CN105436514B - A kind of preparation method and applications of gold nano star/molybdenum disulfide composite - Google Patents
A kind of preparation method and applications of gold nano star/molybdenum disulfide composite Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 90
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 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 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 16
- 238000011065 in-situ storage Methods 0.000 claims abstract description 13
- 206010028980 Neoplasm Diseases 0.000 claims abstract description 3
- 238000002560 therapeutic procedure Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 70
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- 238000005119 centrifugation Methods 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 15
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229940069328 povidone Drugs 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims 3
- 229960000443 hydrochloric acid Drugs 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000004847 absorption spectroscopy Methods 0.000 abstract 1
- 238000007626 photothermal therapy Methods 0.000 description 7
- 238000000862 absorption spectrum Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 210000004881 tumor cell Anatomy 0.000 description 3
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920006335 epoxy glue Polymers 0.000 description 2
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical class Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- 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
- 241000549556 Nanos Species 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000030833 cell death Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 230000017074 necrotic cell death Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 238000001959 radiotherapy Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 238000000015 thermotherapy Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
- A61N5/00—Radiation therapy
- A61N5/06—Radiation therapy using light
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
- A61N5/00—Radiation therapy
- A61N5/06—Radiation therapy using light
- A61N5/067—Radiation therapy using light using laser light
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
- A61N5/00—Radiation therapy
- A61N5/06—Radiation therapy using light
- A61N2005/0658—Radiation therapy using light characterised by the wavelength of light used
- A61N2005/0659—Radiation therapy using light characterised by the wavelength of light used infrared
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- Animal Behavior & Ethology (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method and applications of gold nano star/molybdenum disulfide composite, method is：Molybdenum disulfide seed solution and chlorauric acid solution are mixed, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification.Advantage is：（1）The composite prepared has how dendritic star pattern and homogeneous size；Soilless sticking between particle, with good dispersiveness and biocompatibility, and in molybdenum disulfide lamellar structure, the load density of gold nano star is larger；（2）The ultraviolet-visible absorption spectroscopy peak value of the composite is between 600 1000nm, and temperature is raised rapidly under near-infrared laser irradiation, thus with preferable photothermal conversion performance, has huge application potential in terms of the tumor thermal therapy of biomedical sector；（3）The preparation process technique of the gold nano star/molybdenum disulfide composite is simple to operation, and equipment requirement is low；The impurity content of the composite prepared is few, and yield is high.
Description
Technical field
The invention belongs to photo-thermal therapy composite, it is related to a kind of preparation and application of molybdenum disulfide composite, especially
It is related to a kind of preparation method and applications of gold nano star/molybdenum disulfide composite.
Background technology
Thermotherapy（Photo-thermaL Therapy, PTT）It is the method by heating, changes tumour cell local environment,
Make tumour cell denaturation, necrosis.Reach therapeutic purposes.Heat energy produces different influences to cell, and low dosage heat treatment contributes to
The reply of damage, high dose heat treatment may cause cell death, and medium, gentle, the non-heat treatment for causing dosage can make tumour
Cell becomes sensitive to radiotherapy and many medicines.
Near infrared region（800nm~1200nm）It is the transmission window of body tissue, near infrared light is in body tissue transmitance
Height, compared with its all band, damages small to human body, seeks to have near infrared region the material of good optical characteristic to be used for biomedicine
Field is always the ideal chose of people.Molybdenum disulfide etc. has laminar structured transition metal dichalcogenide, with excellent
Physicochemical properties, obtain the extensive concern of people in recent years.Molybdenum disulfide nano sheet not only can be big using specific surface area
Feature loads specific medicine or photosensitive molecular, and has obvious photothermal conversion ability near infrared region, in biomedicine
Good application prospect is shown in terms of photo-thermal therapy.
Gold nano star because it is unique, adjustable surface plasma body resonant vibration characteristic and synthetic method are simple, chemically
The advantages of matter is stable, yield is high, makes its application in terms of biomedical and medical diagnosis on disease and treatment also more and more extensively, this
Outer gold nano star, which absorbs near infrared light, can produce heating behavior, and this has special superiority in the photo-thermal therapy of disease.
