CN105019014B - 一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的合成方法 - Google Patents
一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的合成方法 Download PDFInfo
- Publication number
- CN105019014B CN105019014B CN201510405482.3A CN201510405482A CN105019014B CN 105019014 B CN105019014 B CN 105019014B CN 201510405482 A CN201510405482 A CN 201510405482A CN 105019014 B CN105019014 B CN 105019014B
- Authority
- CN
- China
- Prior art keywords
- nanocrystalline
- matrix material
- balu
- milliliters
- nonlinear optics
- 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.)
- Expired - Fee Related
Links
- 239000011159 matrix material Substances 0.000 title claims abstract description 13
- 238000010189 synthetic method Methods 0.000 title abstract 2
- 235000002757 Erythrina edulis Nutrition 0.000 claims abstract description 21
- 240000008187 Erythrina edulis Species 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 13
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 239000012467 final product Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000005642 Oleic acid Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 5
- 235000019441 ethanol Nutrition 0.000 claims abstract 3
- 229910002651 NO3 Inorganic materials 0.000 claims abstract 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims abstract 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims abstract 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims 1
- 238000005352 clarification Methods 0.000 claims 1
- 125000005909 ethyl alcohol group Chemical group 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- 239000003643 water by type Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 238000003756 stirring Methods 0.000 abstract description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 abstract description 4
- 239000008367 deionised water Substances 0.000 abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000002159 nanocrystal Substances 0.000 description 16
- 230000003287 optical effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000001308 synthesis method Methods 0.000 description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- APRNQTOXCXOSHO-UHFFFAOYSA-N lutetium(3+);trinitrate Chemical compound [Lu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O APRNQTOXCXOSHO-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- -1 rare earth ions Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 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 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 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 description 1
Landscapes
- Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
Abstract
本发明涉及一种非线性光学纳米晶基体材料的合成方法。一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的化学合成方法，包括如下步骤：将氢氧化钠、油酸、无水乙醇以及去离子水混合搅拌；先后将含有硝酸钡的水溶液以及含有硝酸镥的水溶液加入到溶液中，搅拌后，将所得溶液转移到水热釜中，逐滴加入氟化铵的水溶液，保温；将所得的纳米晶用乙醇和环己烷混合液洗涤，烘干后得到最终产物。该BaLu2F8非线性光学纳米晶基体材料的化学合成方法的优点是采用溶剂热法，合成出的BaLu2F8纳米晶形貌规则，材料为低对称性的单斜晶相。
Description
技术领域
本发明涉及一种非线性光学纳米晶基体材料的合成方法。
背景技术
BaLu2F8是一种高性能非线性光学基体材料，可以应用于激光材料。若能合成出尺寸在纳米量级的BaLu2F8基体材料，通过掺杂合适的稀土离子可以实现高效率的上转换或者下转移发光，从而应用于生物医学领域，比如生物成像、生物检测。发展此类具有特殊形貌的高效率发光纳米材料在很大程度上有助于生物医学的发展。
近年来氟化物纳米晶由于声子能量低，光化学稳定性高，无毒性等特点广泛应用于生物医学领域的研究，其主要的合成方法是湿化学法，比如水热法，共沉淀法，热分解法。然而简单的利用这些方法难以制备纯相BaLu2F8晶体，这主要是由于产物中极易出现BaLuF5混合相。目前，BaLu2F8基体材料的合成方法主要是固相烧结法。比如，Hans U.Güdel等人通过固相烧结法合成了尺寸在毫米量级的Er3+：BaLu2F8以及Nd3+：BaLu2F8激光材料，实现了不同波段的高效上转换发光，他们将此归因于Er3+(Nd3+)在BaLu2F8晶格中有两种不同的占位。然而这种毫米量级的块体材料不能应用于生物医学领域，这主要是由于颗粒尺寸太大，难以与细胞或者一些生物分子结合。
