CN113480189B - 一种自组装制备三维金纳米多孔膜的方法 - Google Patents

一种自组装制备三维金纳米多孔膜的方法 Download PDF

Info

Publication number
CN113480189B
CN113480189B CN202110747215.XA CN202110747215A CN113480189B CN 113480189 B CN113480189 B CN 113480189B CN 202110747215 A CN202110747215 A CN 202110747215A CN 113480189 B CN113480189 B CN 113480189B
Authority
CN
China
Prior art keywords
quartz
glass
gold
self
assembly
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
Application number
CN202110747215.XA
Other languages
English (en)
Other versions
CN113480189A (zh
Inventor
王纯荣
王翠萍
张欢
谭智美
吴国强
洪艳平
颜贤仔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Agricultural University
Original Assignee
Jiangxi Agricultural University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jiangxi Agricultural University filed Critical Jiangxi Agricultural University
Priority to CN202110747215.XA priority Critical patent/CN113480189B/zh
Publication of CN113480189A publication Critical patent/CN113480189A/zh
Application granted granted Critical
Publication of CN113480189B publication Critical patent/CN113480189B/zh
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/06Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
    • C03C17/10Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the liquid phase
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5116Ag or Au
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/88Metals
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/25Metals
    • C03C2217/251Al, Cu, Mg or noble metals
    • C03C2217/254Noble metals
    • C03C2217/255Au

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

一种自组装制备三维金纳米多孔膜的方法,以柠檬酸或柠檬酸钠为还原剂与氯金酸反应制备金胶待用,在使用砂纸将玻璃或石英表面打磨形成粗糙表面,并将形成有粗糙表面的玻璃或石英浸入金胶中自组装反应24h后,取出,烘干即在玻璃或石英表面制备出三维金纳米多孔膜。本发明不需要高分子化合物等基底材料作为模板,采用固体表面自组装制备三维金纳米多孔膜,具有操作简便、低污染的特点,有效降低生产成本;且纳米膜形成无需要高分子模板参与,也不需要化学试剂将金纳米吸附在固体表面,故三维金纳米多孔膜所含杂质少、纯度高,对于分析检测方面的应用极为有利。

