CN110726705B - 一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 - Google Patents
一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 Download PDFInfo
- Publication number
- CN110726705B CN110726705B CN201911023321.2A CN201911023321A CN110726705B CN 110726705 B CN110726705 B CN 110726705B CN 201911023321 A CN201911023321 A CN 201911023321A CN 110726705 B CN110726705 B CN 110726705B
- Authority
- CN
- China
- Prior art keywords
- solution
- dye
- raman
- detection
- noble metal
- 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
- 238000001514 detection method Methods 0.000 title claims abstract description 39
- 239000000758 substrate Substances 0.000 title claims abstract description 33
- 239000004065 semiconductor Substances 0.000 title claims abstract description 26
- 239000007850 fluorescent dye Substances 0.000 title claims abstract description 14
- 239000010409 thin film Substances 0.000 title claims description 18
- 239000000975 dye Substances 0.000 claims abstract description 57
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 31
- 239000000523 sample Substances 0.000 claims abstract description 27
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 23
- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 15
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 13
- 230000001105 regulatory effect Effects 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001228 spectrum Methods 0.000 claims abstract description 8
- 238000004528 spin coating Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 54
- 239000010408 film Substances 0.000 claims description 51
- 239000002070 nanowire Substances 0.000 claims description 38
- 239000002073 nanorod Substances 0.000 claims description 31
- 229910052691 Erbium Inorganic materials 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 15
- 239000002105 nanoparticle Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001338 self-assembly Methods 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- XYYVDQWGDNRQDA-UHFFFAOYSA-K trichlorogold;trihydrate;hydrochloride Chemical compound O.O.O.Cl.Cl[Au](Cl)Cl XYYVDQWGDNRQDA-UHFFFAOYSA-K 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 230000001404 mediated effect Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000000197 pyrolysis Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- FQNHWXHRAUXLFU-UHFFFAOYSA-N carbon monoxide;tungsten Chemical group [W].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] FQNHWXHRAUXLFU-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- LEYFXTUKPKKWMP-UHFFFAOYSA-K trichloroytterbium;hexahydrate Chemical compound O.O.O.O.O.O.Cl[Yb](Cl)Cl LEYFXTUKPKKWMP-UHFFFAOYSA-K 0.000 claims description 4
