CN105537618B - One kind prepares mesoporous Au@SiO2The method of compound particle - Google Patents
One kind prepares mesoporous Au@SiO2The method of compound particle Download PDFInfo
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- CN105537618B CN105537618B CN201511008972.6A CN201511008972A CN105537618B CN 105537618 B CN105537618 B CN 105537618B CN 201511008972 A CN201511008972 A CN 201511008972A CN 105537618 B CN105537618 B CN 105537618B
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- 239000002245 particle Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 30
- 150000001875 compounds Chemical class 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 31
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 31
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 31
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 31
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 27
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229960001231 choline Drugs 0.000 claims abstract description 20
- 229910004042 HAuCl4 Inorganic materials 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- 239000003381 stabilizer Substances 0.000 claims abstract description 3
- 239000010931 gold Substances 0.000 claims description 49
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 claims description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims 2
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims 1
- 230000006911 nucleation Effects 0.000 abstract description 9
- 238000010899 nucleation Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000009738 saturating Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical compound C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 2
- OFLYIWITHZJFLS-UHFFFAOYSA-N [Si].[Au] Chemical compound [Si].[Au] OFLYIWITHZJFLS-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000004557 single molecule detection Methods 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 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 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- 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
-
- B22F1/0007—
Abstract
One kind of the invention prepares mesoporous Au@SiO2The method of compound particle belongs to the technical field of nano material preparation, first in alcohol-water system, using CTAB as golden core stabilizer and the template of shell meso-hole structure, using choline as reducing agent, reduces HAuCl4Prepare golden core；In golden karyomorphism into rear addition TEOS, TEOS is catalyzed by the choline in reaction system, hydrolysis, in golden core surface deposition growing SiO2, it is purified after obtain mesoporous Au@SiO2Compound particle.The present invention is only measured and the nucleation reaction time by regulating and controlling alcohol/water volume ratio, CTAB, so that it may prepare the Au@SiO with different covered effects, mesopore size and shell thickness2Compound particle, easy to operate, regulating effect is good.
Description
Technical field
The invention belongs to technical field prepared by nano material, and in particular to a kind of golden as chlorine using bifunctional molecule choline
Acid (HAuCl4) reducing agent and tetraethyl orthosilicate (TEOS) catalyst, by regulate and control alcohol/water volume ratio, CTAB measure and into
The variables such as nuclear reaction time, one kettle way prepares the Au@SiO with different covered effects, mesopore size and shell thickness2Compound grain
The new method of son.
Technical background
Mesoporous Au@SiO2Compound particle, due to the dual-use function with core, shell unlike material, and stablizes the excellent of gold particle
Gesture, makes it be with a wide range of applications in many fields, and such as catalysis, medicine are transmitted, adsorbed and based on local plasmon resonance
Bio-sensing, the Single Molecule Detection in field etc..Traditional Au@SiO2Compound particle preparation method, mainly two steps or multistep
Method, reduces gold chloride and prepares golden core (mainly in water phase by sodium citrate, sodium borohydride or other go back original reagents first
In), then by golden core after purification, under appropriate ligand reagent stabilization, golden consideration convey is moved on into SiO2Reaction system in (mainly exist
In alcohol phase), through base catalyst hydrolysis, condensation silicon source, finally prepare mesoporous Au@SiO2Compound particle.Such method is often
It is time-consuming, laborious, the gold particle synthesized in water phase is being transferred to the SiO of alcohol phase in addition2When in reaction system, it is easy to go out cash
The phenomenon such as particle buildup and spontaneous nucleation.To overcome these problems, particularly time-consuming, laborious problem, some Research teams start to taste
Pilot production takes one kettle way and prepares mesoporous Au@SiO2Compound particle.Such as, Zhao groups, using formaldehyde as reducing agent, CTAB is used as gold
Particle-stabilised dose and SiO2The pore creating material of shell, then with sodium hydroxide catalyzed, hydrolysis TEOS, final one kettle way is prepared with Jie
The Au@SiO of pore structure2Compound particle.But, the method uses formaldehyde as reducing agent, and reaction condition is not friendly enough, controllable change
Amount is also less, and product structure is more single, and shell thickness is not shown in change yet；For another example He groups, using sodium borohydride as reducing agent also
Former gold chloride prepares small gold particle, then with polyacrylic acid as gold particle capturing agent and kernel template, afterwards, by ammoniacal liquor
Catalysis, hydrolysis TEOS are coated, and finally after kernel template is removed, obtain mesoporous Au@SiO2Compound particle.Although these sides
Method employs one kettle way and prepares mesoporous Au@SiO2Compound particle, but process not enough simplify, at least need two kinds of masters simultaneously
Want reagent, i.e. HAuCl4Reducing agent and TEOS catalyst.Additionally, the structure change of compound particle is also more single, controllable change
Amount is less, particularly mesoporous lamella thickness, often in one kettle way, it is more difficult to realize effective change.And have the shell thickness can
The mesoporous Au@SiO for adjusting2Compound particle, in the neck such as catalysis and bio-sensing, Single Molecule Detection based on local plasmon resonance
Domain, is more of practical significance.
