CN108907222A - 一种金纳米簇的合成方法 - Google Patents

一种金纳米簇的合成方法 Download PDF

Info

Publication number
CN108907222A
CN108907222A CN201810591581.9A CN201810591581A CN108907222A CN 108907222 A CN108907222 A CN 108907222A CN 201810591581 A CN201810591581 A CN 201810591581A CN 108907222 A CN108907222 A CN 108907222A
Authority
CN
China
Prior art keywords
gold
gold nanoclusters
good
solution
nanoclusters
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.)
Withdrawn
Application number
CN201810591581.9A
Other languages
English (en)
Inventor
吴晓红
蒋彩云
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.)
Jiangsu Institute of Economic and Trade Technology
Original Assignee
Jiangsu Institute of Economic and Trade Technology
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 Jiangsu Institute of Economic and Trade Technology filed Critical Jiangsu Institute of Economic and Trade Technology
Priority to CN201810591581.9A priority Critical patent/CN108907222A/zh
Publication of CN108907222A publication Critical patent/CN108907222A/zh
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00Antineoplastic agents
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0553Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/58Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Veterinary Medicine (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)

Abstract

本发明公开了一种金纳米簇的合成方法。本发明通过二乙二醇、双羟乙基胺与金离子进行络合和热还原反应,制备得到金纳米簇。本发明方法克服了现有技术中颗粒尺寸难以控制、颗粒分散不均、金纳米材料难以很好形成金纳米簇的缺陷,制备出比表面积大、粒径均一、荧光效果好的金纳米簇。本发明中制备的金纳米簇,具有很好的荧光效果,同时可以进行光疗,可作为肿瘤早期治疗的潜在药物制剂应用于临床。本发明的合成方法简便易行、荧光效果好、光疗效果好、毒性低,具有广阔的医学临床应用价值和前景。

Description

一种金纳米簇的合成方法
技术领域
本发明涉及金纳米簇可以很好的进行荧光成像,并且具有很好的靶向性和光疗效果,具体涉及金纳米簇的合成方法。
背景技术
金纳米簇是由几个到大约一百个金原子组成的一种新型的荧光纳米材料,近几年来受到了广泛的关注。金纳米簇的直径通常不到2nm,性质在孤立的原子和纳米粒子之间。由于金纳米簇的尺寸和电子的费米波长接近,连续态密度分解成离散的能级,使他们与普通的纳米颗粒(直径大于2nm)的性质有明显的不同,比如,光学性质、化学性质以及电学性质。最显著的特征是部分纳米簇具有很强的发光特性,并且呈现出良好的光稳定性、高的发射效率以及大的斯托克斯位移。此外,最新发展起来的技术能够在各种生物相容性支架上简易地合成水溶性的荧光金属纳米簇,它们有着可调的发射颜色和不同的配体。荧光金纳米簇是一种新型的非常小的、生物相容好的荧光体,它可以用在生物标记及光电子发射器等方面。由于金纳米簇具备荧光寿命较长、斯托克斯位移值较大和比较好的生物相容性等许多优点,因此金纳米簇被广泛用于生物成像和物质检测等方面。
利用荧光成像实现对肿瘤的早期诊断并进行治疗是未来药学及治疗学不断追求的目标,已成为当今研究的热点之一。本发明提供金纳米簇的新合成方法,可以控制粒径大小以及具有良好的荧光成像效果并且将其应用到肿瘤早期诊断和治疗上,具有广阔的应用前景和经济效益。
发明内容
发明目的:本发明提供了一种金纳米簇的新合成方法。
技术方案:针对目前现有技术很难制备晶型好、荧光效果好的金纳米簇的缺陷,本发明提供了一种金纳米簇的新合成方法。
1.一种金纳米簇的合成方法,其特征在于由如下步骤制得:
(1)金的化合物在二乙二醇和双羟乙基胺混合溶液为溶剂的条件下进行超声溶解得到溶液A,溶液A中金离子浓度分别为0.001~1.0mol/L。
(2)将溶液A在温度为40~90℃的条件下加热,剧烈搅拌,反应时间1~5h,再在高温160~220℃条件下反应1~5h,得到产物B;
(3)将B中所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
2.根据权利要求1所述的方法,其中步骤(1)中所述金的化合物是氯金酸、八氯化四金、三氯化金、一氯化金中的一种或者任意几种的混合。
3.根据权利要求1所述的方法,其中步骤(1)中所述二乙二醇和双羟乙基胺混合溶液的浓度比为5:1~1:1。
有益效果:
(1)将金试剂与二乙二醇和双羟乙基胺混合溶液相络合,高温还原反应后制得金纳米簇。该方法操作简便,具有广阔的应用价值和前景。
(2)本发明的优点是:本发明的合成方法简便易行,制备的金纳米簇粒径均一、荧光效果好、毒性低,同时可以进行光疗,可作为肿瘤早期治疗的潜在药物制剂应用于临床。
附图说明
图1是本发明实施例1实验组荧光光谱图。
具体实施方式
实施例1
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度为0.1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间5h,再高温200℃,反应5h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。测得本产品的荧光光谱图,其中a为激发光谱,b为发射光谱,见图1。
实施例2
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度为1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间5h,再高温200℃,反应5h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
实施例3
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度分别为0.1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间1h,再高温200℃,反应1h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
实施例4
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度为0.1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间1h,再高温200℃,反应5h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
实施例5
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度为1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间1h,再高温200℃,反应1h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
实施例6
将氯金酸溶解在二乙二醇和双羟乙基胺浓度比1:1的混合溶液中,所得溶液中金离子浓度为0.1mol/L。将此溶液在温度60℃剧烈搅拌,反应时间5h,再高温220℃,反应5h。所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
以上所述仅是本发明的优选实施方式,应当指出:对于本技术领域的技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。