- IINACGXCEZNYTF-UHFFFAOYSA-K trichloroyttrium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Y+3] IINACGXCEZNYTF-UHFFFAOYSA-K 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 229940068911 chloride hexahydrate Drugs 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- VOAPTKOANCCNFV-UHFFFAOYSA-N hexahydrate;hydrochloride Chemical compound O.O.O.O.O.O.Cl VOAPTKOANCCNFV-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 2
- 238000011002 quantification Methods 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000005672 electromagnetic field Effects 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 229930002875 chlorophyll Natural products 0.000 description 2
- 235000019804 chlorophyll Nutrition 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000013207 serial dilution Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000002866 fluorescence resonance energy transfer Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
-
- 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
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N2021/6417—Spectrofluorimetric devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/653—Coherent methods [CARS]
- G01N2021/655—Stimulated Raman
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Molecular Biology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明属于荧光染料检测领域，公开了一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法。所述方法包括以下步骤：S1.贵金属/半导体调控的发光薄膜基底的制备；S2.均匀旋涂染料探针于基底得到标准样品；S3.测量所得标准样品的拉曼光谱——定性；S4.绘制并分析拉曼强度与染料浓度的标准曲线；S5.测试所得标准样品的荧光光谱；S6.绘制并分析光谱积分面积与染料浓度的标准曲线——定量。本发明采用双重检测的方式，克服了拉曼检测线性饱和的缺陷，利用拉曼检测的“指纹”特性以及荧光传感特性，实现了从定性到定量的精确检测。本发明检测方法新颖独特，成本较低，简便实用，抗干扰能力强。
Description
技术领域
本发明属于荧光染料检测领域，本发明涉及一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法。
背景技术
近些年，检测低浓度、小体积的染料无论是在医学、材料和环保等领域都有着十分重大的意义。表面增强拉曼散射由于其能够提供“指纹”信息的高灵敏度以及操作简单等优点而被常用来检测染料，广泛应用于环境监测，农业、化学生物、食品安全的检测。在拉曼检测中，使用具有强等离激元共振特性的基底，通过激光照射下染料表现出特征拉曼散射光，从而确定染料组分。但是，这种常见的检测方式却一直存在线性饱和的缺陷，即只能在低浓度时一定的小范围内实现强度和浓度的定量分析。此外，由于发光纳米粒子与荧光染料之间可以发生荧光共振能量转移，利用发光薄膜检测染料也逐渐引起科学家的注意，不过是因为通过荧光光谱检测染料浓度，所以这种检测方式不能过对染料进行定性分析。由于检测方法各具特点，且基底薄膜不能互通使用，所以染料检测的方式一直都不理想。
