度的透明度，在激光领域具有巨大的应用前景。Co2+在1.3-1.6μm波段具有强的吸收特性，主要用作1.34μm和1.54μm波段激光器调Q材料的激活离子。但是，目前透明陶瓷的制备条件比较苛刻，杂质和孔隙的引入会影响陶瓷的透明度。如何实现掺杂离子的引入而不破坏陶瓷的透明度及其他性能，是掺杂离子透明陶瓷制备工艺中需要解决的首要问题。
发明内容
本发明的目的在于解决现有透明陶瓷制备工艺困难、固体激光器被动调Q技术材料存在的不足，提供一种Co:ZnAl2O4透明陶瓷及其制备方法和应用。该透明陶瓷具有优异的光学性能、物化性能、高低温稳定性以及比透明微晶玻璃更好的抗热震性和抗激光破坏性，其在被动调Q开关技术中具有良好的性能。
本发明解决其技术问题的方案如下：
一种Co:ZnAl2O4透明陶瓷，其化学组成为(Zn1-xCox)Al2O4，其中x的取值范围为0.0005≤x≤0.002。
所述Co:ZnAl2O4透明陶瓷作为固体激光器被动Q开关基质材料的应用。
一种Co:ZnAl2O4透明陶瓷的制备方法，包括以下步骤：a)向烧杯中加入一定量的NH4Al(SO4)2·12H2O、ZnSO4·7H2O、Co(NO3)·6H2O和去离子水，搅拌一定时间使各物质充分溶解得到混合溶液；b)将混合溶液置于坩埚中并放进马弗炉内加热至一定温度后保温烧结，烧结完成后自然冷却至室温并过筛，得到(Zn1-xCox)Al2O4纳米粉体；c)将一定量TEOS分散于乙醇溶剂中，将其与步骤b)制得的(Zn1-xCox)Al2O4纳米粉体混合均匀，所得混合物经研磨、过筛、干压成型、冷等静压处理得陶瓷坯体；d)将陶瓷坯体置于放电等离子烧结炉中烧结得(Zn1-xCox)Al2O4透明陶瓷。
优选的，各物质的用量按重量份数计为5-20份NH4Al(SO4)2·12H2O，5-20份ZnSO4·7H2O，1-5份Co(NO3)·6H2O，5-20份去离子水，0.1-5份TEOS。
步骤a)中搅拌温度为40-100℃，搅拌速度20-1000rpm，搅拌时间0.5-6h。
步骤b)中马弗炉的升温速率为2-10℃/min，升温至1100-1400℃并保温1-6h，过筛所使用的筛网为200目。
步骤c)干压成型时压片机的压力控制在5-75MPa，冷等静压处理时的压力控制在100-500MPa。
步骤d)放电等离子烧结炉升温速率为2-20℃/min，陶瓷坯体烧结压力20-200MPa，保温温度1200-1400℃，保温时间5-30min。
本发明将TEOS引入到掺Co透明陶瓷的制备中，利用TEOS的溶胶凝胶反应生成二氧化硅胶体粒子。二氧化硅胶体粒子在高温烧结过程中具有良好的流动性，一方面可以填充Co:ZnAl2O4纳米粉体烧结过程中留下的孔洞，另一方面透明性优异的二氧化硅可以与Co离子相互作用，减弱Co对陶瓷透明性的影响。本发明提供的Co:ZnAl2O4透明陶瓷制备工艺简单、周期短、能耗低、成本低，陶瓷的透明性及力学性能没有受到掺杂离子的影响，用于固体激光器被动Q开关具有较高的经济效益和社会效益。
附图说明
图1为本发明实施例2制备的(Zn0.999Co0.001)Al2O4透明陶瓷实物照片。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图及实施例对本发明作进一步详细描述，但这些实施例均不构成对本发明的限制。
实施例1
一种Co:ZnAl2O4透明陶瓷，化学组成为(Zn0.9995Co0.0005)Al2O4，其制备方法如下：
