CN106987248B - 一种基于氧化锡锑的上转换材料 - Google Patents
一种基于氧化锡锑的上转换材料 Download PDFInfo
- Publication number
- CN106987248B CN106987248B CN201710227242.8A CN201710227242A CN106987248B CN 106987248 B CN106987248 B CN 106987248B CN 201710227242 A CN201710227242 A CN 201710227242A CN 106987248 B CN106987248 B CN 106987248B
- Authority
- CN
- China
- Prior art keywords
- conversion
- fabric
- tin
- rare earth
- ytterbium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 72
- 239000004744 fabric Substances 0.000 claims abstract description 34
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000009413 insulation Methods 0.000 claims abstract description 13
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 7
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 5
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims abstract description 5
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 150000002910 rare earth metals Chemical class 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 229920005749 polyurethane resin Polymers 0.000 claims description 9
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 claims description 9
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 8
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- 229910001887 tin oxide Inorganic materials 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 2
- 229920000742 Cotton Polymers 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- -1 rare earth ion Chemical class 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002319 LaF3 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 150000003220 pyrenes Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 210000000145 septum pellucidum Anatomy 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7782—Antimonates; Arsenates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
- D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/47—Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Laminated Bodies (AREA)
Abstract
本发明公开了一种基于氧化锡锑的上转换材料，属于材料技术领域。本发明的上转换材料中的氧化锡锑可以对红外光进行大量屏蔽，而掺杂的一定量的稀土元素铒和镱能够吸收环境中较长波长的红外线能量，透过的红外光进一步经稀土元素4f轨道激发和退激发过程放出近红外能量，进一步有效地达到了隔热的作用。本发明的上转换材料创造性地应用于面料加工，可以制备得到隔热性能良好、可光光透过率良好的面料，面料可以用于制备夏日服装。同时，本发明的上转换材料应用于面料加工或者透明隔热薄膜制备时，使用方法非常简便，而且不需要额外的加工设备，容易进行工业化应用。
Description
技术领域
本发明涉及一种基于氧化锡锑的上转换材料，属于材料技术领域。
背景技术
上转换材料，其应用涉及短波长激光、红外探测与显示、生物标记、光学通讯、防伪等领域。上转换材料是一种红外光激发下能发出可见光的发光材料，即将红外光转换成可见光的材料。其特点是所吸收的光子能量低于发射的光子能量。这种现象违背斯托克定律。因此又被称为反斯托克定律发光材料。