发明内容
为了克服现有技术中存在的缺点，本发明的目的是提出一种工艺简单、重复性好的基于贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法。
本发明的上述目的是通过以下技术方案实现的：
基于贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，包括以下检测步骤：
S1.贵金属/半导体调控的发光薄膜基底的制备：采用水热法生长W18O49纳米线半导体薄膜，将种子介导法得到的Au纳米棒和高温热解法得到的NaYF4:Yb,Er纳米粒子先后组装到半导体薄膜形成贵金属/半导体调控的发光薄膜基底。
S2.均匀旋涂染料探针于基底得到标准样品：将罗丹明6G(R6G)溶解在无水乙醇中用作探针分子，溶液浓度范围从10-3到10-11mol/L，设置旋涂速度为300-400rpm，时间为5-10min,将相同体积不同浓度的染料在基底沉积，干燥5-6h。
S3.测量所得标准样品的拉曼光谱——定性：对不同浓度染料的标准样品进行拉曼测试，拉曼光谱仪使用高分辨率共聚焦拉曼光谱仪，设定相同的参数。激发波长为532.8nm，×50L物镜用于聚焦激光束，积分时间30s，所有采集中的平均斑点直径为1mm。对于每个样品，收集来自不同区域的拉曼光谱，并将信号强度平均以进行最终分析。得到特征拉曼散射光谱，从而确定染料组分。
S4.绘制并分析拉曼强度与染料浓度的标准曲线：绘制标准曲线，分析得出在高浓度出现线性饱和，无法通过拉曼光谱实现染料检测定量。
S5.测试所得标准样品的荧光光谱：采用Jobin Yvon iHR550单色仪采集光谱和980nm激光二极管作为激发光源，设定相同的参数，电压0.5V，狭缝2.24nm。根据染料本身荧光峰位，确定不同浓度染料在基底薄膜上的荧光发光。
S6.绘制并分析光谱积分面积与染料浓度的标准曲线——定量：绘制标准曲线，得出能够在较大浓度范围对染料进行定量分析。
所述S1分如下三步进行制备：
1)采用水热法制备W18O49纳米线薄膜，磁力搅拌溶有25-30mg六羰基钨的无水乙醇溶液，40-60min后移入聚四氟乙烯反应釜中，釜内提前放有2*3cm FTO导电玻璃，随后将反应釜移入180-200℃的烘箱，保温10-12h后，待反应釜温度降至室温后取出，随后用无水乙醇反复冲洗，得到W18O49纳米线薄膜；
2)采用种子介导法制备Au纳米棒，通过简单自组装将Au纳米棒沉积于W18O49纳米线薄膜。首先制备种子溶液，在混合0.5～1mM四氯金酸三水合物与0.2～0.4M十六烷基三甲基溴化铵后加入0.01～0.02M硼氢化钠水溶液，静止30-40min；然后制备生长溶液，将0.037～0.047M十六烷基三甲基溴化铵溶液和4mM油酸钠磁力搅拌，滴加4mM硝酸银后停止搅拌静止15-20min，随后加入四氯金酸三水合物搅拌90-120min，快速加入2～6mL的盐酸后，加入0.064M抗坏血酸溶液，最后将0.08-0.16mL种子溶液注入生长液溶液，剧烈搅拌生长溶液30s，静止12h后，用去离子水洗涤离心即得Au纳米棒。将步骤1)获得的W18O49纳米线薄膜置于分散有Au纳米棒的去离子水混合溶液中，并移入烘箱，将烘箱加热到50-70℃并保温6-8h，待溶液蒸发完全，得到Au纳米棒/W18O49纳米线薄膜；
3)采用高温热解法制备NaYF4:Yb,Er纳米粒子，通过简单自组装将NaYF4:Yb,Er纳米粒子沉积于W18O49纳米线薄膜。称量摩尔比为0.02：0.2：1的六水氯化钇、六水氯化镱、六水氯化饵倒入三口烧瓶，加入6-12mL油酸和15-30mL十八烯，抽真空，将三口烧瓶加热到150℃保温20-30min，降至室温后，将溶有0.148-0.296g氟化铵和0.1-0.2g氢氧化钠的5-10mL甲醇溶液通过注射泵匀速逐滴加入上述三口烧瓶中，通氩气提高温度排除甲醇，最后将温度升至305-310℃保温1.5-2h后，待冷却降至室温，用环己烷与乙醇1:3体积比液体离心洗涤三次，最终得到NaYF4:Yb,Er发光粒子。将步骤2)获得的Au纳米棒/W18O49纳米线薄膜置于分散有NaYF4:Yb,Er发光粒子的环己烷混合溶液中，并移入烘箱，将烘箱加热到50-70℃并保温6-8h，待溶液蒸发完全，得到NaYF4:Yb,Er发光粒子/Au纳米棒/W18O49纳米线基底薄膜。
本发明与现有技术相比的有益效果是：
1.本发明制备的复合基底薄膜，其中半导体W18O49纳米线因其特殊的形貌特征使得薄膜表面并不是平整的完全的被发光粒子覆盖，与贵金属Au纳米棒接触实现了局域电磁场的大幅增强。
2.本发明这种表面不平整的薄膜，一方面可以被用来增强拉曼光谱强度，另一方面可以被用来增强NaYF4:Yb,Er发光粒子的发光强度，提高荧光强度，进而提高检测灵敏度。
3.本发明不是简单的结合两种不同原理的检测方法，是利用得到的特殊形貌基底薄膜实现了将同一基底应用于两种检测方法，并通过这种基底将两种检测方法巧妙结合，且具有制备简易，可重发性高且安全无毒的优异特性。
4.本发明提出了将拉曼检测和荧光检测结合，利用各自的“指纹”特性和传感特性的优点弥补了高浓度线性饱和与无法判断染料组分的各自缺点，实现了先定性再定量的新型染料检测方式。
附图说明
图1为NaYF4:Yb,Er发光粒子/Au纳米棒/W18O49纳米线基底薄膜的截面电镜图。
图2为不同浓度标准样品的拉曼光谱图。
图3为拉曼光谱信号强度与染料浓度的线性关系图。
图4为不同浓度标准样品的荧光光谱图。
