CN110102776A - 一种在有机相中合成金纳米球、金纳米棒、金纳米线的方法 - Google Patents
一种在有机相中合成金纳米球、金纳米棒、金纳米线的方法 Download PDFInfo
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000010931 gold Substances 0.000 title claims abstract description 77
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 29
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 22
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000005642 Oleic acid Substances 0.000 claims abstract description 22
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 22
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
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- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 18
- 239000002070 nanowire Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 4
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- 238000002604 ultrasonography Methods 0.000 claims description 3
- SNXYSMKZWUVGEF-UHFFFAOYSA-K trichlorogold tetrahydrate Chemical compound O.O.O.O.Cl[Au](Cl)Cl SNXYSMKZWUVGEF-UHFFFAOYSA-K 0.000 claims description 2
- NEYLGXVZJUUZMY-UHFFFAOYSA-K potassium;trichlorogold Chemical compound [K].Cl[Au](Cl)Cl NEYLGXVZJUUZMY-UHFFFAOYSA-K 0.000 claims 1
- AKQNYQDSIDKVJZ-UHFFFAOYSA-N triphenylsilane Chemical group C1=CC=CC=C1[SiH](C=1C=CC=CC=1)C1=CC=CC=C1 AKQNYQDSIDKVJZ-UHFFFAOYSA-N 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 2
- 238000005063 solubilization Methods 0.000 abstract description 2
- 230000007928 solubilization Effects 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- BZLZKLMROPIZSR-UHFFFAOYSA-N triphenylsilicon Chemical group C1=CC=CC=C1[Si](C=1C=CC=CC=1)C1=CC=CC=C1 BZLZKLMROPIZSR-UHFFFAOYSA-N 0.000 description 12
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- -1 oleyl amines Chemical class 0.000 description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 5
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 5
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- 238000010183 spectrum analysis Methods 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035040 seed growth Effects 0.000 description 2
- JAJIPIAHCFBEPI-UHFFFAOYSA-N 9,10-dioxoanthracene-1-sulfonic acid Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)O JAJIPIAHCFBEPI-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- TVJORGWKNPGCDW-UHFFFAOYSA-N aminoboron Chemical compound N[B] TVJORGWKNPGCDW-UHFFFAOYSA-N 0.000 description 1
