CN115477539A - 一种氟化钙透明陶瓷及低温制备方法 - Google Patents
一种氟化钙透明陶瓷及低温制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 14
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title abstract description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 title abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
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- 229910004261 CaF 2 Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
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- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
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Abstract
本发明公开了一种氟化钙透明陶瓷及低温制备方法，以纯CaF2粉体、Nd1‑5at%：CaF2粉体或Yb1‑5at%：CaF2粉体为制品的成型原料，在设定温度、压力下保温保压0.5‑2小时于加压成型模具中成型，升温速率10℃/min，温度范围300‑400℃，压力范围300‑600Mpa，粉体成型原料的粒度20‑200nm，水份控制在1‑15wt%。本发明直接采用高压方式，成型、烧结一次顺序完成，获得更为致密、晶粒细小均匀且透光率高的CaF2基透明陶瓷。本发明具有烧结温度低、工艺简单、节约能源的优势，同时减小产品变形量，有利于保障产品品质。
Description
技术领域
本发明属于电子陶瓷材料技术领域，具体涉及一种氟化钙透明陶瓷及低温制备方法。
背景技术
固体激光器广泛的用于约束聚变、医学科学和制造业等领域，增益介质是激光系统的重要组成部分，玻璃、透明陶瓷和单晶材料是常用的增益介质材料。透明陶瓷不仅具有高透光率、高强度、耐热、耐腐蚀等优良性能，而且具有制备成本低、掺杂均匀性好、比单晶材料尺寸大等优点， 广泛应用于激光、红外、新型光源、原子能工业等领域。
影响透明陶瓷光线透过率的主要因素有：陶瓷本身的气孔、第二相和杂质等。因此在透明陶瓷的制备过程中，应选择合适的烧结工艺使得陶瓷样品的气孔率降低，晶粒均匀大小合适，晶界较薄且无杂质。目前透明陶瓷的主要烧结方式有放电等离子体烧结(SPS)、热等静压烧结(HIP)、真空烧结、热压烧结(HP)等。这些传统的烧结工艺在制备透明陶瓷的过程中一般都需要特殊的气氛要求和较高的温度(>1200℃)，因此在生产过程中成本高并且能耗大，而随着陶瓷低温绿色制备的发展趋势,降低陶瓷的烧结温度已是工业应用迫切需要解决的问题。
目前，一种新的陶瓷烧结工艺已经发展出来,称为冷烧结工艺(Cold SinteringProcess,简称CSP),陶瓷冷烧结工艺是向陶瓷粉末中添加瞬态助溶剂,一般在≤400℃的温度下和一定的压力下使粉末完成陶瓷化的过程。
发明内容
本发明的目的在于提供一种CaF2基透明陶瓷及其低温制备方法，实现在不高于400℃且不添加助溶剂的条件下制备出晶粒细小均匀且透光率高的CaF2基透明陶瓷。
本发明所述的CaF2基透明陶瓷优选采用Ca(NO3)2·4H2O和KF·2H2O为原料，同时掺杂稀土元素，稀土元素由稀土硝酸盐为原料所提供，包括硝酸钕、硝酸镱、硝酸饵和硝酸铽，用以制备Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体。以纯CaF2粉体、Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体为制品的成型原料，在设定温度、压力下保温保压0.5-2小时于加压成型模具中成型，加压成型模具的加热方式不受限制，升温速率10℃/min，温度范围300-400℃，压力范围300-600Mpa，粉体成型原料的粒度20-200nm，水份控制在1-15wt%。为保证粉体成型原料的粒度，优选采用共沉淀法制备Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体。
本发明的技术特点和有益效果：
本发明相对于传统烧结工艺，放弃了使用临时粘结剂和烧结助溶剂，直接采用高压方式，成型、烧结一次顺序完成，获得更为致密、晶粒细小均匀且透光率高的CaF2基透明陶瓷。本发明具有烧结温度低、工艺简单、节约能源的优势，同时减小产品变形量，有利于保障产品品质。
附图说明
图1为本发明所述制备方法的流程示意图；
图2为本发明实施例2样品的SEM图；
图3为本发明实施例样品的透过率图谱。
具体实施方式
下面给出几个具体的实施例，用以详细说明本发明的技术方案和技术效果。
实施例1：
（1）称取10g纯CaF2粉体（粒度20-100nm）制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为225℃，喷雾造粒的送料速度为10ml/min，获取的CaF2基粉体颗粒含水量为10wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的CaF2基粉体颗粒放入模具中，使用单轴压力机施加450MPa的压力，并按10℃/min的升温速率将模具加热至380℃，保温1h，冷却、退模得到CaF2透明陶瓷样品1。
（3）测试CaF2透明陶瓷样品1的相对密度为98.58%，在1100nm的在线透射率为76.56%。