图5为荧光光谱积分面积与染料浓度的线性关系图。
具体实施方式
下面通过具体实施例详述本发明，但不限制本发明的保护范围。如无特殊说明，本发明所采用的实验方法均为常规方法，所用实验器材、材料、试剂等均可从商业途径获得。
实施例1
本发明提供一种基于贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，复合薄膜中半导体W18O49纳米线薄膜表现为生长在导电玻璃上具有刺状形貌的基底，利用其表面不平整的特点，沉积贵金属Au纳米棒提高薄膜表面局域电磁场，二次沉积发光纳米粒子增强发光强度。在基底表面旋涂染料后，首先利用裸露的贵金属/半导体的接触，提高低浓度染料的拉曼散射信号，得到染料的拉曼特征峰从而定性分析染料组分。然后在贵金属/半导体调控增强的NaYF4:Yb,Er发光发光薄膜上测试不同浓度染料的荧光光谱，讨论光谱积分面积与浓度的关系，在较大浓度范围得到很好的线性关系从而实现染料的定量分析。
第一步是贵金属/半导体调控的发光薄膜基底的制备，分三步进行制备。
1)采用水热法制备W18O49纳米线薄膜，磁力搅拌溶有25mg六羰基钨的无水乙醇溶液，40min后移入聚四氟乙烯反应釜中，釜内提前放有2*3cm FTO导电玻璃，随后将反应釜移入180℃的烘箱，保温10h后，待反应釜温度降至室温后取出，随后用无水乙醇反复冲洗，得到W18O49纳米线薄膜；
2)采用种子介导法制备Au纳米棒，通过简单自组装将Au纳米棒沉积于W18O49纳米线薄膜。首先制备种子溶液，在混合0.5mM四氯金酸三水合物与0.2M十六烷基三甲基溴化铵后加入0.01M硼氢化钠水溶液，静止30min；然后制备生长溶液，将0.037M十六烷基三甲基溴化铵溶液和4mM油酸钠磁力搅拌，滴加4mM硝酸银后停止搅拌静止15min，随后加入四氯金酸三水合物搅拌90min，快速加入2mL的盐酸后，加入0.064M抗坏血酸溶液，最后将0.08-0.16mL种子溶液注入生长液溶液，剧烈搅拌生长溶液30s，静止12h后，用去离子水洗涤离心即得Au纳米棒。将步骤1)获得的W18O49纳米线薄膜置于分散有Au纳米棒的去离子水混合溶液中，并移入烘箱，将烘箱加热到50℃并保温6h，待溶液蒸发完全，得到Au纳米棒/W18O49纳米线薄膜；
3)采用高温热解法制备NaYF4:Yb,Er纳米粒子，通过简单自组装将NaYF4:Yb,Er纳米粒子沉积于W18O49纳米线薄膜。称量摩尔比为0.02：0.2：1的六水氯化钇、六水氯化镱、六水氯化饵倒入三口烧瓶，加入6mL油酸和15mL十八烯，抽真空，将三口烧瓶加热到150℃保温20min，降至室温后，将溶有0.148g氟化铵和0.1g氢氧化钠的5mL甲醇溶液通过注射泵匀速逐滴加入上述三口烧瓶中，通氩气提高温度排除甲醇，最后将温度升至305℃保温1.5h后，待冷却降至室温，用环己烷与乙醇1:3体积比液体离心洗涤三次，最终得到NaYF4:Yb,Er发光粒子。将步骤2)获得的Au纳米棒/W18O49纳米线薄膜置于分散有NaYF4:Yb,Er发光粒子的环己烷混合溶液中，并移入烘箱，将烘箱加热到50℃并保温6h，待溶液蒸发完全，得到NaYF4:Yb,Er发光粒子/Au纳米棒/W18O49纳米线基底薄膜，如图1所示；
第二步是均匀旋涂染料探针于基底得到标准样品，将R6G溶解在无水乙醇中用作探针分子，溶液浓度范围从10-3到10-11mol/L，。首先制备浓度为10-3mol/L的R6G，通过连续稀释，10倍或102倍得到其他浓度的溶液。将相同体积不同浓度的各等分试样分别旋涂到基底薄膜上，设置旋涂速度为300rpm，时间为5min，随后移入烘箱干燥5h后得到标准样品。
第三步是测量所得标准样品的拉曼光谱——定性，使用高分辨率共聚焦拉曼光谱仪，对步骤二得到的不同浓度染料的标准样品进行拉曼测试，设定相同的参数，设定相同的参数，激发波长为532.8nm，×50L物镜用于聚焦激光束，积分时间30s，所有采集中的平均斑点直径为1mm。对于每个样品，收集来自不同区域的拉曼光谱，并将信号强度平均以进行最终分析。测试得到的拉曼光谱如图2所示，位移峰范围为400-2000cm-1，对比R6G的特征峰，证实了所测标准样品特征峰来自R6G分子，从而确定染料组分为R6G。
第四步是绘制并分析拉曼强度与染料浓度的标准曲线，根据第三步测试得到的不同浓度标准样品的不同强度拉曼信号绘制曲线，如图3，表面增强拉曼信号与浓度的响应关系在10-7到10-11内保持线性关系，但是超过该范围发生线性饱和，所以无法准确根据拉曼信号强度判断相应染料浓度，即无法实现定量检测。
第五步是测试所得标准样品的荧光光谱，光谱的采集时使用Jobin Yvon iHR550单色仪，对步骤二得到的不同浓度染料的标准样品进行荧光光谱测试，980nm激光二极管作为激发光源，测试过程设定相同的参数，电压0.5V，狭缝2.24nm。测试得到的荧光光谱如图4所示，波长范围为500-700nm，对比NaYF4:Yb,Er发光纳米粒子发光光谱和染料本身的荧光峰位，确定不同浓度染料在基底薄膜上的荧光发光。
第六步是绘制并分析光谱积分面积与染料浓度的标准曲线——定量，根据第五步测试得到的不同浓度标准样品的不同荧光光谱绘制曲线，如图5，光谱积分面积与浓度的响应关系在10-3到10-11内保持很好的线性关系，可以通过对应的积分面积确定相应燃料浓度，即实现了定量检测。
实施例2