首先按重量份数计称取5份NH4Al(SO4)2·12H2O，5份ZnSO4·7H2O和1份Co(NO3)·6H2O，将上述物质放入烧杯中，加入5份去离子水。将烧杯置于磁力搅拌器上，在40℃以20rmp的搅拌速度保温搅拌0.5h，使各物质充分溶解并分散均匀。将混合好的溶液置于坩埚中，将坩埚放入马弗炉内，以2℃/min的升温速率升温至1100℃，保温1h，然后自然冷却至室温，得到(Zn0.9995Co0.0005)Al2O4纳米粉体，粉体过200目筛备用。将0.1份的TEOS(正硅酸乙酯)分散于乙醇溶剂中，与粉体混合后研磨、过筛，在压片机上以5MPa的压力干压成型，再经100MPa冷等静压处理制成陶瓷坯体。将陶瓷坯体放入放电等离子烧结炉中烧结，升温速率为2℃/min，保温温度为1200℃，烧结压力为20MPa，烧结保温时间为5min。烧结完成后得到(Zn0.9995Co0.0005)Al2O4透明陶瓷。本发明各实施例所用的化学原料均为分析纯。
经分析测试，本实施例制备的(Zn0.9995Co0.0005)Al2O4透明陶瓷在可见光波段550nm处的直线透过率为55％，在红外波段2500nm处的直线透过率为80％。
实施例2
一种Co:ZnAl2O4透明陶瓷，化学组成为(Zn0.999Co0.001)Al2O4，其制备方法如下：
首先按重量份数计称取20份NH4Al(SO4)2·12H2O，20份ZnSO4·7H2O和5份Co(NO3)·6H2O，将上述物质放入烧杯中，加入20份去离子水。将烧杯置于磁力搅拌器上，在100℃以1000rmp的搅拌速度保温搅拌6h，使各物质充分溶解并分散均匀。将混合好的溶液置于坩埚中，将坩埚放入马弗炉内，以10℃/min的升温速率升温至1400℃，保温6h，然后自然冷却至室温，得到(Zn0.999Co0.001)Al2O4纳米粉体，粉体过200目筛备用。将5份的TEOS分散于乙醇溶剂中，与粉体混合后研磨、过筛，在压片机上以75MPa的压力干压成型，再经500MPa冷等静压处理制成陶瓷坯体。将陶瓷坯体放入放电等离子烧结炉中烧结，升温速率为20℃/min，保温温度为1400℃，烧结压力为200MPa，烧结保温时间为30min。烧结完成后得到(Zn0.999Co0.001)Al2O4透明陶瓷，实物照片如图1所示。
经分析测试，本实施例制备的(Zn0.999Co0.001)Al2O4透明陶瓷在可见光波段550nm处的直线透过率为60％，在红外波段2500nm处的直线透过率为85％。
实施例3
一种Co:ZnAl2O4透明陶瓷，化学组成为(Zn0.9985Co0.0015)Al2O4，其制备方法如下：
首先按重量份数计称取16份NH4Al(SO4)2·12H2O，8份ZnSO4·7H2O和2份Co(NO3)·6H2O，将上述物质放入烧杯中，加入15份去离子水。将烧杯置于磁力搅拌器上，在70℃以200rmp的搅拌速度保温搅拌6h，使各物质充分溶解并分散均匀。将混合好的溶液置于坩埚中，将坩埚放入马弗炉内，以10℃/min的升温速率升温至1300℃，保温3h，然后自然冷却至室温，得到(Zn0.9985Co0.0015)Al2O4纳米粉体，粉体过200目筛备用。将2份的TEOS分散于乙醇溶剂中，与粉体混合后研磨、过筛，在压片机上以50MPa的压力干压成型，再经250MPa冷等静压处理制成陶瓷坯体。将陶瓷坯体放入放电等离子烧结炉中烧结，升温速率为20℃/min，保温温度为1240℃，烧结压力为100MPa，烧结保温时间为15min。烧结完成后得到(Zn0.9985Co0.0015)Al2O4透明陶瓷。
经分析测试，本实施例制备的(Zn0.9985Co0.0015)Al2O4透明陶瓷在可见光波段550nm处的直线透过率为63％，在红外波段2500nm处的直线透过率为80％。
实施例4