Description

一种自组装制备三维金纳米多孔膜的方法
技术领域
本发明涉及纳米粒子制备技术领域,尤其涉及一种自组装制备三维金纳米多孔膜的方法。
背景技术
金作为常见的贵重金属之一,由其制备的纳米结构具有优异的物理和化学性能,在拉曼光谱等领域具有广泛的用途,现已应用于食品、药品、环境等方面的检测研究。其中,三维金纳米多孔结构具有特殊的形状和光学性质,同时又拥有大量的“热点”与被检测物相互作用,可以对被检测物的拉曼光谱信号具有巨大的增强效应,在表面拉曼光谱检测方面受到了广泛关注。目前,国内外合成的三维金纳米多孔结构工艺比较复杂,主要制备方法有利用表面活性剂分子参与的软模板法和通过高分子化合物形成的多孔结构硬模板法,这两类传统制备工艺均需要模板参与、工艺比较复杂、纳米结构不易控制,且污染较大;另外,为了将金纳米结构固定在基底材料上,往往需要加入化学试剂对金纳米表面进行修饰,以增加其被固定的稳定性。
发明内容
本发明提供一种自组装制备三维金纳米多孔膜的方法,以解决上述背景技术中存在的问题。
本发明所解决的技术问题采用以下技术方案来实现:
一种自组装制备三维金纳米多孔膜的方法,以柠檬酸或柠檬酸钠为还原剂与氯金酸反应制备金胶待用,在使用砂纸将玻璃或石英表面打磨形成粗糙表面,并将形成有粗糙表面的玻璃或石英浸入金胶中自组装反应24h后,取出,烘干即在玻璃或石英表面制备出三维金纳米多孔膜;具体步骤如下:
(1)配置混合溶液
以柠檬酸或柠檬酸钠为还原剂与氯金酸混合得混合溶液;
(2)金胶制备
将步骤(1)所得混合溶液放置在反应池中,加热,进行化学还原反应1h制备金胶;
(3)玻璃或石英表面处理
将玻璃或石英表面用砂纸打磨,形成粗糙表面;
(4)制备三维金纳米多孔膜
将形成有粗糙表面的玻璃或石英表面浸入金胶反应24h,取出,烘干,即在玻璃或石英表面制备出三维金纳米多孔膜。
在本发明中,步骤(1)中,所述混合溶液中各组分最终浓度为:柠檬酸质量百分比为0.01%~0.2%,氯金酸质量百分比为0.01%~0.5%。
在本发明中,步骤(2)中,所述加热温度为100℃。
在本发明中,步骤(3)中,所述砂纸为60目~1200目。
在本发明中,步骤(4)中,所述烘干温度为40℃~100℃。
有益效果:
(1)本发明不需要高分子化合物等基底材料作为模板,采用固体表面自组装制备三维金纳米多孔膜,具有操作简便、低污染的特点,有效降低生产成本;
(2)本发明中所使用的原料比较容易获得,工艺方法简单,纳米膜形成无需要高分子模板参与,也不需要化学试剂将金纳米吸附在固体表面,故三维金纳米多孔膜所含杂质少、纯度高,对于分析检测方面的应用极为有利。
附图说明
图1为本发明的最佳实施例中制备的球形金纳米粒子表面膜截面示意图。
图2为本发明的最佳实施例中制备的球形金纳米粒子表面膜1示意图。
图3为本发明的最佳实施例中制备的三维金纳米多孔膜示意图。
图4为本发明的最佳实施例中制备的球形金纳米粒子表面膜2示意图。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体图示,进一步阐述本发明。
实施例1制备球形金纳米粒子表面膜1
将柠檬酸(或柠檬酸钠)与氯金酸混合溶解得到柠檬酸(或柠檬酸钠)质量百分比为0.02%与氯金酸质量百分比为0.01%的混合溶液,而后将混合溶液置入反应池中加热煮沸进行化学还原反应1h,制备金胶待用;在使用60目砂纸将玻璃表面打磨形成粗糙表面,并将其浸入金胶中自组装反应24h,取出,烘干,即在玻璃表面制备出球形金纳米粒子表面膜1,整个过程可以重复多次以调整球形金纳米粒子表面膜1的厚度。
实施例2制备三维金纳米多孔膜
将柠檬酸(或柠檬酸钠)与氯金酸混合溶解得到柠檬酸(或柠檬酸钠)质量百分比为0.1%与氯金酸质量百分比为0.2%的混合溶液,而后将混合溶液置入反应池中加热煮沸进行化学还原反应1h,制备金胶待用;在使用320目砂纸将玻璃表面打磨形成粗糙表面,并将其浸入金胶中自组装反应24h,取出,烘干,即在玻璃表面制备出三维金纳米多孔膜;整个过程可以重复多次以调整三维金纳米多孔膜的厚度。
实施例3制备球形金纳米粒子表面膜2
将柠檬酸(或柠檬酸钠)与氯金酸混合溶解得到柠檬酸(或柠檬酸钠)质量百分比为0.2%与氯金酸质量百分比为0.5%的混合溶液,而后将混合溶液置入反应池中加热煮沸进行化学还原反应1h,制备金胶待用;在使用1200目砂纸将石英表面打磨形成粗糙表面,并将其浸入金胶中自组装反应24h,取出,烘干,即在石英表面制备出球形金纳米粒子表面膜2,整个过程可以重复多次以调整球形金纳米粒子表面膜2的厚度。
在上述实施例1~实施例3中,以柠檬酸(或柠檬酸钠)与氯金酸为原料,采用水热法制备金胶,加热温度为100℃,而后将玻璃或石英浸入金胶中,以在玻璃或石英上自组装制备三维金纳米多孔膜,其仅在金纳米粒子形貌有区别,其原理是:利用固体表面引导金纳米粒子在自组装作用下,调控金纳米膜上粒子形貌;该方法能够不需要添加高分子有机物制备三维骨架,也不需要化学功能试剂即可将金纳米吸附在高分子骨架表面,进行自组装三维金纳米多孔膜,具有操作简便、所含杂质少、金纳米纯度高、环保的特点,对于其在分析检测方面的应用极为有利。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (4)