本发明提供一种基于贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，复合薄膜中半导体W18O49纳米线薄膜表现为生长在导电玻璃上具有刺状形貌的基底，利用其表面不平整的特点，沉积贵金属Au纳米棒提高薄膜表面局域电磁场，二次沉积发光纳米粒子增强发光强度。在基底表面旋涂染料后，首先利用裸露的贵金属/半导体的接触，提高低浓度染料的拉曼散射信号，得到染料的拉曼特征峰从而定性分析染料组分。然后在贵金属/半导体调控增强的NaYF4:Yb,Er发光发光薄膜上测试不同浓度染料的荧光光谱，讨论光谱积分面积与浓度的关系，在较大浓度范围得到很好的线性关系从而实现染料的定量分析。
第一步是贵金属/半导体调控的发光薄膜基底的制备，分三步进行制备。
1)采用水热法制备W18O49纳米线薄膜，磁力搅拌溶有30mg六羰基钨的无水乙醇溶液，60min后移入聚四氟乙烯反应釜中，釜内提前放有2*3cm FTO导电玻璃，随后将反应釜移入200℃的烘箱，保温12h后，待反应釜温度降至室温后取出，随后用无水乙醇反复冲洗，得到W18O49纳米线薄膜；
2)采用种子介导法制备Au纳米棒，通过简单自组装将Au纳米棒沉积于W18O49纳米线薄膜。首先制备种子溶液，在混合1mM四氯金酸三水合物与0.4M十六烷基三甲基溴化铵后加入0.02M硼氢化钠水溶液，静止40min；然后制备生长溶液，将0.047M十六烷基三甲基溴化铵溶液和4mM油酸钠磁力搅拌，滴加4mM硝酸银后停止搅拌静止20min，随后加入四氯金酸三水合物搅拌120min，快速加入6mL的盐酸后，加入0.064M抗坏血酸溶液，最后将0.08-0.16mL种子溶液注入生长液溶液，剧烈搅拌生长溶液30s，静止12h后，用去离子水洗涤离心即得Au纳米棒。将步骤1)获得的W18O49纳米线薄膜置于分散有Au纳米棒的去离子水混合溶液中，并移入烘箱，将烘箱加热到70℃并保温8h，待溶液蒸发完全，得到Au纳米棒/W18O49纳米线薄膜；
3)采用高温热解法制备NaYF4:Yb,Er纳米粒子，通过简单自组装将NaYF4:Yb,Er纳米粒子沉积于W18O49纳米线薄膜。称量摩尔比为0.02：0.2：1的六水氯化钇、六水氯化镱、六水氯化饵倒入三口烧瓶，加入12mL油酸和30mL十八烯，抽真空，将三口烧瓶加热到150℃保温30min，降至室温后，将溶有0.296g氟化铵和0.2g氢氧化钠的10mL甲醇溶液通过注射泵匀速逐滴加入上述三口烧瓶中，通氩气提高温度排除甲醇，最后将温度升至310℃保温2h后，待冷却降至室温，用环己烷与乙醇1:3体积比液体离心洗涤三次，最终得到NaYF4:Yb,Er发光粒子。将步骤2)获得的Au纳米棒/W18O49纳米线薄膜置于分散有NaYF4:Yb,Er发光粒子的环己烷混合溶液中，并移入烘箱，将烘箱加热到70℃并保温8h，待溶液蒸发完全，得到NaYF4:Yb,Er发光粒子/Au纳米棒/W18O49纳米线基底薄膜；
第二步是均匀旋涂染料探针于基底得到标准样品，将R6G溶解在无水乙醇中用作探针分子，溶液浓度范围从10-3到10-11mol/L。首先制备浓度为10-3mol/L的R6G，通过连续稀释，10倍或102倍得到其他浓度的溶液。将相同体积不同浓度的各等分试样分别旋涂到基底薄膜上，设置旋涂速度为400rpm，时间为10min，随后移入烘箱干燥6h后得到标准样品。
第三步是测量所得标准样品的拉曼光谱——定性，使用高分辨率共聚焦拉曼光谱仪，对步骤二得到的不同浓度染料的标准样品进行拉曼测试，设定相同的参数，设定相同的参数，激发波长为532.8nm，×50L物镜用于聚焦激光束，积分时间30s，所有采集中的平均斑点直径为1mm。对于每个样品，收集来自不同区域的拉曼光谱，并将信号强度平均以进行最终分析。测试得到的拉曼光谱图确定染料组分为R6G。
第四步是绘制并分析拉曼强度与染料浓度的标准曲线，根据第三步测试得到的不同浓度标准样品的不同强度拉曼信号绘制曲线。
第五步是测试所得标准样品的荧光光谱，光谱的采集时使用Jobin Yvon iHR550单色仪，对步骤二得到的不同浓度染料的标准样品进行荧光光谱测试，980nm激光二极管作为激发光源，测试过程设定相同的参数，电压0.5V，狭缝2.24nm。测试得到的荧光光谱图，对比NaYF4:Yb,Er发光纳米粒子发光光谱和染料本身的荧光峰位，确定不同浓度染料在基底薄膜上的荧光发光。
第六步是绘制并分析光谱积分面积与染料浓度的标准曲线——定量，根据第五步测试得到的不同浓度标准样品的不同荧光光谱绘制曲线，可以通过对应的积分面积确定相应燃料浓度，即实现了定量检测。
以上所述实施方式仅为本发明的优选实施例，而并非本发明可行实施的全部实施例。对于本领域一般技术人员而言，在不背离本发明原理和精神的前提下对其所作出的任何显而易见的改动，都应当被认为包含在本发明的权利要求保护范围之内。
Claims (4)
1.一种贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，其特征是，包括以下检测步骤：
步骤S1. 贵金属/半导体调控的发光薄膜基底的制备；
步骤S2. 均匀旋涂染料探针于基底得到标准样品；
步骤S3. 测量所得标准样品的拉曼光谱一一定性；
步骤S4. 绘制并分析拉曼强度与染料浓度的标准曲线；
步骤S5. 测试所得标准样品的荧光光谱；
步骤S6. 绘制并分析光谱积分面积与染料浓度的标准曲线一一定量；
所述步骤S1更具体为：分如下三步进行制备：
1) 采用水热法制备W18O49纳米线薄膜，磁力搅拌溶有25-30 mg六羰基钨的无水乙醇溶液，40-60min后移入聚四氟乙烯反应釜中，釜内提前放有2*3 cm FTO导电玻璃，随后将反应釜移入180-200 ℃的烘箱，保温10-12 h后，待反应釜温度降至室温后取出，随后用无水乙醇反复冲洗，得到W18O49纳米线薄膜；