由于稀土离子具有丰富的电子能级、高原子磁矩、未成对的4f电子数较多以及电子的跃迁特性，所以稀土离子具有优异的光、电、磁、催化、储氢及超导等性能，可制备出很多性能优越的稀土功能材料，在生物、信息、新材料、新能源等现代科学技术中起着十分核心的作用。如研究者们利用稀土元素的物理性质和化学性质，制备出了稀土磁性材料、稀土发光材料、稀土储能材料、稀土催化材料、稀土生物材料、稀土农用材料等。稀土离子作为掺杂离子在制备上转换发光材料中扮演着极为重要的角色，当前掺杂研究主要集中在铒Er3+、铥Tm3+和钬Ho3+。在LaF3中掺人物质的量的分数分别为12％和3％的Yb3+和Er3+时发出黄光，而掺人物质的量的分数分别为20％和1％的Yb3+和H03十时发出绿光，而且发光强度随着反应时间和反应温度的变化而有所变化。将不同浓度的Yb3+、Er3+和Tm3+共掺到NaYF4纳米颗粒中，可得到从可见光到近红外光的多色荧光材料。
目前，由于技术及成本原因，上转换材料还未广泛应用于服用面料。
发明内容
为了解决上述问题，本发明提供了一种基于氧化锡锑的上转换材料及其制备方法。本发明的采用水热法制备含有稀土上转换材料的氧化锡锑纳米材料，并将其应用于隔热服用面料的开发。通过控制合适比例的上转换材料与氧化锡锑的协同作用，以隔绝环境近红外及红外区辐射，达到隔热的功能。
本发明的上转换材料，主要是通过掺杂稀土元素铒和镱实现上转换功能；所述上转换材料的制备方法是：
(1)以一定摩尔比的氧化锡、氧化锑、硝酸铒、硝酸镱为主要原料，加入蒸馏水与冰醋酸作为混合溶剂，在反应釜中反应一段时间；
(2)然后密封反应釜，于在160-200℃烘箱中反应4小时，取出，自然冷却；
(3)将反应产物过滤、干燥，而后将产物在600-800℃煅烧2-4小时；
(4)将产物机械粉碎，得到稀土元素掺杂的氧化锡锑上转换材料。
在一种实施方式中，所述氧化锡、氧化锑、硝酸铒、硝酸镱的摩尔比为45:4.7:0.2:0.2。
在一种实施方式中，所述蒸馏水与冰醋酸的体积比为1:1。
在一种实施方式中，所述反应釜中的反应条件是：180℃反应6小时。
在一种实施方式中，所述煅烧是在800℃煅烧2h。
本发明的第二个目的是提供一种面料的整理方法，所述方法是先上转换材料充分研磨，然后加入水、在pH 7～8下直接超声分散到水性聚氨酯树脂中得到涂料，然后将面料浸渍到涂料中，面料经轧车轧2-5次，于80℃固化一段时间，得到隔热功能的面料。
在一种实施方式中，超声分散，是分两阶段进行；先超声波频率为8000-10000Hz下处理20-30min，然后于超声波频率为500-800Hz下处理20-30min。
在一种实施方式中，所述上转换材料、水、水性聚氨酯树脂的质量比为1:20:80。
在一种实施方式中，所述轧车轧压率为90％-98％。
在一种实施方式中，所述面料为棉织物。
在一种实施方式中，固化的时间为3h。
在一种实施方式中，所述充分研磨是研磨至50-500nm。
本发明的第三个目的是提供一种透明隔热薄膜，所述透明隔热薄膜是利用本发明的上转换材料制备得到的；所述制备具体是：将先上转换材料充分研磨，然后加入水、在pH7～8下直接超声分散到水性聚氨酯树脂中得到涂料；将涂料镀膜在洁净的玻璃基底上，然后于80℃固化一段时间，得到隔热薄膜。
在一种实施方式中，所述上转换材料、水、水性聚氨酯树脂的质量比为1:20:80。
在一种实施方式中，所述超声分散，是分两阶段进行；先超声波频率为8000-10000Hz下处理20-30min，然后于超声波频率为500-800Hz下处理20-30min。。
在一种实施方式中，薄膜厚度为10μm。
本发明的优点和效果：
(1)本发明的上转换材料，是一种能够将远红外能量转换为近红外能量的上转换材料，上转换材料中的氧化锡锑可以对红外光进行大量屏蔽，而掺杂的一定量的稀土元素铒和镱能够吸收环境中较长波长的红外线能量，透过的红外光进一步经稀土元素4f轨道激发和退激发过程放出近红外能量，进一步有效地达到了隔热的作用。
(2)本发明的上转换材料创造性地应用于面料加工，可以制备得到隔热性能良好的面料，而且可光光透过率良好，面料可以用于制备夏日服装。制备的隔热织物，柔软性好，不会影响衣物的穿着舒适感。
(3)本发明的上转换材料应用于面料加工时，使用方法非常简便，而且不需要额外的加工设备，容易进行工业化应用；
(4)本发明的上转换材料用于透明隔热薄膜，通过对分散方法进行改进使得制备工艺较现有的更加简便，制备得到的薄膜性能良好。
附图说明
图1为稀土掺杂氧化锡锑上转换材料的透射电镜图。
具体实施方案
下面是对本发明进行具体描述。
实施例1：上转换材料的制备
上转换材料的制备方法是：
(1)以摩尔比45:4.7:0.2:0.2的氧化锡、氧化锑、硝酸铒、硝酸镱为主要原料，加入蒸馏水与冰醋酸(蒸馏水与冰醋酸的体积比为1:1)作为混合溶剂，在反应釜中反应一段时间；
(2)然后关闭反应釜，于在180℃烘箱中反应4小时，取出，自然冷却；
(3)将反应产物中的溶剂蒸发，而后将产物在800℃煅烧2小时；
(4)将产物机械粉碎，得到稀土元素掺杂的氧化锡锑上转换材料。
实施例2：上转换材料的制备
上转换材料的制备方法是：
(1)以摩尔比45:4.7:0.3:0.3的氧化锡、氧化锑、硝酸铒、硝酸镱为主要原料，加入蒸馏水与冰醋酸(蒸馏水与冰醋酸的体积比为1:1)作为混合溶剂，在反应釜中反应一段时间；
(2)然后关闭反应釜，于在180℃烘箱中反应4小时，取出，自然冷却；
(3)将反应产物中的溶剂蒸发，而后将产物在800℃煅烧2小时；
(4)将产物机械粉碎，得到稀土元素掺杂的氧化锡锑上转换材料。
实施例3：上转换材料的制备
上转换材料的制备方法是：
(1)以摩尔比45:8:0.3:0.3的氧化锡、氧化锑、硝酸铒、硝酸镱为主要原料，加入蒸馏水与冰醋酸(蒸馏水与冰醋酸的体积比为1:1)作为混合溶剂，在反应釜中反应一段时间；