Such as document Adv. Mater., 2014,26 (21):The molybdenum disulfide reported in 3433-3440 has in itself
Good light thermal property, the molybdenum disulfide modified with PEG can realize high drug load and targeting, pass through photo-thermal controlled release medicine
Thing.But the near infrared absorption of molybdenum disulfide in itself is far below gold nano star/molybdenum disulfide composite.
Chinese patent CN104525938A reports a kind of molybdenum disulfide/gold nanorods composite, preparation method and use
On the way, disclose one kind and rely on electrostatic interaction, will be combined in electronegative molybdenum disulfide nano sheet and in electropositive gold nanorods,
Obtain molybdenum disulfide/gold nanorods composite.Show that gold nanorods/molybdenum disulfide has preferable light thermal property, but both
With reference to being method by self assembly, experimental technique is complicated, and density is uncontrollable.We enrich exposed by molybdenum disulfide surface
Sulphur atom and the golden amount for forming stable Au-S keys, gold chloride being added by control, regulate and control the close of molybdenum disulfide surface gold grain
Degree, and then control the density of gold nano star.
Therefore, it is excellent with reference to both using the controllable gold nano star/molybdenum disulfide composite of in situ synthesis integral density
Gesture, plays its common strong point, while bigger drugloading rate is realized, obtains the more excellent composite of photo-thermal effect, is
This area needs the problem solved.
The content of the invention
It is an object of the present invention to provide that a kind of density is controllable by situ synthesis, drugloading rate bigger, photo-thermal effect more
Plus the preparation method of excellent gold nano star/molybdenum disulfide composite, and enable to the composite preferably to apply
In photo-thermal therapy field.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of gold nano star/molybdenum disulfide composite, methods described is：By molybdenum disulfide seed solution
With chlorauric acid solution mixing, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification.
Wherein molybdenum disulfide seed solution is made by following methods：
（1）Mass concentration is the mg/mL molybdenum disulfide solution of 0.01 mg/mL ~ 0.08 and mass fraction is 1% ~ 10%
Aqueous povidone solution is stirred and evenly mixed, and adds the aqueous solution of chloraurate that molar concentration is 1mM ~ 100mM；
（2）By step（1）5 ~ 20min of reaction, 50 DEG C ~ 100 under the conditions of the mixed solution of acquisition is successively placed in 20 DEG C ~ 30 DEG C
5 ~ 10 min are reacted under the conditions of DEG C, reaction solution centrifugation abandons supernatant, product is distributed in water.
Preferably, the molybdenum disulfide seed solution is made by following methods：
（1）By aqueous povidone solution that mass fraction is 1% ~ 10% and mass concentration be 0.01 mg/mL ~
0.08 mg/mL molybdenum disulfide solution by volume 1:4~1:40 mixing, stir；
（2）5 ~ 20min is reacted under the conditions of 20 ~ 30 DEG C, while stirring to step（1）Solution in molar concentration is added dropwise
For 1mM ~ 100mM chlorauric acid solution, 5 ~ 10 min are reacted after completion of dropwise addition under the conditions of 50 DEG C ~ 100 DEG C；
（3）Solution becomes claret from grey black, and reaction terminates, using centrifugation method of purification concentration step（2）What is obtained is molten
Liquid, centrifugation product is distributed in ultra-pure water.
Wherein, molybdenum disulfide seed solution and chlorauric acid solution growth in situ process are as follows：
（1）Sequentially added in being the mg/mL molybdenum disulfide seed solutions of 0.01 mg/mL ~ 0.08 to mass concentration mole dense
The ascorbic acid of the hydrochloric acid and 100mM for 1M is spent, is stirred；
（2）To step（1）The silver nitrate solution and 10mM gold chlorides that molar concentration is 1mM are added in the solution of acquisition simultaneously
Solution, after reaction terminates, centrifugation purification.
Preferably, the molybdenum disulfide seed solution and chlorauric acid solution growth in situ process are as follows：
（1）By volume 1:10~1:Mass concentration is that 0.01 mg/mL ~ 0.08 mg/mL molybdenum disulfide seeds are molten by 100
Liquid is dispersed in ultra-pure water, is stirred and evenly mixed；
（2）In step（1）It is 1M hydrochloric acid and resisting for 100mM that molar concentration is sequentially added in the mixed colloidal solution of acquisition
The volume ratio of bad hematic acid, hydrochloric acid and ascorbic acid is 1:10~1:40, it is uniformly mixed；
（3）To step（2）The silver nitrate solution and 10mM gold chlorides that molar concentration is 1mM are added in the solution of acquisition simultaneously
The volume ratio of solution, silver nitrate and gold chloride is 6:1~1:3, centrifugation is purified twice after reaction terminates.