2) 采用种子介导法制备Au纳米棒，通过简单自组装将Au纳米棒沉积于W18O49纳米线薄膜；首先制备种子溶液，在混合0.5~1 mM四氯金酸三水合物与0.2~0.4 M十六烷基三甲基溴化铵后加入0.01~0.02 M硼氢化钠水溶液，静止30-40min；然后制备生长溶液，将0.037~0.047 M十六烷基三甲基溴化铵溶液和4 mM油酸钠磁力搅拌，滴加4 mM硝酸银后停止搅拌静止15-20min，随后加入四氯金酸三水合物搅拌90-120min，快速加入2~6 mL的盐酸后，加入0.064 M抗坏血酸溶液，最后将0.08-0.16 mL种子溶液注入生长液溶液，剧烈搅拌生长溶液30 s，静止12h后，用去离子水洗涤离心即得Au纳米棒；将步骤1)获得的W18O49纳米线薄膜置于分散有Au纳米棒的去离子水混合溶液中，并移入烘箱，将烘箱加热到50-70℃并保温6-8 h，待溶液蒸发完全，得到Au纳米棒/W18O49纳米线薄膜；
3) 采用高温热解法制备NaYF4:Yb,Er纳米粒子，通过简单自组装将NaYF4:Yb,Er纳米粒子沉积于W18O49纳米线薄膜；称量摩尔比为0.02：0.2：1的六水氯化钇、六水氯化镱、六水氯化饵倒入三口烧瓶，加入6-12 mL油酸和15-30 mL十八烯，抽真空，将三口烧瓶加热到150℃保温20-30 min，降至室温后，将溶有0.148-0.296 g氟化铵和0.1-0.2 g氢氧化钠的5-10mL甲醇溶液通过注射泵匀速逐滴加入上述三口烧瓶中，通氩气提高温度排除甲醇，最后将温度升至305-310℃保温1.5-2 h后，待冷却降至室温，用环己烷与乙醇1:3体积比液体离心洗涤三次，最终得到NaYF4:Yb,Er发光粒子；将步骤2)获得的Au纳米棒/W18O49纳米线薄膜置于分散有NaYF4:Yb,Er发光粒子的环己烷混合溶液中，并移入烘箱，将烘箱加热到50-70℃并保温6-8 h，待溶液蒸发完全，得到NaYF4:Yb,Er发光粒子/Au纳米棒/W18O49纳米线基底薄膜。
2.如权利要求1所述的一种贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，其特征是，所述步骤S2具体为：将罗丹明6G溶解在无水乙醇中用作探针分子，溶液浓度范围从10-3到10-11mol/L，设置旋涂速度为300-400rpm，时间为5-10 min, 将相同体积不同浓度的染料在基底沉积，干燥5-6h。
3.如权利要求2所述的一种贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，其特征是，所述步骤S3具体为：对不同浓度染料的标准样品进行拉曼测试，拉曼光谱仪使用高分辨率共聚焦拉曼光谱仪，设定相同的参数；激发波长为532.8 nm，×50 L物镜用于聚焦激光束，积分时间30 s，所有采集中的平均斑点直径为1 mm；对于每个样品，收集来自不同区域的拉曼光谱，并将信号强度平均以进行最终分析；得到特征拉曼散射光谱，从而确定染料组分。
4.如权利要求3所述的一种贵金属/半导体调控的发光薄膜基底的新型荧光染料检测方法，其特征是，所述步骤S5具体为：采用Jobin Yvon iHR550 单色仪采集光谱和980 nm激光二极管作为激发光源，设定相同的参数，电压0.5 V，狭缝2.24 nm；根据染料本身荧光峰位，确定不同浓度染料在基底薄膜上的荧光发光。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911023321.2A CN110726705B (zh) | 2019-10-25 | 2019-10-25 | 一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911023321.2A CN110726705B (zh) | 2019-10-25 | 2019-10-25 | 一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110726705A CN110726705A (zh) | 2020-01-24 |
| CN110726705B true CN110726705B (zh) | 2022-07-22 |
Family
ID=69222073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911023321.2A Active CN110726705B (zh) | 2019-10-25 | 2019-10-25 | 一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110726705B (zh) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112246252B (zh) * | 2020-09-28 | 2023-02-28 | 大连民族大学 | 一种高效表面等离激元光催化剂及制备方法 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101019019A (zh) * | 2004-04-23 | 2007-08-15 | 奥克尼卡公司 | 表面强化的光谱学活性复合纳米颗粒 |