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Abstract
一种合成金纳米球、金纳米棒、金纳米线的方法,所述方法为:将金前驱体溶于有机溶剂中,然后加入增溶剂,超声,接着加入还原剂,室温搅拌反应2~6h,得到金纳米材料;本发明将油胺油酸引入到金前驱体的增溶步骤中,使得金前驱体可以在有机溶剂中具有良好的分散性,并利用油胺、油酸在金纳米材料表面选择性吸附,实现了金纳米球、金纳米棒、金纳米线的合成,通过简单的调整金前驱体与还原剂、增溶剂的比例,可以有效控制金纳米球的粒径以及金纳米材料的形貌;本发明方法简单易行,重复性高,稳定性高,产率高。
Description
(一)技术领域:
本发明涉及在有机相中合成金纳米球、金纳米棒、金纳米线的方法。
(二)背景技术:
近几十年来,金纳米材料因其独特的尺寸效应和电子结构,在催化、生物医学、生物成像、电子学、光子学以及表面增强拉曼光谱等研究领域有着重大的应用前景,受到科研人员的广泛关注。球形金纳米颗粒的粒径以及金纳米材料的形貌对其性能有着重要的影响。
目前,常规的有机相金纳米材料制备方法包括使用氨基-硼烷络合物还原有机溶剂中金盐合成均匀金纳米球,使用电子束光刻技术合成金纳米棒以及使用长链烷基胺充当还原剂和封端剂合成金纳米线。上述技术中,大部分的方法都存在反应时间长,温度高,操作复杂,成本高等缺点。如专利CN103769605A发明了一种油溶性金纳米颗粒的合成方法,该发明将短链有机胺引入到晶种生长法的生长溶液中,得到大尺寸Au纳米颗粒。但是种子液的生长过程中需要使用注射泵精确控制生长液的流速,操作较为繁琐,且反应时间较长(>12h)。因此开发一种简单易行的金纳米球、金纳米棒、金纳米线合成方法具有重要意义。
(三)发明内容
本发明的目的是提供一种室温条件下合成金纳米球、金纳米棒、金纳米线的方法。将油胺油酸引入到金前驱体的增溶步骤中,使得金前驱体可以在有机溶剂中具有良好的分散性。并利用油胺、油酸在金纳米材料表面选择性吸附,实现了金纳米球、金纳米棒、金纳米线的合成。通过简单的调整金前驱体与还原剂、增溶剂的比例,可以有效控制金纳米球的粒径以及金纳米材料的形貌。
本发明的技术方案如下:
一种合成金纳米球、金纳米棒、金纳米线的方法,所述方法为:
将金前驱体溶于有机溶剂中,然后加入增溶剂,超声(功率为100~150W,时间为0.5~1min,溶液由金黄色浑浊溶液变为淡黄色透明溶液),接着加入还原剂,室温(25~35℃)搅拌反应2~6h,得到金纳米材料(直接以溶液形式保存,无需从体系中分离);
所述金前驱体为氯金酸四水合物或氯金酸钾,所述有机溶剂为氯仿,所述金前驱体与有机溶剂的质量比为1:2400~12000;
所述还原剂为三苯基硅烷,所述金前驱体与还原剂的质量比为1:1.9~300;推荐所述还原剂以4.8~150mg/mL还原剂的氯仿溶液的形式投料;
所述增溶剂为油胺和油酸的混合溶剂;
当金前驱体、油酸、油胺的质量比为1:0.2~2.7:0.8~12时,最终所得金纳米材料为金纳米球;
当金前驱体、油酸、油胺的质量比为1:18~32.4:19.2~27.2时,最终所得金纳米材料为金纳米棒;
当金前驱体、油酸、油胺的质量比为1:5.4~16.2:28.8~72时,最终所得金纳米材料为金纳米线。
本发明所述方法制得的金纳米球粒径3~100nm,金纳米棒长径比为1.5~13,超细金纳米线长径比为50~1000。
本发明的主要优点在于:
(1)采用一步法湿法合成金纳米球、金纳米棒、金纳米线,方法简单易行,重复性高,稳定性高,产率高。
(2)实现了从纳米球,纳米棒到纳米线的合成。
(3)反应时间短,最长不超过6h。
(4)反应条件温和,均在室温条件下反应。
(5)所得金纳米材料能稳定保存2个月以上不发生团聚。
(四)附图说明
图1为实施例1(a),实施例2(b),实施例3(c)所合成的不同粒径金纳米球的透射电镜图片。
图2为实施例4(a),实施例5(b)所合成的不同长径比金纳米棒的透射电镜图片。
图3为实施例6(a),实施例7(b),实施例8(c)所合成的不同长径比金纳米线的透射电镜图片。
图4为实施例1所合成金纳米球的能谱分析图,其中C和Cu元素的峰来自超薄碳支持膜,Si元素的峰来自还原剂。
图5为实施例4所合成金纳米棒的能谱分析图,其中C和Cu元素的峰来自超薄碳支持膜,Si元素的峰来自还原剂。
图6为实施例6所合成金纳米线的能谱分析图,其中C和Cu元素的峰来自超薄碳支持膜,Si元素的峰来自还原剂。
(五)具体实施方式
下面结合具体实施例对本发明作进一步阐述,但本发明并不限于以下实施例。
所述方法如无特别说明均为常规方法。所述原材料如无特别说明均能从公开商业途径获得。
实施例1
取5.0mg氯金酸,溶于8.0mL(12g)氯仿中,获得金黄色氯金酸溶液。再用移液枪吸取3μL(2.7mg)油酸和15μL(12mg)油胺至氯金酸溶液中,超声1min,溶液由金黄色变为淡黄色。用钥匙称取9.5mg三苯基硅烷固体粉末,将其溶于2.0mL氯仿中,超声1min,至三苯基硅烷完全溶解。将三苯基硅烷溶液加入金前驱体溶液,磁力搅拌,在室温(25-35℃)下反应2.5h,得如图1a所示平均粒径为13.9nm的金纳米球。
实施例2
按照与实施例1相同步骤,氯金酸添加量改为1.0mg,三苯基硅烷添加量改为300.0mg,得到如图1b所示平均粒径为2nm的金纳米球。