1.一种自组装制备三维金纳米多孔膜的方法,其特征在于,以柠檬酸或柠檬酸钠为还原剂与氯金酸反应制备金胶待用,在使用砂纸将玻璃或石英表面打磨形成粗糙表面,并将形成有粗糙表面的玻璃或石英浸入金胶中自组装反应24 h后,取出,烘干即在玻璃或石英表面制备出三维金纳米多孔膜;具体步骤如下:
(1)配置混合溶液
以柠檬酸或柠檬酸钠为还原剂与氯金酸混合得混合溶液;
(2)金胶制备
将步骤(1)所得混合溶液放置在反应池中,加热,进行化学还原反应1 h制备金胶;
(3)玻璃或石英表面处理
将玻璃或石英表面用砂纸打磨,形成粗糙表面;
(4)制备三维金纳米多孔膜
将形成有粗糙表面的玻璃或石英浸入金胶反应24 h,取出,烘干,烘干温度为40℃~100℃,即在玻璃或石英表面制备出三维金纳米多孔膜。
2.根据权利要求1所述的一种自组装制备三维金纳米多孔膜的方法,其特征在于,步骤(1)中,所述混合溶液中各组分最终浓度为:柠檬酸质量百分比为0.01%~0.2%,氯金酸质量百分比为0.01%~0.5%。
3.根据权利要求1所述的一种自组装制备三维金纳米多孔膜的方法,其特征在于,步骤(2)中,所述加热温度为100℃。
4.根据权利要求1所述的一种自组装制备三维金纳米多孔膜的方法,其特征在于,步骤(3)中,所述砂纸为60目~1200目。
CN202110747215.XA 2021-07-02 2021-07-02 一种自组装制备三维金纳米多孔膜的方法 Expired - Fee Related CN113480189B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110747215.XA CN113480189B (zh) 2021-07-02 2021-07-02 一种自组装制备三维金纳米多孔膜的方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110747215.XA CN113480189B (zh) 2021-07-02 2021-07-02 一种自组装制备三维金纳米多孔膜的方法

Publications (2)

Publication Number Publication Date
CN113480189A CN113480189A (zh) 2021-10-08
CN113480189B true CN113480189B (zh) 2022-08-19

Family

ID=77940075

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110747215.XA Expired - Fee Related CN113480189B (zh) 2021-07-02 2021-07-02 一种自组装制备三维金纳米多孔膜的方法

Country Status (1)

Country Link
CN (1) CN113480189B (zh)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999047570A1 (en) * 1998-03-18 1999-09-23 University Of Rochester Macromolecular self-assembly of microstructures, nanostructures, objects and mesoporous solids
US6025202A (en) * 1995-02-09 2000-02-15 The Penn State Research Foundation Self-assembled metal colloid monolayers and detection methods therewith
US20150345025A1 (en) * 2012-11-09 2015-12-03 Ben Gurion University Of The Negev Research And Development Authority Gold nanostructures and processes for their preparation
CN110987897A (zh) * 2019-11-19 2020-04-10 中国科学院大学温州研究院(温州生物材料与工程研究所) 一种用于气体检测的表面增强拉曼散射基底材料及其制备方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5376556A (en) * 1989-10-27 1994-12-27 Abbott Laboratories Surface-enhanced Raman spectroscopy immunoassay
US7212284B2 (en) * 2004-05-12 2007-05-01 General Electric Company Method for forming nanoparticle films and application thereof
JP5782643B2 (ja) * 2010-12-17 2015-09-24 国立研究開発法人産業技術総合研究所 ガラスコート金ナノ粒子及び蛍光増強金ナノ粒子とこれらの製造方法
CN102944542A (zh) * 2012-10-18 2013-02-27 胡建明 磨砂玻璃表面增强拉曼基底及其制备方法
CN102978592B (zh) * 2012-12-24 2014-11-05 厦门大学 一种硅表面湿法沉积金纳米颗粒的方法
CN103217410A (zh) * 2013-04-02 2013-07-24 南京理工大学 金纳米粒子修饰金刚石薄膜表面增强拉曼光谱基底的制备方法
CN104384508B (zh) * 2014-11-26 2016-07-06 厦门大学 一种二氧化硅包金纳米粒子针孔填补方法
CN106770171A (zh) * 2016-12-29 2017-05-31 中国科学院城市环境研究所 表面增强拉曼光谱基底和样品的制备方法
CN110567933A (zh) * 2019-06-28 2019-12-13 华东理工大学 Sers基底及其制备方法
CN110747435B (zh) * 2019-11-05 2021-03-30 清华大学 一种基于电化学粗化的纳米金薄膜sers基底制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6025202A (en) * 1995-02-09 2000-02-15 The Penn State Research Foundation Self-assembled metal colloid monolayers and detection methods therewith
WO1999047570A1 (en) * 1998-03-18 1999-09-23 University Of Rochester Macromolecular self-assembly of microstructures, nanostructures, objects and mesoporous solids
US20150345025A1 (en) * 2012-11-09 2015-12-03 Ben Gurion University Of The Negev Research And Development Authority Gold nanostructures and processes for their preparation
CN110987897A (zh) * 2019-11-19 2020-04-10 中国科学院大学温州研究院(温州生物材料与工程研究所) 一种用于气体检测的表面增强拉曼散射基底材料及其制备方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Formation Process of Two-Dimensional Networked Gold Nanowires by Citrate Reduction of AuCl4- and the Shape Stabilization;Lihua Pei等;《Langmuir》;20040729;第20卷(第18期);全文 *
Self-assembly urchin-like Au-NSs arrays and application as surface-enhanced Raman scattering substrate;Chengquan Zhong等;《Materials Letters》;20190101;第234卷;全文 *
自组装金纳米粒子薄膜AFM研究;姜德生等;《电子显微学报》;20040425(第02期);全文 *