Claims (3)

1.一种金纳米簇的合成方法,其特征在于由如下步骤制得:
(1)金的化合物在二乙二醇和双羟乙基胺混合溶液为溶剂的条件下进行超声溶解得到溶液A,溶液A中金离子浓度分别为0.001~1.0mol/L;
(2)将溶液A在温度为40~90℃的条件下加热,剧烈搅拌,反应时间1~5h,再在高温160~220℃条件下反应1~5h,得到产物B;
(3)将B中所得产物冷却后用去离子水多次离心洗涤,获得相应产品。
2.根据权利要求1所述的方法,其中步骤(1)中所述金的化合物是氯金酸、八氯化四金、三氯化金、一氯化金中的一种或者任意几种混合物。
3.根据权利要求1所述的方法,其中步骤(1)中所述二乙二醇和双羟乙基胺混合溶液的浓度比为5:1~1:1。
CN201810591581.9A 2018-06-10 2018-06-10 一种金纳米簇的合成方法 Withdrawn CN108907222A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810591581.9A CN108907222A (zh) 2018-06-10 2018-06-10 一种金纳米簇的合成方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810591581.9A CN108907222A (zh) 2018-06-10 2018-06-10 一种金纳米簇的合成方法

Publications (1)

Publication Number Publication Date
CN108907222A true CN108907222A (zh) 2018-11-30

Family

ID=64419114

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810591581.9A Withdrawn CN108907222A (zh) 2018-06-10 2018-06-10 一种金纳米簇的合成方法

Country Status (1)

Country Link
CN (1) CN108907222A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109434133A (zh) * 2018-12-20 2019-03-08 江苏经贸职业技术学院 一种基于相转移法Au纳米材料的合成方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101511952A (zh) * 2006-08-07 2009-08-19 印可得株式会社 银纳米颗粒的制备方法和含有银纳米颗粒的银墨组合物
CN101610864A (zh) * 2007-02-15 2009-12-23 同和电子科技有限公司 银粒子粉末的制造方法
CN102105245A (zh) * 2008-07-23 2011-06-22 建筑研究和技术有限公司 在多元醇中制备金属纳米颗粒的方法
WO2014119793A1 (ja) * 2013-02-04 2014-08-07 国立大学法人山形大学 金属銀の析出方法、および被覆銀微粒子、細線状の被覆金属銀
CN104540622A (zh) * 2012-08-07 2015-04-22 株式会社大赛璐 用于生产银纳米粒子的方法和银纳米粒子
CN104755200A (zh) * 2012-08-23 2015-07-01 三星精密化学株式会社 金属纳米粒子的制造方法及利用该金属纳米粒子的金属纳米粒子油墨的制造方法
US20150290714A1 (en) * 2014-04-14 2015-10-15 Korea Basic Science Institute Manufacturing method of spherical gold (au) nanoparticles and spherical gold (au) nanoparticle manufactured by using the same