实施例3
按照与实施例1相同步骤,油酸的添加量改为1μL(0.9mg),油胺的添加量改为5μL(4mg),得到如图1c所示平均粒径为100nm的金纳米球。
实施例4
取5.0mg氯金酸,溶于8.0mL(12g)氯仿中,获得金黄色氯金酸溶液。再用移液枪吸取180μL(162mg)油酸和170μL(136mg)油胺至氯金酸溶液中,超声1min,溶液由橙黄色变为淡黄色。用钥匙称取9.5mg三苯基硅烷固体粉末,将其溶于2.0mL氯仿中,超声1min,至三苯基硅烷完全溶解。将三苯基硅烷溶液加入金前驱体溶液,磁力搅拌,在室温(25-35℃)下反应4h,得如图2a长径比1.5的金纳米棒。
实施例5
按照与实施例4相同步骤,油胺和油酸添加量改为油酸100μL(90mg)和油胺120μL(96mg),得到如图2b所示的长径比为13的金纳米棒。
实施例6
取5.0mg氯金酸,溶于8.0mL(12g)氯仿溶液中,获得金黄色氯金酸溶液。再用移液枪吸取90μL(81mg)油酸和180μL(144mg)油胺至氯金酸溶液中,超声1min,溶液由橙色变为淡橙色。用钥匙称取9.5mg三苯基硅烷固体粉末,将其溶于2.0mL氯仿溶液中,超声1min,至三苯基硅烷完全溶解。将将三苯基硅烷溶液加入金前驱体溶液,磁力搅拌,在室温(25-35℃)下反应6h,得如图3a长径比为50的金纳米线。
实施例7
按照与实施例6相同步骤,油酸和油胺添加量改为油酸30μL(27mg)和油胺450μL(360mg),得到如图3b所示的长径比为1000的金纳米线。
实施例8
用移液枪吸取90μL(81mg)油酸和450μL(360mg)油胺至8.0mL(12g)氯仿中,然后取4.6mg氯金酸钾至油胺、油酸混合溶剂中,超声1min,溶液由无色变为淡橙色。用钥匙称取9.5mg三苯基硅烷固体粉末,将其溶于2.0mL氯仿中,超声1min,至三苯基硅烷完全溶解。将三苯基硅烷溶液加入金前驱体溶液,磁力搅拌,在室温(25-35℃)下反应6h,得如图3c所示的长径比为50的金纳米线。
对比例
专利CN103769605A发明了一种油溶性金纳米颗粒的合成方法,该发明将短链有机胺引入到晶种生长法的生长溶液中,得到大尺寸Au纳米颗粒。反应将180mL正辛烷、80mL油胺、20mL正丁胺和0.2mL 6nm金纳米颗粒,置于60℃水浴中搅拌10min。用注射泵以0.4mL/h的速度连续加入氯金酸的乙醇溶液,24h后停止加入样品,继续反应1h后得到47nm Au纳米颗粒。
该方法种子生长法制备球形金纳米颗粒与本方法相比,反应时间较长,操作比较复杂,对仪器设备以及操作人员的要求比较高。另一方面,该方法只控制了金纳米球的粒径,而本发明的制备方法可以通过简单调整金前驱体与还原剂、增溶剂的比例,有效控制金纳米球的粒径以及金纳米材料的形貌。
Claims (8)
1.一种合成金纳米球、金纳米棒、金纳米线的方法,其特征在于,所述方法为:
将金前驱体溶于有机溶剂中,然后加入增溶剂,超声,接着加入还原剂,室温搅拌反应2~6h,得到金纳米材料;
所述增溶剂为油胺和油酸的混合溶剂;
当金前驱体、油酸、油胺的质量比为1:0.2~2.7:0.8~12时,最终所得金纳米材料为金纳米球;
当金前驱体、油酸、油胺的质量比为1:18~32.4:19.2~27.2时,最终所得金纳米材料为金纳米棒;
当金前驱体、油酸、油胺的质量比为1:5.4~16.2:28.8~72时,最终所得金纳米材料为金纳米线。
2.如权利要求1所述的方法,其特征在于,所述超声的功率为100~150W,时间为0.5~1min。
3.如权利要求1所述的方法,其特征在于,所述金前驱体为氯金酸四水合物或氯金酸钾。
4.如权利要求1所述的方法,其特征在于,所述有机溶剂为氯仿。
5.如权利要求1所述的方法,其特征在于,所述金前驱体与有机溶剂的质量比为1:2400~12000。
6.如权利要求1所述的方法,其特征在于,所述还原剂为三苯基硅烷。
7.如权利要求1所述的方法,其特征在于,所述金前驱体与还原剂的质量比为1:1.9~300。
8.如权利要求1所述的方法,其特征在于,所述还原剂以4.8~150mg/mL还原剂的氯仿溶液的形式投料。
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CN110640160A (zh) * | 2019-09-23 | 2020-01-03 | 昆明理工大学 | 一种棒状铂纳米颗粒的制备方法 |
CN110732677A (zh) * | 2019-10-17 | 2020-01-31 | 浙江工业大学 | 一种形貌可控的油溶性钯纳米材料的制备方法 |
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CN113500201A (zh) * | 2021-06-30 | 2021-10-15 | 海南深远海新能源科技有限公司 | 一种金及其核壳纳米晶的制备方法及装置 |
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CN108031861A (zh) * | 2017-12-18 | 2018-05-15 | 中国科学院深圳先进技术研究院 | 金属纳米材料及其制备方法 |
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