(2)然后关闭反应釜，于在180℃烘箱中反应4小时，取出，自然冷却；
(3)将反应产物中的溶剂蒸发，而后将产物在800℃煅烧2小时；
(4)将产物机械粉碎，得到稀土元素掺杂的氧化锡锑上转换材料。
实施例4：上转换材料用于面料整理
将实施例1-3制备得到的稀土元素掺杂的氧化锡锑上转换材料，分别用于面料整理，具体方法如下：
先上转换材料充分研磨，然后加入水、在pH 7～8下直接超声分散到水性聚氨酯树脂中得到涂料，其中上转换材料、水、水性聚氨酯树脂的质量比为1:20:80；超声分散是先超声波频率为8000Hz下处理25min，然后于超声波频率为500Hz下处理25min。然后将白色棉织物(纯棉机织布(40S×40S/133*72))浸渍到涂料中，面料经轧车轧3次，轧压率为97％，于80℃固化3h，得到隔热功能的织物。
其中，实施例1-3的上转换材料制备得到的隔热功能的织物，隔热性能如表1所示。
表1上转换材料对织物隔热性能的改善
其中，(1)对照1是指省略实施例1中的硝酸铒、硝酸镱且其他步骤和参数与实施例1完全一致制备得到的材料；(2)相对值是相对于原棉织物(即未经处理的织物)而言；比如原棉织物的可见光透过率为M，实施例1上转化材料经本实施例处理后得到的隔热功能的织物的可见光透过率为X，那么可见光透过率相对值为(X/M)*100％。
测定可见光透过率、红外光区透过率的仪器是傅里叶红外光谱仪，在500-4000cm-1范围内测定样品的可见光及红外透过率。
由表1可知，按照本实施例方法得到的具有隔热功能的织物，其可见光透过率与原织物差别不大，但是红外光区的透过率却明显减少，说明实施例1-3制备得到的上转化材料，能够有效地吸收并转化环境中较长波长的红外线，从而达到比对照1更好的隔热效果。另外，实施例1的上转化材料制备的隔热织物，柔软性好，不会影响衣物的穿着舒适感。
此外，发明人发现，在面料的整理过程中，轧车轧次数保持在3次左右为宜，仅轧一次无法保证良好的红外光阻隔性能。保持轧压率在97％左右，也是尽量保证了织物上余留的涂料的含量，在适合的涂料含量/厚度下，才能保证良好的红外光阻隔效果。
实施例5：上转换材料用于制备透明隔热薄膜
将实施例1-3制备得到的稀土元素掺杂的氧化锡锑上转换材料，分别用于透明隔热薄膜制备，具体方法如下：
将先上转换材料充分研磨，然后加入水、在pH 7～8下直接超声分散到水性聚氨酯树脂中得到涂料，其中上转换材料、水、水性聚氨酯树脂的质量比为1:20:80；超声分散是先超声波频率为8000Hz下处理25min，然后于超声波频率为500Hz下处理25min。将涂料镀膜在洁净的玻璃基底上，然后于80℃固化一段时间，得到隔热薄膜，薄膜厚度为10μm。结果如表2所示。
表2上转换材料对透明隔热薄膜性能的改善
其中，对照1是指省略实施例1中的硝酸铒、硝酸镱且其他步骤和参数与实施例1完全一致制备得到的材料。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (10)
1.一种上转换材料，其特征在于，所述上转换材料主要是通过掺杂稀土元素铒和镱实现上转换功能；所述上转换材料的制备方法是：
(1)以一定摩尔比的氧化锡、氧化锑、硝酸铒、硝酸镱为主要原料，加入蒸馏水与冰醋酸作为混合溶剂，在反应釜中反应一段时间；其中，所述氧化锡、氧化锑、硝酸铒、硝酸镱的摩尔比为45:4.7:0.2:0.2、45:4.7:0.3:0.3或45:8:0.3:0.3；
(2)然后密封反应釜，于在160-200℃烘箱中反应4小时，取出，自然冷却；
(3)将反应产物过滤、干燥，而后将产物在600-800℃煅烧2-4小时；
(4)将产物机械粉碎，得到稀土元素掺杂的氧化锡锑上转换材料。
2.根据权利要求1所述的上转换材料，其特征在于，所述氧化锡、氧化锑、硝酸铒、硝酸镱的摩尔比为45:4.7:0.2:0.2。
3.根据权利要求1所述的上转换材料，其特征在于，所述蒸馏水与冰醋酸的体积比为1:1。
4.根据权利要求1所述的上转换材料，其特征在于，所述煅烧是在800℃煅烧2h。
5.一种面料的整理方法，其特征在于，所述方法是先将权利要求1～4任一所述的上转换材料充分研磨，然后加入水、在pH7～8下直接超声分散到水性聚氨酯树脂中得到涂料，然后将面料浸渍到涂料中，面料经轧车轧2-5次，于80℃固化一段时间，得到隔热功能的面料。
6.根据权利要求5所述的方法，其特征在于，所述超声分散是分两阶段进行；先超声波频率为8000-10000Hz下处理20-30min，然后于超声波频率为500-800Hz下处理20-30min。
7.根据权利要求5所述的方法，其特征在于，所述轧车轧压率为90％-98％。
8.根据权利要求5所述的方法，其特征在于，所述上转换材料、水、水性聚氨酯树脂的质量比为1:20:80。
9.一种透明隔热薄膜，其特征在于，所述透明隔热薄膜是利用权利要求1～4任一所述的上转换材料制备得到的；所述制备具体是：将先上转换材料充分研磨，然后加入水、在pH7～8下直接超声分散到水性聚氨酯树脂中得到涂料；将涂料镀膜在洁净的玻璃基底上，然后于80℃固化一段时间，得到隔热薄膜。
10.权利要求9所述的透明隔热薄膜的应用。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710227242.8A CN106987248B (zh) | 2017-04-10 | 2017-04-10 | 一种基于氧化锡锑的上转换材料 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710227242.8A CN106987248B (zh) | 2017-04-10 | 2017-04-10 | 一种基于氧化锡锑的上转换材料 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106987248A CN106987248A (zh) | 2017-07-28 |