实施例2：
（1）称取10g纯CaF2粉体（粒度20-100nm）制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为225℃，喷雾造粒的送料速度为10ml/min，获取的CaF2基粉体颗粒含水量为10wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的所述CaF2基粉体颗粒放入模具中，使用单轴压力机施加450MPa的压力，并按10℃/min的升温速率将模具加热至400℃，保温1h，冷却、退模得到CaF2透明陶瓷样品2。
（3）测试CaF2透明陶瓷样品2的相对密度为99.02%，在1100nm的在线透射率为79.02%。
实施例3：
（1）以商业的化学试剂Ca(NO3)2·4H2O和KF·2H2O为原料，硝酸钕为掺杂原料，采用共沉淀法制备Nd5at%：CaF2粉体。称取10g Nd 5at%:CaF2粉体制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为225℃，喷雾造粒的送料速度为10ml/min，获取的CaF2基粉体颗粒含水量为10wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的所述CaF2基粉体颗粒放入模具中，使用单轴压力机施加600MPa的压力，并按10℃/min的升温速率将模具加热至400℃，保温1h，冷却、退模得到CaF2基透明陶瓷样品3。
（3）测试CaF2基透明陶瓷样品的相对密度为98.07%，在1100nm的在线透射率为70.86%。
实施例4：
（1）以商业的化学试剂Ca(NO3)2·4H2O和KF·2H2O为原料，硝酸钕为掺杂原料，采用共沉淀法制备Nd1at%：CaF2粉体。称取10g Nd 1at%:CaF2粉体制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为200℃，喷雾造粒的送料速度为1ml/min，获取的Nd 1at%:CaF2粉体颗粒含水量为15wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的所述CaF2基粉体颗粒放入模具中，使用单轴压力机施加300MPa的压力，并按10℃/min的升温速率将模具加热至400℃，保温2h，冷却、退模得到Nd 1at%:CaF2透明陶瓷样品4。
（3）测试Nd1at%:CaF2透明陶瓷样品4的相对密度为95.89%，在1100nm的在线透射率为82.68%。
实施例5：
（1）以商业的化学试剂Ca(NO3)2·4H2O和KF·2H2O为原料，硝酸镱为掺杂原料，采用共沉淀法制备Yb5at%：CaF2粉体。称取10g Yb 5at%:CaF2粉体制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为230℃，喷雾造粒的送料速度为20ml/min，获取的Yb 5at%:CaF2粉体颗粒含水量为1wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的所述CaF2基粉体颗粒放入模具中，使用单轴压力机施加450MPa的压力，并按10℃/min的升温速率将模具加热至300℃，保温0.5h，冷却、退模得到Yb 5at%:CaF2透明陶瓷样品5。
（3）测试Yb5at%:CaF2透明陶瓷样品的相对密度为95.00%，在1100nm的在线透射率为86.53%。
实施例6：
（1）以商业的化学试剂Ca(NO3)2·4H2O和KF·2H2O为原料，硝酸镱为掺杂原料，采用共沉淀法制备Yb1at%：CaF2粉体。称取10g Yb1at%:CaF2粉体制备CaF2基粉体浆料进行喷雾造粒，喷雾造粒的进风温度为225℃，喷雾造粒的送料速度为10ml/min，获取的Yb1at%:CaF2粉体颗粒含水量为10wt%。
（2）选用带加热功能的钢制模具，模具内孔直径为12mm，模具使用前先用脱脂棉花蘸上无水乙醇分别将模具内壁、顶杆、垫块擦拭干净，待模具干燥后，再称取适量的所述CaF2基粉体颗粒放入模具中，使用单轴压力机施加450MPa的压力，并按10℃/min的升温速率将模具加热至350℃，保温1h，冷却、退模得到Yb1at%:CaF2透明陶瓷样品6。
（3）测试Yb1at%:CaF2透明陶瓷样品的相对密度为95.00%，在1100nm的在线透射率为74.29%。
综合上述实施例样品测试数据，本发明获得的透明陶瓷的相对密度达95.00%以上，透射率达74.29%以上。
Claims (3)
1.一种CaF2基透明陶瓷，其特征在于，所述CaF2基透明陶瓷的制备条件：(1)原料为CaF2基粉体，粒度20-200nm，含水量1-15wt%；所述CaF2基粉体为纯CaF2粉体、Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体；（2）在300-600Mpa压力下烧结，烧结温度300-400℃，保温保压时间0.5-2小时。
2.根据权利要求1所述的CaF2基透明陶瓷，其特征在于，其制备方法包括以下步骤：以纯CaF2粉体、Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体为制品成型原料，置于加压成型模具中，在设定温度、压力下保温保压。
3.根据权利要求2所述的CaF2基透明陶瓷制备方法，其特征在于，所述Nd1-5at%：CaF2粉体或Yb1-5at%：CaF2粉体是以Ca(NO3)2·4H2O和KF·2H2O为原料，掺杂元素以稀土硝酸盐为原料，采用共沉淀法制得的CaF2基粉体。
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