CN103251949A - Nanometer composite material having gold/tetra-sulfide hepta-copper core-shell structure and preparation method thereof - Google Patents
Nanometer composite material having gold/tetra-sulfide hepta-copper core-shell structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nanometer composite material having a gold/tetra-sulfide hepta-copper core-shell structure and a preparation method of the nanometer composite material. The method comprises the following steps of: reducing chloroauric acid under a boiling condition to obtain a gold nano-particle sol solution; cleaning and concentrating the solution; dispersing into a cupric nitrate solution to ensure that the volume ratio of the gold nano-particle sol solution and the cupric nitrate solution is 0.05-0.5; reducing by using hydrazine hydrate to obtain gold/cuprous oxide core-shell structure particles; and finally, reacting gold/ cuprous oxide particles with excessive amount of sodium sulfide in ethyl alcohol to obtain the nanometer composite material having the gold/tetra-sulfide hepta-copper core-shell structure. The preparation method of the composite material is simple and mild in condition; and in the preparation process, the particle dispersibility is good, the size is accurately controlled, the aim of medicinal-thermal co-therapy (medicine chemotherapy and laser-induced thermotherapy) against cancers is fulfilled, and the significance to the development of a cancer treatment method is realized.
Description
Technical field
The present invention relates to a kind of gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials and preparation method thereof.Belong to gold and sulfide technical field of composite materials.
Background technology
Cancer is threatening human beings'health greatly as a kind of public health problem of the whole world, and becomes first killer who causes human death day by day.Therefore, about treatment for cancer be huge challenge and the primary study direction of medical domain always.At present, the traditional treatment method for cancer mainly contains chemotherapy, radiotherapy, operative treatment and hormone immunity treatment etc., although these methods have certain effect for treatment for cancer, but also exist simultaneously and cause human normal cell's death easily, the shortcoming of destroying the human immune system and causing several aspects such as recurrence again of cancer.Research and clinical data show widely, laserthermia can overcome the shortcoming of these traditional therapies well for treatment for cancer, realized the important breakthrough to treatment of cancer, its principle mainly is laser light energy is converted into heat energy causes tumor tissues temperatures at localized regions fast rise until surpassing the threshold value that cell survives institute's heatproof degree by using certain photo-thermal conversion agent, thereby melting fast of carrying out of cancerous cell killed, reach therapeutic effect.Therefore, in order to realize the better healing to cancer, the synthetic photo-thermal transforming agent with high photo-thermal conversion efficiency of research has crucial effects for laserthermia in the development aspect the treatment of cancer.Copper sulphur compound (Cu appraises at the current rate
2-xS, 0＜x＜1, mainly comprise four sulfurations, seven bronze medals, five sulfuration nine bronze medals and copper sulfide etc.) because the existence of its stronger local surfaces plasma resonance effect, thereby can show very high photo-thermal transformation efficiency, having broad application prospects aspect the laserthermia of cancer.At present, be applied to the cancer laserthermia about the copper sulphur compound as the photo-thermal transforming agent both at home and abroad certain research is arranged, but the copper sulphur compound particle size that obtains is all bigger, and synthetic method complexity, the condition harshness, preparation cost is higher, has therefore limited its further application aspect the research of cancer clinical treatment greatly.In other one side, in order further to improve the effect for the treatment of cancer, often medicine chemotherapy and laserthermia are carried out combination in the research, by the synergism of these two kinds of methods, effectively realize the quick treatment to cancer.Based on this, prepare a kind of copper sulphur compound nano-particle with nucleocapsid structure by template, utilizing on the one hand internal cavities to carry out medicine carries and passs, utilize copper sulphur compound shell that laser light energy is converted into heat energy on the other hand, thereby reach the medicine of tumor tissues heat is treated altogether, be significant for the development of cancer treatment method.