发明内容
本发明的目的是公开一种简单的化学合成方法，用于合成平均尺寸为长142纳米，宽44纳米的规则的薄片状BaLu2F8非线性光学纳米晶基体材料，其晶体结构为单斜相。
为了实现上述发明目的，本发明采用下述的技术方案。
一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的化学合成方法，包括如下步骤：
(1)将0.6g氢氧化钠、20毫升油酸、14毫升无水乙醇以及2毫升去离子水混合搅拌，得到澄清的溶液A；
(2)先后将2毫升含有0.5毫摩尔硝酸钡的水溶液以及4毫升含有1毫摩尔硝酸镥的水溶液加入到A溶液中，充分搅拌后，将所得溶液转移到50毫升水热釜中，随后逐滴加入4毫升含有4毫摩尔氟化铵的水溶液，最后在180℃-220℃的温度下保温48-72小时；
(3)将步骤(2)所得的纳米晶用乙醇和环己烷混合液洗涤，然后于40℃-80℃烘干后得到最终产物。
本发明的一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的化学合成方法，采用溶剂热法，合成出的BaLu2F8纳米晶形貌规则，其平均尺寸为长142纳米，宽44纳米，此种材料为低对称性的单斜晶相，通过掺杂合适的稀土离子，可以实现高效率的上转换或者下转移发光，可望在生物医学和太阳能电池领域得到广泛的应用。
附图说明
图1：实施例1中BaLu2F8纳米晶的X射线衍射图；
图2：实施例1中BaLu2F8纳米晶的透射电镜图，图中的标尺长度为200nm；
图3：实施例1中BaLu2F8纳米晶的高分辨图谱，图中的标尺长度为5nm，A代表d(001)＝0.421nm，B代表d(130)＝0.302nm；
图4：实施例2中Yb/Er:BaLu2F8纳米晶的上转换发光图谱，其中A代表2H11/2-----＞ 4I15/2,B代表4S3/2-----＞ 4I15/2，C代表4F9/2-----＞ 4I15/2。
具体实施方式
下面结合图1、图2、图3和图4对本专利做进一步的说明。
实施例1
图1、图2和图3所示一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料，化学合成方法包括如下步骤：
(1)将0.6g氢氧化钠、20毫升油酸、14毫升无水乙醇以及2毫升去离子水混合搅拌，得到澄清的溶液A；
(2)先后将2毫升含有0.5毫摩尔硝酸钡的水溶液以及4毫升含有1毫摩尔硝酸镥的水溶液加入到A溶液中，充分搅拌后，将所得溶液转移到50毫升水热釜中，随后逐滴加入4毫升含有4毫摩尔氟化铵的水溶液，最后在180℃-220℃的温度下保温48-72小时；
(3)将步骤(2)所得的纳米晶用乙醇和环己烷混合液洗涤，然后于40℃-80℃烘干后得到最终产物。
合成出的最终产物BaLu2F8纳米晶形貌规则，其平均尺寸为长142纳米，宽44纳米。
实施例2
如图4所示的Yb/Er:BaLu2F8纳米晶，合成方法包括如下步骤：
(1)将0.6g氢氧化钠，20毫升油酸，14毫升无水乙醇以及2毫升去离子水混合搅拌，得到澄清的溶液A；
(2)先后将2毫升含有0.5毫摩尔硝酸钡的水溶液以及4毫升含有0.78毫摩尔硝酸镥,0.2毫摩尔硝酸镱以及0.02毫摩尔硝酸铒的水溶液加入到A溶液中，充分搅拌后，将所得溶液转移到50毫升水热釜中，随后逐滴加入4毫升含有4毫摩尔氟化铵的水溶液，最后在180℃的温度下保温72小时；
(3)将步骤(2)所得的纳米晶用乙醇和环己烷混合液洗涤，然后于60℃烘干后得到最终产物。
Claims (1)
1.一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的化学合成方法，其特征在于包括如下步骤：
(1)将0.6g氢氧化钠、20毫升油酸、14毫升无水乙醇以及2毫升去离子水混合搅拌，得到澄清的溶液A；
(2)先后将2毫升含有0.5毫摩尔硝酸钡的水溶液以及4毫升含有1毫摩尔硝酸镥的水溶液加入到A溶液中，充分搅拌后，将所得溶液转移到50毫升水热釜中，随后逐滴加入4毫升含有4毫摩尔氟化铵的水溶液，最后在180℃-220℃的温度下保温48-72小时；
(3)将步骤(2)所得的纳米晶用乙醇和环己烷混合液洗涤，然后于40℃-80℃烘干后得到最终产物。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510405482.3A CN105019014B (zh) | 2015-07-09 | 2015-07-09 | 一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的合成方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510405482.3A CN105019014B (zh) | 2015-07-09 | 2015-07-09 | 一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的合成方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105019014A CN105019014A (zh) | 2015-11-04 |
| CN105019014B true CN105019014B (zh) | 2017-07-25 |
Family
ID=54409300
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510405482.3A Expired - Fee Related CN105019014B (zh) | 2015-07-09 | 2015-07-09 | 一种用于制备规则的薄片状BaLu2F8非线性光学纳米晶基体材料的合成方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105019014B (zh) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111020740A (zh) * | 2020-01-07 | 2020-04-17 | 巢湖市方太渔具有限责任公司 | 一种木质素磺酸钙改性的渔网丝的制备方法 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105428541A (zh) * | 2015-11-04 | 2016-03-23 | 西安建筑科技大学 | 核壳结构上转换材料的制备及其在钙钛矿太阳能电池中的应用 |
-
2015
- 2015-07-09 CN CN201510405482.3A patent/CN105019014B/zh not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105428541A (zh) * | 2015-11-04 | 2016-03-23 | 西安建筑科技大学 | 核壳结构上转换材料的制备及其在钙钛矿太阳能电池中的应用 |
Non-Patent Citations (3)
| Title |
|---|
| Hydrothermal Synthesis and Luminescence of Eu-Doped Ba0.92Y2.15F8.29 Submicrospheres;Yeju Huang;《J. Phys. Chem. C》;20090831;第113卷;第16962–16968页 * |
| Solvothermal processes: a route to the stabilization of new materials;Ge´rard Demazeau;《J.Mater.Chem》;19991231;第9卷;第15-18页 * |