| WO2012164024A1 (en) * | 2011-06-03 | 2012-12-06 | Bayer Technology Services Gmbh | Process for continuously preparing rare earth doped fluorescent nanoparticles, their solution and system therefor |
| CN103865537A (zh) * | 2012-12-17 | 2014-06-18 | 中国科学院大连化学物理研究所 | 一种稀土上转换纳米荧光探针及其制备和应用 |
| CN104479679A (zh) * | 2014-11-12 | 2015-04-01 | 辽宁大学 | 一种NaYF4:Yb3+/Er3+@Ag纳米复合材料及其制备方法及应用 |
| CN109971461A (zh) * | 2019-04-01 | 2019-07-05 | 暨南大学 | 一种上转换荧光选择性增强的复合材料及其制备方法 |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011084641A2 (en) * | 2009-12-16 | 2011-07-14 | The Regents Of The University Of California | Gold coating of rare earth nano-phosphors and uses thereof |
| US9080106B2 (en) * | 2010-07-12 | 2015-07-14 | Ocean's King Lighting Science & Technology Co., Ltd. | Oxide luminescent materials and preparation methods thereof |
| CN102127444B (zh) * | 2010-12-10 | 2013-05-08 | 吉林大学 | 纳米金修饰的增强型上转换发光复合材料及其制备方法 |
| WO2013112856A2 (en) * | 2012-01-26 | 2013-08-01 | The Regents Of The University Of Colorado, A Body Corporate | Multifunctional nanomaterials for the treatment of cancer |
| CN105694889B (zh) * | 2014-11-27 | 2019-05-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | 上转换发光材料、其制备方法及应用 |
| CN105241858B (zh) * | 2015-10-20 | 2019-01-18 | 天津师范大学 | 一种采用上转换纳米粒子对染料罗丹明b进行检测的方法 |
| CN105295912B (zh) * | 2015-10-29 | 2017-07-11 | 大连民族大学 | 一种高效绿色上转换发光复合薄膜及其制备方法 |
-
2019
- 2019-10-25 CN CN201911023321.2A patent/CN110726705B/zh active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101019019A (zh) * | 2004-04-23 | 2007-08-15 | 奥克尼卡公司 | 表面强化的光谱学活性复合纳米颗粒 |
| WO2012164024A1 (en) * | 2011-06-03 | 2012-12-06 | Bayer Technology Services Gmbh | Process for continuously preparing rare earth doped fluorescent nanoparticles, their solution and system therefor |
| CN103865537A (zh) * | 2012-12-17 | 2014-06-18 | 中国科学院大连化学物理研究所 | 一种稀土上转换纳米荧光探针及其制备和应用 |
| CN104479679A (zh) * | 2014-11-12 | 2015-04-01 | 辽宁大学 | 一种NaYF4:Yb3+/Er3+@Ag纳米复合材料及其制备方法及应用 |
| CN109971461A (zh) * | 2019-04-01 | 2019-07-05 | 暨南大学 | 一种上转换荧光选择性增强的复合材料及其制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 基于W18O49的表面增强拉曼散射性能与机理研究;顾凌军;《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》;20190115(第01期);第9、13、31-40页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110726705A (zh) | 2020-01-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Silver deposited polystyrene (PS) microspheres for surface-enhanced Raman spectroscopic-encoding and rapid label-free detection of melamine in milk powder | |