A kind of application of gold nano star/molybdenum disulfide composite, the photothermal conversion that the material has near infrared region is imitated
Should, available for photo-thermal therapy.
The present invention utilizes seed mediated growth method, first prepares homogeneous, highdensity molybdenum disulfide seed solution, then make with gold chloride
For gold salt, ascorbic acid is as reducing agent, and silver nitrate is quick to prepare gold nano star/molybdenum disulfide composite as derivant.
The present invention characterizes the shape of the gold nano star/molybdenum disulfide composite prepared using transmission electron microscope
Looks, uv-visible absorption spectra characterizes material surface plasma resonance characteristic.
Beneficial effect
The preparation method and applications of gold nano star/molybdenum disulfide composite of the present invention have advantages below：
（1）The composite prepared using the method for the invention has how dendritic star pattern and homogeneous chi
It is very little；Soilless sticking between particle, with good dispersiveness and biocompatibility, and in molybdenum disulfide lamellar structure, gold nano
The load density of star is larger；
（2）The uv-visible absorption spectra peak value of the composite is between 600-1000nm, in near-infrared laser irradiation
Lower temperature is raised rapidly, thus with preferable photothermal conversion performance, is had in terms of the tumor thermal therapy of biomedical sector
There is huge application potential；
（3）The preparation process technique of the gold nano star/molybdenum disulfide composite is simple to operation, and equipment requirement is low；System
The impurity content of standby obtained composite is few, and yield is high.
Brief description of the drawings
Fig. 1 is the obtained gold nano star/molybdenum disulfide composite under the conditions of gold chloride amount is 125 μ L of embodiment 3
TEM schemes；
Fig. 2 is the TEM figures for the molybdenum disulfide seed that embodiment 1 is prepared；Wherein, figure a is two under the μ L of gold chloride amount 50
The TEM figures of molybdenum sulfide seed；Scheme the TEM figures that b is molybdenum disulfide seed under the μ L of gold chloride amount 110；Figure c is the μ L of gold chloride amount 150
The TEM figures of lower molybdenum disulfide seed；Scheme the TEM figures that d is molybdenum disulfide seed under the μ L of gold chloride amount 200；
Fig. 3 is gold nano star/molybdenum disulfide composite that embodiment 2 is made under the conditions of the different usage amounts of silver nitrate
TEM figure；Wherein, figure a is the TEM figures for the gold nano star/molybdenum disulfide composite being made under the conditions of the μ L of silver nitrate 50；Figure
B is the TEM figures of obtained gold nano star/molybdenum disulfide composite under the conditions of the μ L of silver nitrate 100；Figure c is the μ L bars of silver nitrate 200
The TEM figures of obtained gold nano star/molybdenum disulfide composite under part；It is obtained gold nano under the conditions of the μ L of silver nitrate 300 to scheme d
The TEM figures of star/molybdenum disulfide composite；
Fig. 4 is the obtained gold nano star/molybdenum disulfide composite under the conditions of gold chloride amount is 125 μ L of embodiment 3
UV-visible absorption spectrum；
Fig. 5 is that the obtained gold nano star/molybdenum disulfide composite under the conditions of gold chloride amount is 125 μ L of embodiment 3 exists
Temperature variation curve under 0.577W/cm2 785nm near-infrared lasers irradiation.
Embodiment
The present invention is described in further detail with reference to embodiments：
Embodiment 1 prepares molybdenum disulfide seed solution
（1）It is 0.025 mg/mL that the polyvinylpyrrolidone for being 5% by 400 μ L mass fractions, which is added to 4mL mass concentrations,
In molybdenum disulfide solution, stir and evenly mix；Four groups of molybdenum disulfide solution for standby, respectively A, B, C, D are prepared by same composition proportioning；
（2）With vigorous stirring, the μ L of volume 50,110 μ L, 150 μ L, 200 μ L 10mM chlorauric acid solution are taken, dropwise
It is added separately to step（1）In four groups of mixed colloidal solutions of middle preparation, stirring at normal temperature 10min reacts under the conditions of 60 DEG C
5min；
（3）Step（2）After reaction terminates, above-mentioned four groups of molybdenum disulfide seed solutions are concentrated using centrifugation method of purification, wherein
Centrifugation purification parameter is 6000 rpm, 10min, and the molybdenum disulfide seeded dispersion finally given is settled to 1mL, 4 in ultra-pure water
DEG C storage.
