CN107216148A - 一种深蓝色纳米陶瓷功能粉体的制备方法和用途 - Google Patents
一种深蓝色纳米陶瓷功能粉体的制备方法和用途 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 45
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 21
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011858 nanopowder Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 7
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- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- 229910052718 tin Inorganic materials 0.000 claims abstract description 5
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 4
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 4
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 4
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 4
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
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- 229910052732 germanium Inorganic materials 0.000 claims abstract description 4
- 229910052738 indium Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910052745 lead Inorganic materials 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 229910052701 rubidium Inorganic materials 0.000 claims abstract description 4
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims description 12
- 239000011733 molybdenum Substances 0.000 claims description 12
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- 239000007788 liquid Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
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- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 3
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 3
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
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- 239000010937 tungsten Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
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- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
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- 239000011701 zinc Substances 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical class [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical class [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及纳米材料，尤其涉及一种纳米功能粉体及其制备方法和用途。一种深蓝色纳米陶瓷功能粉体，所述的功能性纳米粉体指氧空位的纳米氧化钼或元素掺杂的氧化钼纳米粉体，其中掺杂元素为Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Al、Ga、In、Tl、Ge、Sn、Pb、As、Sb、Bi、Se、Te、Ti、Mn、Fe、Co、Ni、Cu、或Zn中的一种或几种混合元素。所述的深蓝色纳米陶瓷粉体的制备方法，包括如下步骤：a) 用液相法制备具有氧化钼的前驱体；b) 对前驱体进行结晶化热处理得到结晶性好的粉体。本发明的纳米功能粉体能大规模地工业化生产，功耗低。