Summary of the invention
The object of the present invention is to provide a kind of gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials and preparation method thereof.Described gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials are expected to reach cancer are carried out the purpose that medicine heat is treated (combination of medicine chemotherapy and laserthermia) altogether, development for cancer treatment method is significant, this preparation methods is simple, mild condition.
The present invention is achieved by the following technical solutions, a kind of gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials, it is characterized in that, the particle diameter of this gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials is 50 ~ 200 nm, its core is gold nano grain, particle diameter is 10 ~ 30 nm, and the gold nano grain core is coating four sulfurations, seven bronze medal shells outward, and shell thickness is 10 ~ 40 nm.
The preparation method of the gold of said structure/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials is characterized in that comprising the steps:
1) be to be heated to boiling under 0.01% aqueous solution of chloraurate stirs with mass fraction, adding mass concentration subsequently is 1.0% sodium citrate aqueous solution, and its volumetric usage is 1/50 of aqueous solution of chloraurate, behind reaction 15 ~ 60 min, be cooled to room temperature, obtain the sol solution of gold nano grain;
2) with 1) sol solution of the gold nano grain of step preparation, behind speed centrifugalize 5 ~ 20 min with 6000 ~ 12000 r/min, remove supernatant, add deionized water by the volume of gold nano grain sol solution 1/2 in the lower floor gold nano grain precipitation and disperse, obtain gold nano grain solution;
3) in the copper nitrate solution of 0.005 ~ 0.1 mol/L, add polyvinylpyrrolidone, the concentration that makes polyvinylpyrrolidone is 0.01 ~ 0.2 g/ml, obtain the mixed solution of copper nitrate, under 20 ~ 80 ℃ of stirrings of constant temperature, by volume for 1:0.05 ~ 0.5 with copper nitrate mixed solution and step 2) the gold nano grain solution that makes mixes, add mass fraction again and be 99% hydrazine hydrate, wherein the volume ratio of hydrazine hydrate and copper nitrate mixed solution is 0.0002 ~ 0.002:1, behind reaction 2 ~ 60 min, product is separated cleaning remove the unreacted ion, obtain gold/Red copper oxide nuclear shell structure nano granule;
4) with 3) gold/Red copper oxide nuclear shell structure nano granule of step preparation is scattered in the ethanol, its concentration is 2 ~ 0.1 mg/ml, be that 1.1 ~ 5.0:1 stirs down that to add concentration in the alcoholic solution of gold/Red copper oxide nuclear shell structure nano granule be 0.05 ~ 1.0 mol/L sodium sulfide solution by the amount of substance ratio of sodium sulfide and Red copper oxide, behind reaction 20 ~ 120 min, product is cleaned separation, obtain gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials.
Gold provided by the invention/four sulfurations, seven bronze medal nano composite materials have nucleocapsid structure, its center is gold nano grain, shell is four sulfurations, seven bronze medals, particle size distribution is even, the gold of granule interior endorses to carry out grafting with band sulfydryl medicine, cavity then can be used for carrying of non-grafting class medicine and pass, thereby reach this material to the purpose of multiple drug selectivity controllable release, the shell of four sulfurations, seven bronze medals can be converted into heat energy with laser light energy simultaneously, be expected to final the realization photo-thermal of tumor tissues is treated altogether, be significant for the development of cancer treatment method.Composite material and preparation method thereof provided by the invention is simple, mild condition, in preparation process, the granule favorable dispersibility, and the amount of the gold nano grain solution by the control concentration of copper nitrate solution and adding can realize the accuracy controlling to gold/four sulfuration seven bronze medal nuclear-shell structured nano-composite material particle sizes and internal cavities size.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the gold that makes of embodiment 1/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials
The low power transmission electron microscope photo that Fig. 2 makes for embodiment 1.
The high power transmission electron microscope photo that Fig. 3 makes for embodiment 1.