The pattern for four groups of molybdenum disulfide seeds that the present embodiment is prepared is characterized by transmission electron microscope, as a result such as
Shown in Fig. 2.From TEM figure results, four groups of molybdenum disulfide seed material uniform particle diameters that the present embodiment is prepared, distribution are equal
It is even.The molybdenum disulfide seed solution that embodiment 1 is prepared is used in embodiment 2 and embodiment 3 prepare gold nano star/curing
The raw material of molybdenum composite material.
The in situ synthesis of embodiment 2 prepares gold nano star/molybdenum disulfide composite
The molybdenum disulfide seed solution prepared when the amount of gold chloride is 110 μ L in Example 1, prepares gold nano star/bis-
Vulcanize molybdenum composite material：
（1）By 100 μ L molybdenum disulfide seed solutions, in the ultra-pure water for adding 5 mL, stir and evenly mix；
（2）5 μ L 1M hydrochloric acid and 50 μ L 100mM ascorbic acid are taken to be added separately to step successively（1）The epoxy glue of preparation
In liquid solution, stir and evenly mix, four groups, respectively E, F, G, H are prepared by same composition proportioning；
（3）While being stirred vigorously, the μ L of volume 50,100 μ L, 200 μ L, 300 μ L 1mM silver nitrate solutiones and 125 μ are taken
L 10mM chlorauric acid solutions are added separately to step simultaneously（2）In in obtained four groups of mixed solutions, reaction 30s is completed；
（4）Step（3）After reaction terminates, using centrifugation method of purification concentration step（3）The four groups of solution obtained, centrifugation purification
Parameter is 4000 rpm, 10min, and centrifugation is purified three times, and the gold nano star/molybdenum disulfide composite finally given is scattered in super
In pure water.
The shape for gold nano star/molybdenum disulfide composite that the present embodiment is prepared is characterized by transmission electron microscope
Looks, as a result as shown in figure 3, from TEM figure results：Gold nano star/molybdenum disulfide composite that the present embodiment is prepared
The load density of gold nano star is larger.
The in situ synthesis of embodiment 3 prepares gold nano star/molybdenum disulfide composite
Under conditions of silver nitrate amount is 200 μ L in Example 2, under different gold chloride concentration, gold nano star looks are adjustable
Gold nano star/molybdenum disulfide composite preparation method it is as follows：
（1）By 100 μ L gold seeds solution, in the ultra-pure water for adding 5 mL, stir and evenly mix；
（2）5 μ L 1M hydrochloric acid and 50 μ L 100mM ascorbic acid are taken to be added separately to step successively（1）The epoxy glue of preparation
In liquid solution, stir and evenly mix, four groups, respectively Q, R, S, T are prepared by same composition proportioning；
（3）While being stirred vigorously, it is 50 μ L, 75 μ L, 100 μ L, 125 μ to take 200 μ L 1mM silver nitrate solutiones and volume
L 10mM chlorauric acid solutions are added separately to step simultaneously（2）In in obtained four groups of mixed solutions, reaction 30s is completed；
（4）Step（3）After reaction terminates, using centrifugation method of purification concentration step（3）The four groups of solution obtained, centrifugation purification
Parameter is 4000 rpm, 10min, and centrifugation is purified three times, and the gold nano star/molybdenum disulfide composite finally given is scattered in super
In pure water.
Group T gold nanos star/molybdenum disulfide composite that the present embodiment is prepared is characterized by transmission electron microscope
Pattern, as a result as shown in Figure 1；Material surface plasma resonance characteristic is characterized by uv-visible absorption spectra, as a result such as
Shown in Fig. 4；And material is investigated in 0.577W/cm2785nm near-infrared lasers irradiation under temperature change, as a result such as Fig. 5 institutes
Show.The result shown from above-mentioned figure, gold nano star/molybdenum disulfide composite that the present embodiment is prepared has good
Good dispersiveness and biocompatibility, and in molybdenum disulfide lamellar structure, the load density of gold nano star is larger；Its is ultraviolet-
Visible absorption spectra peak value is between 600-1000nm, and temperature is raised rapidly under near-infrared laser irradiation, thus with preferable
Photothermal conversion performance.