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101511952A (zh) * 2006-08-07 2009-08-19 印可得株式会社 银纳米颗粒的制备方法和含有银纳米颗粒的银墨组合物
CN101610864A (zh) * 2007-02-15 2009-12-23 同和电子科技有限公司 银粒子粉末的制造方法
CN102105245A (zh) * 2008-07-23 2011-06-22 建筑研究和技术有限公司 在多元醇中制备金属纳米颗粒的方法
CN104540622A (zh) * 2012-08-07 2015-04-22 株式会社大赛璐 用于生产银纳米粒子的方法和银纳米粒子
CN104755200A (zh) * 2012-08-23 2015-07-01 三星精密化学株式会社 金属纳米粒子的制造方法及利用该金属纳米粒子的金属纳米粒子油墨的制造方法
WO2014119793A1 (ja) * 2013-02-04 2014-08-07 国立大学法人山形大学 金属銀の析出方法、および被覆銀微粒子、細線状の被覆金属銀
JP2014152337A (ja) * 2013-02-04 2014-08-25 Yamagata Univ 金属銀の析出方法、および被覆銀微粒子、細線状の被覆金属銀
US20150290714A1 (en) * 2014-04-14 2015-10-15 Korea Basic Science Institute Manufacturing method of spherical gold (au) nanoparticles and spherical gold (au) nanoparticle manufactured by using the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
卢文婷等: "聚酰胺-胺型树形分子模板法制备Pt纳米簇", 《化学学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109434133A (zh) * 2018-12-20 2019-03-08 江苏经贸职业技术学院 一种基于相转移法Au纳米材料的合成方法

Similar Documents

Publication Publication Date Title
Duan et al. Recent progress in upconversion luminescence nanomaterials for biomedical applications
Wang et al. A self-quenching-resistant carbon dots powder with tunable solid-state fluorescence and their applications in light-emitting diodes and fingerprints detection
Cao et al. High-quality water-soluble and surface-functionalized upconversion nanocrystals as luminescent probes for bioimaging
Rafique et al. Morphological evolution of upconversion nanoparticles and their biomedical signal generation
Liao et al. Photoinduced electron transfer of poly (o-phenylenediamine)–Rhodamine B copolymer dots: application in ultrasensitive detection of nitrite in vivo
Lan et al. Highly stable organic fluorescent nanorods for living-cell imaging
Panov et al. Microwave-assisted solvothermal synthesis of upconverting and downshifting rare-earth-doped LiYF4 microparticles
JP2011526883A (ja) pH感受性金属ナノ粒子およびその製造方法
Jain et al. Rare-earth-doped Y3Al5O12 (YAG) nanophosphors: synthesis, surface functionalization, and applications in thermoluminescence dosimetry and nanomedicine
CN108456518B (zh) 一种强烈红色荧光的稀土纳米粒子及其制备方法和在细胞成像中的应用
CN108127124A (zh) 一种荧光颜色可调控的铜纳米簇的制备方法
CN103540310A (zh) 用于多形貌稀土上转换发光纳米晶表面直接介孔修饰的制备方法
CN106433627A (zh) 一种Cr3+掺杂的镓酸锌近红外长余辉发光纳米颗粒及制备方法
CN108907221A (zh) 一种铜纳米簇的合成方法
CN107158378A (zh) 一种光热效应用硫化铜锰蛋白复合纳米颗粒及其制备方法
CN111742034A (zh) 具有高度非辐射衰减抑制的碗烯包裹的aie纳米点用于增强体内癌症光诊疗
CN109504366A (zh) 一种稀土络合物包覆纳米空心SiO2和包覆型稀土络合物及其制备方法
CN111269720A (zh) 一种稀土掺杂双长余辉纳米材料及其制备方法和用途
CN105368447B (zh) 1‑甲基‑5‑巯基四氮唑‑牛血清白蛋白‑金纳米团簇荧光材料及其制备方法
CN112111266A (zh) 一种生物体内温度检测纳米晶材料及其制备方法和检测试剂盒
Xu et al. Construction of NaYF4: Eu@ carbon dots nanocomposites for multifunctional applications
CN110408377A (zh) 一种稀土掺杂NaCeF4近红外荧光纳米探针及其制备方法和生物应用
CN108907222A (zh) 一种金纳米簇的合成方法
Cui et al. Comparison of two strategies for the synthesis of upconverting nanoparticles as biological labels
Shao et al. Hydrothermal synthesis of poly (acrylic acid)-functionalized α-(β-) NaYF4: Yb, Er up-conversion nano-/micro-phosphors

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
WW01 Invention patent application withdrawn after publication

Application publication date: 20181130

WW01 Invention patent application withdrawn after publication