The specific embodiment
Embodiment 1
1) getting 25 ml mass fractions is to be heated to boiling under 0.01% aqueous solution of chloraurate stirs, and adding 0.5 ml concentration subsequently is 1.0% sodium citrate aqueous solution, react 15 min after, be cooled to room temperature, obtain gold nano particle colloidal sols solution.
2) with 1) the aurosol solution (20 ml) of step preparation, behind speed centrifugalize 20 min with 6000 r/min, remove supernatant, adding 10 ml deionized waters in lower floor's gold nano grain disperses, and obtains gold nano grain solution.
3) getting 50 ml concentration is the copper nitrate solution of 0.005 mol/L, obtain the copper nitrate mixed solution to wherein adding 0.5 g polyvinylpyrrolidone, under 80 ℃ of stirrings of constant temperature, add 2.5 ml steps 2) the gold nano grain solution that makes, and then to add 0.01 ml mass fraction be 99% hydrazine hydrate, after reacting 2 min, product is separated and removes the unreacted ion with washed with de-ionized water three times, obtain gold/Red copper oxide nuclear shell structure nano granule.
4) with 3) gold/Red copper oxide nuclear shell structure nano granule of step preparation is scattered in the 50 ml ethanol, its concentration is 0.1 mg/ml, stirring down, adding 0.04 ml concentration is 1.0 mol/L sodium sulfide solutions, after reacting 20 min, separated product is also used washed with de-ionized water three times, obtains gold/four sulfuration seven bronze medal nuclear-shell structured nano-composite materials and carries out XRD and transmission electron microscope observing.Fig. 1 is X ray diffracting spectrum, and Fig. 2 is the low power transmission electron microscope photo of composite, and Fig. 3 is the high power transmission electron microscope photo of composite.
Test result: X-ray diffraction spectrum confirms that composite vulcanizes these two kinds of materials of seven bronze medals by gold and four and forms, the transmission electron microscope photo confirms that gold/four sulfurations, seven bronze medal nano composite materials have nucleocapsid structure, and nuclear is gold grain, shell is four sulfurations, seven bronze medals, the granule mean diameter is about 90 nanometers, has good dispersibility.
Embodiment 2
1) getting 25 ml mass fractions is to be heated to boiling under 0.01% aqueous solution of chloraurate stirs, and adding 0.5 ml concentration subsequently is 1.0% sodium citrate aqueous solution, react 40 min after, be cooled to room temperature, obtain gold nano particle colloidal sols solution.
2) with 1) the aurosol solution (20 ml) of step preparation, behind speed centrifugalize 10 min with 10000 r/min, remove supernatant, adding 10 ml deionized waters in lower floor's gold nano grain disperses, and obtains gold nano grain solution.
3) getting 50 ml concentration is the copper nitrate solution of 0.05 mol/L, obtain the copper nitrate mixed solution to wherein adding 5 g polyvinylpyrrolidones, under 80 ℃ of stirrings of constant temperature, add 5 ml steps 2) the gold nano grain solution that makes, and then to add 0.05 ml mass fraction be 99% hydrazine hydrate, after reacting 40 min, product is separated and removes the unreacted ion with washed with de-ionized water three times, obtain gold/Red copper oxide nuclear shell structure nano granule.
4) with 3) gold/Red copper oxide nuclear shell structure nano granule of step preparation is scattered in the 50 ml ethanol, its concentration is 0.5 mg/ml, stirring down, adding 1.74 ml concentration are 0.2 mol/L sodium sulfide solution, after reacting 60 min, separated product is also used washed with de-ionized water three times, obtains gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials.
Embodiment 3
1) getting 50 ml mass fractions is to be heated to boiling under 0.01% aqueous solution of chloraurate stirs, and adding 1 ml concentration subsequently is 1.0% sodium citrate aqueous solution, react 60 min after, be cooled to room temperature, obtain gold nano particle colloidal sols solution.
2) with 1) 50 ml aurosol solution of step preparation, behind speed centrifugalize 5 min with 12000 r/min, remove supernatant, adding 25 ml deionized waters in lower floor's gold nano grain disperses, and obtains gold nano grain solution.