Claims (5)
1. a kind of preparation method of gold nano star/molybdenum disulfide composite, it is characterised in that methods described is：By curing
Molybdenum seed solution and chlorauric acid solution mixing, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification；It is described
Molybdenum disulfide seed solution is made by following methods：（1）It is that 0.01 mg/mL ~ 0.08 mg/mL molybdenum disulfide is molten by mass concentration
Liquid and mass fraction stir and evenly mix for 1% ~ 10% aqueous povidone solution, and it is 1mM ~ 100mM's to add molar concentration
Aqueous solution of chloraurate；（2）By step（1）5 ~ 20min of reaction, 50 under the conditions of the mixed solution of acquisition is successively placed in 20 DEG C ~ 30 DEG C
DEG C ~ 100 DEG C under the conditions of react 5 ~ 10 min, reaction solution centrifugation abandon supernatant, product is distributed in water.
2. a kind of preparation method of gold nano star/molybdenum disulfide composite, it is characterised in that methods described is：By curing
Molybdenum seed solution and chlorauric acid solution mixing, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification；It is described
Molybdenum disulfide seed solution is made by following methods：（1）By mass fraction for 1% ~ 10% aqueous povidone solution with
Mass concentration is the mg/mL molybdenum disulfide solution of 0.01 mg/mL ~ 0.08 by volume 1:4~1:40 mixing, stir；（2）
5 ~ 20min is reacted under the conditions of 20 ~ 30 DEG C, while stirring to step（1）Solution in molar concentration is added dropwise for 1mM ~ 100mM
Chlorauric acid solution, after completion of dropwise addition under the conditions of 50 DEG C ~ 100 DEG C react 5 ~ 10 min；（3）It is red that solution becomes wine from grey black
Color, reaction terminates, using centrifugation method of purification concentration step（2）The solution of acquisition, centrifugation product is distributed in ultra-pure water.
3. a kind of preparation method of gold nano star/molybdenum disulfide composite, it is characterised in that methods described is：By curing
Molybdenum seed solution and chlorauric acid solution mixing, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification；It is described
Molybdenum disulfide seed solution and chlorauric acid solution growth in situ process are as follows：（1）It is 0.01 mg/mL ~ 0.08 to mass concentration
It is 1M hydrochloric acid and 100mM ascorbic acid that molar concentration is sequentially added in mg/mL molybdenum disulfide seed solutions, is stirred；
（2）To step（1）The silver nitrate solution and 10mM chlorauric acid solutions that molar concentration is 1mM are added in the solution of acquisition simultaneously, instead
After should terminating, centrifugation purification.
4. a kind of preparation method of gold nano star/molybdenum disulfide composite, it is characterised in that methods described is：By curing
Molybdenum seed solution and chlorauric acid solution mixing, gold nano star/molybdenum disulfide composite is obtained through growth in situ, purification；It is described
Molybdenum disulfide seed solution and chlorauric acid solution growth in situ process are as follows：（1）By volume 1:10~1:100 by mass concentration
It is dispersed in ultra-pure water, stirs and evenly mixs for the mg/mL molybdenum disulfide seed solutions of 0.01 mg/mL ~ 0.08；（2）In step（1）Obtain
Mixed colloidal solution in sequentially add hydrochloric acid that molar concentration is 1M and 100mM ascorbic acid, hydrochloric acid and ascorbic acid
Volume ratio be 1:10~1:40, it is uniformly mixed；（3）To step（2）Adding molar concentration in the solution of acquisition simultaneously is
The volume ratio of 1mM silver nitrate solution and 10mM chlorauric acid solutions, silver nitrate and gold chloride is 6:1~1:3, reaction terminate after from
The heart is purified twice.
5. any described gold nano star/molybdenum disulfide composite of Claims 1 to 4 is being used as tumor thermal therapy material
Application in raw material.
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