Description
技术领域
本发明涉及纳米材料，尤其涉及一种纳米功能粉体及其制备方法和用途。
背景技术
建筑外墙的隔热层已经广泛在业内采用，对环境友好的隔热膜的研究是优化我国建筑节能领域的热点研究，在科学界和工业界已经吸引大批研究院所和高科技企业的研发投入，而高隔热粉体的制备始终是该领域的重点和难点。
经过不断的研究探索，目前研究出来的隔热粉体如氧化铟锡、氧化锡锑、氧化铝锌等半导体氧化物对于800-1200纳米波段的近红外波段的阻隔效率并不是很明显；而六硼化镧、六硼化钇等硼化物对800-1200纳米波段的近红外已有很好的阻隔效率，但是这些硼化物对可见光的阻隔率也较高，因此如何有效阻隔近红外波段同时保持较高的可见光透过率已成为高阻隔粉体的研究难点。
钨青铜粉体是一种非常有前景的制备高隔热的纳米粉体，对800-1200纳米波段的近红外波段具有非常优异的阻隔效率，同时对可见光则阻隔率较低，而以往制备这种粉体通常是用水热法或是溶剂热法，但是这些方法耗能多、产量小，导致最终无法大规模的生产，进一步限制这一材料的大规模使用。
发明内容
本发明旨在克服现有技术的缺陷，提供一种深蓝色纳米陶瓷功能粉体的制备方法和用途。本发明能大规模地生产，耗能低，满足市场的需求。
本发明一种深蓝色纳米陶瓷功能粉体，所述的功能性纳米粉体指氧空位的纳米氧化钼或元素掺杂的氧化钼纳米粉体，其中掺杂元素为Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Al、Ga、In、Tl、Ge、Sn、Pb、As、Sb、Bi、Se、Te、Ti、Mn、Fe、Co、Ni、Cu、或Zn中的一种或几种混合元素。
所述的深蓝色纳米陶瓷功能粉体，所述掺杂元素占总重量的0-50%。
所述的深蓝色纳米陶瓷功能粉体，它具有半导体性质，其光学曲线表现为具有红外阻隔能力的纳米粉体。
所述的深蓝色纳米陶瓷粉体的制备方法，包括如下步骤：
a) 用液相法制备具有氧化钼的前驱体；
b) 对前驱体进行结晶化热处理得到结晶性好的粉体。
所述步骤a)中原料包括选自氧化钼、钼酸、钼酸钠、钼酸铵、或氯化钼含有钼元素的钼源，包括如下步骤：钼离子溶液或钼化合物粒子悬浊液中加入酸或碱，让钼源完全溶解，之后混入掺杂元素，让液体蒸发得到所需掺杂的氧化钼的前驱体；
所述步骤b)中的热处理是在非氧化性气氛中，是还原性气氛或惰性气氛，如氢气、 氢氮混合气、氢氩混合气、 氨气、氨气和氮气混合气、氨气和氩气的混合气、硫化氢、高真空气氛、高纯氮气、或高纯氩气。
步骤b)中的热处理温度为400～1200℃，热处理时间为5～1200分钟。
所述热处理温度为600到900℃，热处理时间为300-600分钟。
所述的具有深蓝色纳米陶瓷功能粉体在用于制备的隔热涂料、无机纳米色料或是有机塑料薄膜的改性剂的应用。
所述的隔热涂料或有机塑料薄膜在节能贴膜、节能玻璃和节能电子元器件中的应用。
本发明掺杂元素能够控制所得氧化钼类物质的太阳光阻隔性能。掺杂剂中的掺杂元素与钼元素的摩尔比可以根据掺杂元素的掺杂量来确定，本发明所述的具有深蓝色纳米功能粉体可用于制备节能涂料、节能贴膜、节能玻璃或其它节能电子元器件。本发明能大规模地运用于工业化生产，耗能低，满足市场需求。
具体实施方式
一种深蓝色纳米陶瓷功能粉体，所述的功能性纳米粉体指氧空位的纳米氧化钼或元素掺杂的氧化钼纳米粉体，其中掺杂元素为Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Al、Ga、In、Tl、Ge、Sn、Pb、As、Sb、Bi、Se、Te、Ti、Mn、Fe、Co、Ni、Cu、或Zn中的一种或几种混合元素。
所述的深蓝色纳米陶瓷功能粉体，所述掺杂元素占总重量的0-50%。
所述的深蓝色纳米陶瓷功能粉体，它具有半导体性质，其光学曲线表现为具有红外阻隔能力的纳米粉体。
所述的深蓝色纳米陶瓷粉体的制备方法，包括如下步骤：
a) 用液相法制备具有氧化钼的前驱体；
b) 对前驱体进行结晶化热处理得到结晶性好的粉体。
所述步骤a)中原料包括选自氧化钼、钼酸、钼酸钠、钼酸铵、或氯化钼含有钼元素的钼源，包括如下步骤：钼离子溶液或钼化合物粒子悬浊液中加入酸或碱，让钼源完全溶解，之后混入掺杂元素，让液体蒸发得到所需掺杂的氧化钼的前驱体；
所述步骤b)中的热处理是在非氧化性气氛中，是还原性气氛或惰性气氛，如氢气、 氢氮混合气、氢氩混合气、 氨气、氨气和氮气混合气、氨气和氩气的混合气、硫化氢、高真空气氛、高纯氮气、或高纯氩气。
步骤b)中的热处理温度为400～1200℃，热处理时间为5～1200分钟。
所述热处理温度为600到900℃，热处理时间为300-600分钟。
所述的具有深蓝色纳米陶瓷功能粉体在用于制备的隔热涂料、无机纳米色料或是有机塑料薄膜的改性剂的应用。