Also Published As

Publication number Publication date
CN113480189A (zh) 2021-10-08

Similar Documents

Publication Publication Date Title
Gao et al. Ceramic membranes with mussel-inspired and nanostructured coatings for water-in-oil emulsions separation
Chen et al. Preparation of high-flux γ-alumina nanofiltration membranes by using a modified sol–gel method
CN105158229B (zh) 一种高灵敏性可循环表面增强拉曼光谱基底制备方法
Liu et al. Shape-and size-dependent catalysis activities of iron-terephthalic acid metal-organic frameworks
CN109164074B (zh) 一种单分散胺化纳米金刚石胶体溶液的制备方法及其二次分散工艺和在细胞标记中的应用
CN107349787B (zh) 一种添加氨基化石墨烯量子点的正渗透膜制备方法、所制备的正渗透膜以及该膜的应用
Guo et al. Vertical 3D Printed Forest‐Inspired Hierarchical Plasmonic Superstructure for Photocatalysis
CN105112897A (zh) 一种多孔铜金复合纳米膜材料的制备方法
CN111617744B (zh) 一种基于Fe-MOFs的磁性多孔碳吸附材料及其制法
Jiang et al. Anti-aggregation and morphology-controlled effects of bacterial cellulose encapsulated BiOBr for enhanced photodegradation efficiency
JP2013542157A (ja) 不規則多孔質二酸化ケイ素材料の製造及びその製造における脂肪アルコールポリオキシエチレンエーテルの応用
CN113480189B (zh) 一种自组装制备三维金纳米多孔膜的方法
CN103264166A (zh) 银纳米片厚度可控的自组装银球sers基底的制备方法
Zhang et al. Self-assembly of porous cellulose fibers and the incorporation of graphene carbon quantum dots for stable luminescence
CN113369490A (zh) 一种空心球形银粉的制备方法
Lu et al. Bio-synthesis of molecularly imprinted membrane with photo-regeneration availability for selective separation applications
CN109616308B (zh) 一种球形纳米氧化铱dna提取磁性粉末及其生产方法
CN108822738B (zh) 一种琉璃化学抛光液
Zheng et al. Facile synthesis of magnetic resorcinol–formaldehyde (RF) coated carbon nanotubes for methylene blue removal
CN106111030B (zh) 一种金/碳复合微球及其制备方法
CN206896898U (zh) 一种超疏水金属丝网
CN111975010A (zh) 一种基于d-阿拉伯糖还原的金纳米粒子制备
Chen et al. A simple method of preparing Ag nanoparticles coated silica colloidal crystals and polymer-Ag nanoparticles composite macroporous films
CN113564532A (zh) 一种Janus微球及其制备方法和应用
Cheng et al. Preparation of micron–sized polystyrene/silver core–shell microspheres by ultrasonic assisted electroless plating

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
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20220819