CN113480189B - 一种自组装制备三维金纳米多孔膜的方法 - Google Patents
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000010931 gold Substances 0.000 title claims abstract description 55
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000012528 membrane Substances 0.000 title claims abstract description 24
- 238000001338 self-assembly Methods 0.000 title claims abstract description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011521 glass Substances 0.000 claims abstract description 26
- 239000010453 quartz Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000001509 sodium citrate Substances 0.000 claims abstract description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000006722 reduction reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 15
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- 239000010970 precious metal Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
- C03C17/10—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the liquid phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating 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
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
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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
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。
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