| CN106987248B true CN106987248B (zh) | 2019-08-06 |
Family
ID=59415909
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710227242.8A Active CN106987248B (zh) | 2017-04-10 | 2017-04-10 | 一种基于氧化锡锑的上转换材料 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106987248B (zh) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830803A (zh) * | 2006-03-27 | 2006-09-13 | 上海应用技术学院 | 掺锑和稀土的氧化锡导电粉的制备方法 |
| CN1847156A (zh) * | 2006-03-27 | 2006-10-18 | 上海应用技术学院 | 掺锑和稀土的氧化锡复合导电粉的制备方法 |
| CN103102083A (zh) * | 2013-02-26 | 2013-05-15 | 杭州电子科技大学 | 一种纳米氧化锡锑透明隔热薄膜的制备方法 |
-
2017
- 2017-04-10 CN CN201710227242.8A patent/CN106987248B/zh active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830803A (zh) * | 2006-03-27 | 2006-09-13 | 上海应用技术学院 | 掺锑和稀土的氧化锡导电粉的制备方法 |
| CN1847156A (zh) * | 2006-03-27 | 2006-10-18 | 上海应用技术学院 | 掺锑和稀土的氧化锡复合导电粉的制备方法 |
| CN103102083A (zh) * | 2013-02-26 | 2013-05-15 | 杭州电子科技大学 | 一种纳米氧化锡锑透明隔热薄膜的制备方法 |
Non-Patent Citations (3)
| Title |
|---|
| Optical characteristics of Er3+-Yb3+ doped SnO2 xerogels;E.A.Morais等;《Journal of Alloys and Compounds》;20021231;第344卷;第217-220页 |
| Red Upconversion Luminescence and Paramagnetism in Er/Yb Doped SnO2;Shweta Sharma等;《Electronic Materials Letters》;20131231;第1-6页 |
| Yb3+ effect on the spectroscopic properties of Er–Yb codoped SnO2 thin films;C. Bouzidi等;《Journal of Luminescence》;20110628;第2630-2635页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106987248A (zh) | 2017-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Singh et al. | EPR, FTIR, optical absorption and photoluminescence studies of Fe2O3 and CeO2 doped ZnO–Bi2O3–B2O3 glasses | |
| Zhang et al. | Achieving an ultra-broadband infrared emission through efficient energy transfer in LiInP2O7: Cr3+, Yb3+ phosphor | |
| Monika et al. | Near-infrared light excited highly pure green upconversion photoluminescence and intrinsic optical bistability sensing in a Ho3+/Yb3+ co-doped ZnGa2O4 phosphor through Li+ doping | |
| Gavrilović et al. | Enhancement of luminescence emission from GdVO4: Er3+/Yb3+ phosphor by Li+ co-doping | |
| Chen et al. | Comparison of visible fluorescence properties between sol–gel derived Er3+–Yb3+ and Er3+–Y3+ co-doped TiO2 films | |
| Velázquez et al. | Transparent SiO 2-GdF 3 sol–gel nano-glass ceramics for optical applications | |