| Navarro et al. | Resonant light scattering spectroscopy of gold, silver and gold–silver alloy nanoparticles and optical detection in microfluidic channels | |
| Li et al. | Ag nanowire/nanoparticle-decorated MoS2 monolayers for surface-enhanced Raman scattering applications | |
| CN105259157B (zh) | 一种热点可见的表面增强拉曼散射基底、制备方法及利用该基底检测分子的方法 | |
| US9075010B2 (en) | Enhancement of molecular emission using optical-antenna structures | |
| Li et al. | Study on annealed graphene oxide nano-sheets for improving the surface enhanced fluorescence of silver nanoparticles | |
| CN103344624B (zh) | 一种溶液法制备表面增强拉曼散射基底的方法及应用 | |
| Liang et al. | Periodic arrays of 3D AuNP‐capped VO2 shells and their temperature‐tunable SERS performance | |
| CN114563385B (zh) | 一种基于谷胱甘肽保护的金铜纳米团簇与Ce3+形成组装体的荧光探针及其应用 | |
| CN109752363A (zh) | 一种速溶茶粉中农药残留的便携式拉曼光谱检测方法 | |
| Wang et al. | Influence of SiO2 layer on the plasmon quenched upconversion luminescence emission of core-shell NaYF4: Yb, Er@ SiO2@ Ag nanocomposites | |
| CN110726705B (zh) | 一种基于贵金属/半导体调控的发光薄膜基底的荧光染料检测方法 | |
| CN112938979A (zh) | 具有SERS效应的MXene复合材料及其制备方法和应用 | |
| Sun et al. | Silver decahedral nanoparticles with uniform and adjustable sizes for surface-enhanced Raman scattering-based thiram residue detection | |
| CN107903891B (zh) | 一种铜纳米团簇自组装体的制备方法及应用 | |
| Shang et al. | Ag@ DWs nanopillars as a nanoprobe for detection of R6G via surface-enhanced fluorescent | |
| Babamiri et al. | Solid surface fluorescence immunosensor for ultrasensitive detection of hepatitis B virus surface antigen using PAMAM/CdTe@ CdS QDs nanoclusters | |
| CN112394052A (zh) | 一种基于上转换纳米材料与bhq-1共振能量转移检测人附睾蛋白4的方法 | |
| Wang et al. | Optical properties of Ag@ cicada wing substrate deposited by Ag nanoparticles | |
| CN112014371B (zh) | 一种柔性半透明表面增强拉曼基底的制备方法及应用 | |
| Albini et al. | Glass supported SERS chips for emerging pollutant analyses | |
| Pan et al. | Investigation of sensitive SERS detection via a perovskite-coated Ag nanofilm | |
| Lin et al. | Quantitative SERS measurements by self-assembled ultra-smooth Au nanosphere superlattice with embedded internal reference | |
| Yi et al. | Electrochemiluminescence of CdTe quantum dots and sensitive detection of hemoglobin | |
| CN114910461B (zh) | 一种sers基底及其制备方法和应用 |
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 |