一种Co:ZnAl2O4透明陶瓷，化学组成为(Zn0.998Co0.002)Al2O4，其制备方法如下：
首先按重量份数计称取20份NH4Al(SO4)2·12H2O，10份ZnSO4·7H2O和3份Co(NO3)·6H2O，将上述物质放入烧杯中，加入15份去离子水。将烧杯置于磁力搅拌器上，在80℃以250rmp的搅拌速度保温搅拌5h，使各物质充分溶解并分散均匀。将混合好的溶液置于坩埚中，将坩埚放入马弗炉内，以5℃/min的升温速率升温至1400℃，保温1h，然后自然冷却至室温，得到(Zn0.998Co0.002)Al2O4纳米粉体，粉体过200目筛备用。将1份的TEOS分散于乙醇溶剂中，与粉体混合后研磨、过筛，在压片机上以45MPa的压力干压成型，再经250MPa冷等静压处理制成陶瓷坯体。将陶瓷坯体放入放电等离子烧结炉中烧结，升温速率为8℃/min，保温温度为1260℃，烧结压力为100MPa，烧结保温时间为20min。烧结完成后得到(Zn0.998Co0.002)Al2O4透明陶瓷。
经分析测试，本实施例制备的(Zn0.998Co0.002)Al2O4透明陶瓷在可见光波段550nm处的直线透过率为58％，在红外波段2500nm处的直线透过率为82％。
本发明实施例制备的Co:ZnAl2O4透明陶瓷具有优良的光学性能，适用于制作固体激光器被动Q开关。

Claims (8)

1.一种Co:ZnAl2O4透明陶瓷，其特征在于：该透明陶瓷的化学组成为(Zn1-xCox)Al2O4，其中x的取值范围为0.0005≤x≤0.002。
2.权利要求1所述的Co:ZnAl2O4透明陶瓷作为固体激光器被动Q开关基质材料的应用。
3.一种Co:ZnAl2O4透明陶瓷的制备方法，其特征在于包括以下步骤：a)向烧杯中加入一定量的NH4Al(SO4)2·12H2O、ZnSO4·7H2O、Co(NO3)·6H2O和去离子水，搅拌一定时间使各物质充分溶解得到混合溶液；b)将混合溶液置于坩埚中并放进马弗炉内加热至一定温度后保温烧结，烧结完成后自然冷却至室温并过筛，得到(Zn1-xCox)Al2O4纳米粉体；c)将一定量TEOS分散于乙醇溶剂中，将其与步骤b)制得的(Zn1-xCox)Al2O4纳米粉体混合均匀，所得混合物经研磨、过筛、干压成型、冷等静压处理得陶瓷坯体；d)将陶瓷坯体置于放电等离子烧结炉中烧结得(Zn1-xCox)Al2O4透明陶瓷。
4.如权利要求3所述的Co:ZnAl2O4透明陶瓷的制备方法，其特征在于：各物质的用量按重量份数计为5-20份NH4Al(SO4)2·12H2O，5-20份ZnSO4·7H2O，1-5份Co(NO3)·6H2O，5-20份去离子水，0.1-5份TEOS。
5.如权利要求3所述的Co:ZnAl2O4透明陶瓷的制备方法，其特征在于：步骤a)中搅拌温度为40-100℃，搅拌速度20-1000rpm，搅拌时间0.5-6h。
6.如权利要求3所述的Co:ZnAl2O4透明陶瓷的制备方法，其特征在于：步骤b)中马弗炉的升温速率为2-10℃/min，升温至1100-1400℃并保温1-6h，过筛所使用的筛网为200目。
7.如权利要求3所述的Co:ZnAl2O4透明陶瓷的制备方法，其特征在于：步骤c)干压成型时压片机的压力控制在5-75MPa，冷等静压处理时的压力控制在100-500MPa。
8.如权利要求3所述的Co:ZnAl2O4透明陶瓷的制备方法，其特征在于：步骤d)放电等离子烧结炉升温速率为2-20℃/min，陶瓷坯体烧结压力20-200MPa，保温温度1200-1400℃，保温时间5-30min。
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