所述的隔热涂料或有机塑料薄膜在节能贴膜、节能玻璃和节能电子元器件中的应用。
实施例1
称取10.0 kg氯化钼、40.0 kg去离子水，1.0 kg 五水四氯化锡，搅拌直至澄清透明溶液，用碳酸氢铵饱和溶液调节pH约为7.0左右，最后之后过滤、用蒸馏水清洗3-5次，100℃干燥约24小时，得到前驱体固体。
将所得到的固体前驱体放入管式炉中，通入高纯氩气，在600℃热处理120分钟，冷却，得到锡掺杂的钨青铜粉体。
采用XRD、TEM和分光光度计对所获粉体性能进行了表征，参见实施例1。
实施例2
称取10 kg钼酸铵、40 kg去离子水，1.0 kg 硝酸锶，搅拌直至澄清透明溶液，用1 mol/L盐酸调节溶液的酸碱度至约pH约1.0左右，充分搅拌指导钨源充分析出，在用1mol/L的氢氧化钾溶液调节pH约为7.0左右，最后之后过滤、用蒸馏水清洗3-5次，100℃干燥约24小时，得到前驱体固体。
将所得到的固体前驱体放入管式炉中，通入高纯氩气，在800℃热处理120分钟，冷却，得到锶掺杂的氧化钼纳米粉体。
采用扫描电子显微镜对所获粉体性能进行了颗粒尺寸表征，得到的颗粒尺寸与实施例1大小相近。
实施例3
称取10.0 kg氯化钼、40.0 kg去离子水，1.0 kg 氢氧化钠，搅拌直至澄清透明溶液，之后在120℃左右缓慢搅拌直到液体完全蒸干，将干燥的白色粉体研发，过筛。
将所得到的固体前驱体放入管式炉中，通入高纯还原性气体（氢氩混合气），在600℃热处理120分钟，冷却，得到钠掺杂的氧化钼纳米粉体。
采用扫描电子显微镜对所获粉体性能进行了颗粒尺寸表征，得到的颗粒尺寸与实施例1大小相近。
实施例4
称取10 kg氯化钼、40 kg去离子水，1.0 kg 氢氧化钾，搅拌直至澄清透明溶液，之后在100℃左右缓慢搅拌直到液体完全蒸干，将干燥的白色粉体研发，过筛。
将所得到的固体前驱体放入管式炉中，通入高纯还原性气体（氢氩混合气），在800℃热处理120分钟，冷却，得到钾掺杂的氧化钼纳米粉体。
采用扫描电子显微镜对所获粉体性能进行了颗粒尺寸表征，得到的颗粒尺寸与实施例1大小相近。
实施例5
称取10 kg氯化钼、40 kg去离子水，1.0 kg 氢氧化钡，搅拌直至澄清透明溶液，之后在100℃左右缓慢搅拌直到液体完全蒸干，将干燥的白色粉体研发，过筛。
将所得到的固体前驱体放入管式炉中，通入高纯还原性气体（氢氩混合气），在800℃热处理120分钟，冷却，得到钡掺杂的钼纳米粉体。
采用扫描电子显微镜对所获粉体性能进行了颗粒尺寸表征，得到的颗粒尺寸与实施例1大小相近。
实施例6
称取10 kg氯化钼、40 kg去离子水，1.0 kg 硝酸铈，搅拌直至澄清透明溶液，之后在100℃左右缓慢搅拌直到液体完全蒸干，将干燥的白色粉体研发，过筛。
将所得到的固体前驱体放入管式炉中，通入高纯还原性气体（氢氩混合气），在800℃热处理120分钟，冷却，得到铈掺杂的氧化钼纳米粉体。
采用扫描电子显微镜对所获粉体性能进行了颗粒尺寸表征，得到的颗粒尺寸与实施例1大小相近。
Claims (10)
1.一种深蓝色纳米陶瓷功能粉体，其特征在于，所述的功能性纳米粉体指氧空位的纳米氧化钼或元素掺杂的氧化钼纳米粉体，其中掺杂元素为Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Al、Ga、In、Tl、Ge、Sn、Pb、As、Sb、Bi、Se、Te、Ti、Mn、Fe、Co、Ni、Cu、或Zn中的一种或几种混合元素。
2.如权利要求1所述的深蓝色纳米陶瓷功能粉体，其特征在于，所述掺杂元素占总重量的0-50%。
3.如权利要求1所述的深蓝色纳米陶瓷功能粉体，其特征在于，它具有半导体性质，其光学曲线表现为具有红外阻隔能力的纳米粉体。
4.如权利要求1、2或3所述的深蓝色纳米陶瓷粉体的制备方法，其特征在于，包括如下步骤：
a) 用液相法制备具有氧化钼的前驱体；
b) 对前驱体进行结晶化热处理得到结晶性好的粉体。
5.如权利要求4所述的方法，其特征在于，所述步骤a)中原料包括选自氧化钼、钼酸、钼酸钠、钼酸铵、或氯化钼含有钼元素的钼源，包括如下步骤：钼离子溶液或钼化合物粒子悬浊液中加入酸或碱，让钼源完全溶解，之后混入掺杂元素，让液体蒸发得到所需掺杂的氧化钼的前驱体。
6.如权利要求4所述深蓝色纳米陶瓷粉体的制备方法，其特征在于，所述步骤b)中的热处理是在非氧化性气氛中，是还原性气氛或惰性气氛，如氢气、 氢氮混合气、氢氩混合气、氨气、氨气和氮气混合气、氨气和氩气的混合气、硫化氢、高真空气氛、高纯氮气、或高纯氩气。
7.如权利要求6所述的深蓝色纳米陶瓷粉体的制备方法，其特征在于：步骤b)中的热处理温度为400～1200℃，热处理时间为5～1200分钟。
8.如权利要求7所述的深蓝色纳米陶瓷粉体的制备方法，其特征在于，所述热处理温度为600到900℃，热处理时间为300-600分钟。
9.如权利要求1～3任一项所述的具有深蓝色纳米陶瓷功能粉体在用于制备的隔热涂料、无机纳米色料或是有机塑料薄膜的改性剂的应用。
10.如权利要求9所述的隔热涂料或有机塑料薄膜在节能贴膜、节能玻璃和节能电子元器件中的应用。
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