3) getting 50 ml concentration is the copper nitrate solution of 0.1 mol/L, obtain the copper nitrate mixed solution to wherein adding 10 g polyvinylpyrrolidones, under 20 ℃ of stirrings of constant temperature, add 25 ml steps 2) the gold nano grain solution that makes, and then to add 0.1 ml mass fraction be 99% hydrazine hydrate, after reacting 60 min, product is separated and removes the unreacted ion with washed with de-ionized water three times, obtain gold/Red copper oxide nuclear shell structure nano granule.
4) with 3) gold/Red copper oxide nuclear shell structure nano granule of step preparation is scattered in the 50 ml ethanol, its concentration is 2 mg/ml, stirring down, adding 17.5 ml concentration are 0.05 mol/L sodium sulfide solution, after reacting 120 min, separated product is also used washed with de-ionized water three times, obtains gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials.
Claims (2)
1. gold/four vulcanize seven bronze medal nuclear-shell structured nano-composite materials, it is characterized in that, the particle diameter of this gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials is 50 ~ 200 nm, its core is gold nano grain, particle diameter is 10 ~ 30 nm, the gold nano grain core is coating four sulfurations, seven bronze medal shells outward, and shell thickness is 10 ~ 40 nm.
2. the preparation method by the described gold of claim 1/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials is characterized in that comprising the steps:
1) be to be heated to boiling under 0.01% aqueous solution of chloraurate stirs with mass fraction, adding mass concentration subsequently is 1.0% sodium citrate aqueous solution, and its volumetric usage is 1/50 of aqueous solution of chloraurate, behind reaction 15 ~ 60 min, be cooled to room temperature, obtain the sol solution of gold nano grain;
2) with 1) sol solution of the gold nano grain of step preparation, behind speed centrifugalize 5 ~ 20 min with 6000 ~ 12000 r/min, remove supernatant, add deionized water by the volume of gold nano grain sol solution 1/2 in the lower floor gold nano grain precipitation and disperse, obtain gold nano grain solution;
3) in the copper nitrate solution of 0.005 ~ 0.1 mol/L, add polyvinylpyrrolidone, the concentration that makes polyvinylpyrrolidone is 0.01 ~ 0.2 g/ml, obtain the mixed solution of copper nitrate, under 20 ~ 80 ℃ of stirrings of constant temperature, by volume for 1:0.05 ~ 0.5 with copper nitrate mixed solution and step 2) the gold nano grain solution that makes mixes, add mass fraction again and be 99% hydrazine hydrate, wherein the volume ratio of hydrazine hydrate and copper nitrate mixed solution is 0.0002 ~ 0.002:1, behind reaction 2 ~ 60 min, product is separated cleaning remove the unreacted ion, obtain gold/Red copper oxide nuclear shell structure nano granule;
4) with 3) gold/Red copper oxide nuclear shell structure nano granule of step preparation is scattered in the ethanol, its concentration is 2 ~ 0.1 mg/ml, be that 1.1 ~ 5.0:1 stirs down that to add concentration in the alcoholic solution of gold/Red copper oxide nuclear shell structure nano granule be 0.05 ~ 1.0 mol/L sodium sulfide solution by the amount of substance ratio of sodium sulfide and Red copper oxide, behind reaction 20 ~ 120 min, product is cleaned separation, obtain gold/four sulfurations, seven bronze medal nuclear-shell structured nano-composite materials.