| Syntheses and optical properties of monodisperse BaLnF5(Ln=La-Lu.Y) nanocrystals;Lei Lei et al.;《Journal of Alloys and Compounds》;20120628;第540卷;第27-31页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105019014A (zh) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Controlled synthesis of Ln3+ (Ln= Tb, Eu, Dy) and V5+ ion-doped YPO4 nano-/microstructures with tunable luminescent colors | |
| Li et al. | Different microstructures of β-NaYF4 fabricated by hydrothermal process: effects of pH values and fluoride sources | |
| Mao et al. | Synthesis and luminescence properties of erbium-doped Y2O3 nanotubes | |
| Zeng et al. | Synthesis and photoluminescent properties of rare earth doped ZnO hierarchical microspheres | |
| Li et al. | Shape-controllable synthesis and morphology-dependent luminescence properties of GaOOH: Dy3+ and β-Ga2O3: Dy3+ | |
| Sharma et al. | Green luminescent ZnO: Cu 2+ nanoparticles for their applications in white-light generation from UV LEDs | |
| Zhao et al. | Is BiPO4 a better luminescent host? Case study on doping and annealing effects | |
| Nguyen et al. | Shape-and size-controlled synthesis of monoclinic ErOOH and cubic Er2O3 from micro-to nanostructures and their upconversion luminescence | |
| Teshima et al. | Flux growth of highly crystalline NaYF4: Ln (Ln= Yb, Er, Tm) crystals with upconversion fluorescence | |
| He et al. | Self-assembled β-NaGdF4 microcrystals: hydrothermal synthesis, morphology evolution, and luminescence properties | |
| Zheng et al. | Facile hydrothermal synthesis and luminescent properties of large-scale GdVO4: Eu3+ nanowires | |
| Liang et al. | Hydrothermal synthesis and upconversion luminescent properties of YVO4: Yb3+, Er3+ nanoparticles | |
| Ahmad et al. | Hexagonally ordered KLaF4 host: phase-controlled synthesis and luminescence studies | |
| Wang et al. | Multicolor tunable luminescence based on Tb3+/Eu3+ doping through a facile hydrothermal route | |
| Fisher et al. | Synthesis of LaPO4: Eu nanostructures using the sol− gel template method | |
| Qu et al. | Controlled fabrication and shape-dependent luminescence properties of hexagonal NaCeF4, NaCeF4: Tb3+ nanorods via polyol-mediated solvothermal route | |
| Zhuang et al. | Tunable thickness and photoluminescence of bipyramidal hexagonal β-NaYF4 microdisks | |
| Zeng et al. | Highly uniform Tm3+-doped NaYbF4 microtubes: Controlled synthesis and intense ultraviolet photoluminescence | |
| Zhu et al. | Optical properties of Eu3+-doped Y2O3 nanotubes and nanosheets synthesized by hydrothermal method | |
| Ray et al. | Size and shape-tailored hydrothermal synthesis and characterization of nanocrystalline LaPO4: Eu3+ phosphor | |
| CN102994089A (zh) | 超小核壳结构碱土氟化物纳米晶的制备方法 | |
| He et al. | Reducing grain size and enhancing luminescence of NaYF4: Yb3+, Er3+ upconversion materials | |
| Thirumalai et al. | Controlled synthesis, formation mechanism and lumincence properties of novel 3-dimensional Gd 2 (MoO 4) 3: Eu 3+ nanostructures | |
| Yang et al. | Kinetic control over YVO4: Eu3+ nanoparticles for tailored structure and luminescence properties | |
| Gu et al. | Preparation and photoluminescence of single-crystalline GdVO4: Eu3+ nanorods by hydrothermal conversion of Gd (OH) 3 nanorods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170725 Termination date: 20190709 |