| Nagabhushana et al. | Synthesis, characterization and photoluminescence properties of CaSiO3: Dy3+ nanophosphors | |
| Tang et al. | Effects of Ca2+ doping on upconversion luminescence intensity and crystal field asymmetry of β-NaYF4: Yb3+/Er3+ microcrystals | |
| CN102924083B (zh) | 一种碳化锆陶瓷粉体的制备方法 | |
| Sun et al. | Effect of Zn2+ and Li+ ions doped on microstructure and upconversion luminescence of Y2O3: Er3+-Yb3+ thin films | |
| Zhang et al. | Highly distorted Cr3+-doped fluoroantimonate with high absorption efficiency for multifunctional near-infrared spectroscopy applications | |
| Xu et al. | Novel SrGd 2 Al 2 O 7: Mn 4+, Nd 3+, and Yb 3+ phosphors for c-Si solar cells | |
| Wang et al. | Broadband Near‐Infrared Down‐Shifting by Yb–O Charge‐Transfer Band in Yb3+ Singly Doped Tellurite Glasses | |
| Yang et al. | Crystal structure and up-conversion luminescence properties of K3ScF6: Er3+, Yb3+ cryolite | |
| CN105219388A (zh) | 一种铒掺杂氧化镧钇发光材料及其制备方法 | |
| Pan et al. | Activators lattice migration strategy customized for tunable luminescence of Ce3+ doped β-Ca3 (PO4) 2 | |
| Tong et al. | Upconversion luminescence and temperature sensing performance of Er3+ ions doped self-activated KYb (MoO4) 2 phosphors | |
| Jovanović et al. | Up-conversion luminescence of GdVO4: Nd3+/Er3+ and GdVO4: Nd3+/Ho3+ phosphors under 808 nm excitation | |
| CN106987248B (zh) | 一种基于氧化锡锑的上转换材料 | |
| Dehelean et al. | IR, UV–vis spectroscopic and DSC investigations of europium doped tellurite glasses obtained by sol–gel synthesis | |
| Hirano et al. | Intense up-conversion luminescence of Er3+/Yb3+ co-doped YNbO4 through hydrothermal route | |
| Yu et al. | Fabrication of Er 3+-doped LaOCl nanostructures with upconversion and near-infrared luminescence performances | |
| CN110846033A (zh) | 一种防潮性能优良的稀土掺杂上转换发光材料及其制备方法 | |
| Joshi et al. | Upconversion and anomalous power dependence in Ca12Al14O33: Er3+/Yb3+ single phase nanophosphor | |
| Wang et al. | Preparation of Gd2O2S: Yb3+, Er3+, Tm3+ sub-micro phosphors by sulfurization of the oxides derived from sol-gel method and the upconversion luminescence properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230801 Address after: 215532 Bosideng Industrial Park, Guli Town, Changshu City, Suzhou City, Jiangsu Province Patentee after: BOSIDENG DOWN WEAR Co.,Ltd. Address before: 1800 No. 214122 Jiangsu city of Wuxi Province Li Lake Avenue Patentee before: Jiangnan University |