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| CN105618781A (en) * | 2016-01-02 | 2016-06-01 | 华东理工大学 | Preparation method of Au@Cu2-xSe cage-like core-shell nanostructures |
| CN106475554A (en) * | 2015-08-31 | 2017-03-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Metal selenide coats the two-step method synthetic method of noble metal nanocrystalline |
| CN107297511A (en) * | 2016-04-15 | 2017-10-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method that dynamic reversible regulates and controls surface plasma body resonant vibration property |
| CN109465017A (en) * | 2018-11-19 | 2019-03-15 | 黑龙江大学 | A kind of seven bronze medals-eight of four vulcanization vulcanize controllable method for preparing and the application of nine bronze medal heterojunction structure hollow cubic body catalysts |
| CN110151993A (en) * | 2019-05-29 | 2019-08-23 | 上海师范大学 | A kind of diagnosis and treatment of colon cancer intelligence nanogold-cuprous oxide preparation and its application |
| CN110980796A (en) * | 2019-12-27 | 2020-04-10 | 上海保鼎科技服务有限公司 | Cu assembled by thin sheets7S4Nano flower material and preparation method and application thereof |
| CN115212896A (en) * | 2022-07-26 | 2022-10-21 | 河北工业大学 | Nano-porous copper-loaded heptacopper tetrasulfide @ cuprous oxide nanowire cluster composite material and preparation method and application thereof |
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2013
- 2013-04-15 CN CN2013101299139A patent/CN103251949A/en active Pending
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| LIZHEN ZHOU 等: "Ion-Exchange Route to Au−CuxOS Yolk−Shell Nanostructures with Porous Shells and Their Ultrasensitive H2O2 Detection", 《ACS APPLIED MATERIALS & INTERFACES》 * |
| LIZHEN ZHOU 等: "Ion-Exchange Route to Au−CuxOS Yolk−Shell Nanostructures with Porous Shells and Their Ultrasensitive H2O2 Detection", 《ACS APPLIED MATERIALS & INTERFACES》, no. 04, 27 November 2012 (2012-11-27) * |
Cited By (11)
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| CN106475554A (en) * | 2015-08-31 | 2017-03-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Metal selenide coats the two-step method synthetic method of noble metal nanocrystalline |
| CN105618781A (en) * | 2016-01-02 | 2016-06-01 | 华东理工大学 | Preparation method of Au@Cu2-xSe cage-like core-shell nanostructures |
| CN105618781B (en) * | 2016-01-02 | 2018-06-12 | 华东理工大学 | A kind of Au@Cu2-xThe preparation method of Se caged nanometer nuclear shell nano-structures |
| CN107297511A (en) * | 2016-04-15 | 2017-10-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method that dynamic reversible regulates and controls surface plasma body resonant vibration property |
| CN107297511B (en) * | 2016-04-15 | 2019-04-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method of dynamic reversible regulation surface plasma body resonant vibration property |
| CN109465017A (en) * | 2018-11-19 | 2019-03-15 | 黑龙江大学 | A kind of seven bronze medals-eight of four vulcanization vulcanize controllable method for preparing and the application of nine bronze medal heterojunction structure hollow cubic body catalysts |
| CN109465017B (en) * | 2018-11-19 | 2021-06-08 | 黑龙江大学 | Controllable preparation method and application of heptacopper tetrasulfide-nonacopper octasulfide heterostructure hollow cubic catalyst |
| CN110151993A (en) * | 2019-05-29 | 2019-08-23 | 上海师范大学 | A kind of diagnosis and treatment of colon cancer intelligence nanogold-cuprous oxide preparation and its application |
| CN110980796A (en) * | 2019-12-27 | 2020-04-10 | 上海保鼎科技服务有限公司 | Cu assembled by thin sheets7S4Nano flower material and preparation method and application thereof |
| CN115212896A (en) * | 2022-07-26 | 2022-10-21 | 河北工业大学 | Nano-porous copper-loaded heptacopper tetrasulfide @ cuprous oxide nanowire cluster composite material and preparation method and application thereof |
| CN115212896B (en) * | 2022-07-26 | 2023-07-14 | 河北工业大学 | Nano-porous copper-loaded hepta copper tetrasulfide@cuprous oxide nanowire cluster composite material and preparation method and application thereof |
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Application publication date: 20130821 |