The content of the invention
The technical problem to be solved in the present invention is the problem for overcoming background technology to exist, using one kettle way, only by regulation and control
The variables such as alcohol/water volume ratio, CTAB amounts and nucleation reaction time, prepare with different covered effects, mesopore size and difference
The mesoporous Au@SiO of shell thickness2The method of compound particle.
Specific technical scheme is as follows：
One kind prepares mesoporous Au@SiO2The method of compound particle, first in alcohol-water system, with cetyl trimethyl bromine
Change ammonium (CTAB) as golden core stabilizer and the template of shell meso-hole structure, using choline as reducing agent, reduce HAuCl4
Prepare golden core；In golden karyomorphism into rear addition tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate is by the choline in reaction system
Catalysis, hydrolysis, in golden core surface deposition growing SiO2, it is purified after obtain mesoporous Au@SiO2Compound particle.
One kind of the invention prepares mesoporous Au@SiO2The method of compound particle, preferred Loading sequence is：Water, ethanol, courage
Alkali, cetyl trimethylammonium bromide (CTAB), gold chloride (HAuCl4), it is eventually adding tetraethyl orthosilicate (TEOS).
One kind of the invention prepares mesoporous Au@SiO2The method of compound particle, prepares the process and deposition growing SiO of golden core2
During, preferably 80 DEG C of reaction temperature.
One kind of the invention prepares mesoporous Au@SiO2In the method for compound particle, in whole reaction system, alcohol water volume
Than preferably 1：15~3：13, concentration of the choline in whole reaction system preferably 4.17 × 10-4G/mL, cetyl trimethyl bromine
Change concentration preferably 1.0 × 10 of the ammonium in whole reaction system-3~1.9 × 10-3G/mL, gold chloride is in whole reaction system
The preferred 0.339mM of concentration, concentration of the tetraethyl orthosilicate in whole reaction system preferably 1.9 × 10-3g/mL。
One kind of the invention prepares mesoporous Au@SiO2The method of compound particle, described purification can be entered by following processes
OK：The product for obtaining will be reacted carries out twice process of " centrifugation, washing ", and 120 DEG C of drying are calcined 5 hours for 550 DEG C afterwards
Remove impurity.
One kind of the invention prepares mesoporous Au@SiO2The method of compound particle, more specifically step are：First, in alcohol water
It is choline (Choline) aqueous solution of 0.01g/mL that mass concentration is added in system, adds cetyl trimethylammonium bromide
(CTAB), that the temperature of reaction system is constant to after 80 DEG C, it is the HAuCl of 8.14mM to add molar concentration4The aqueous solution, after mixing
System in the relation of amount of each reactant be：The volume ratio of alcohol water is 1：15~3：13, the concentration of choline is 4.17 × 10-4g/
The concentration of mL, CTAB is 1.0 × 10-3~1.9 × 10-3G/mL, HAuCl4Concentration is 0.339mM, and whole reaction system is at 80 DEG C
After reaction 4~15 minutes, TEOS is added, the consumption of TEOS is：The concentration of TEOS is 1.9 × 10 in system after adding TEOS- 3G/mL, continues in 80 DEG C of stirring reactions 0.5 hour, and will react the product for obtaining carries out twice mistake of " centrifugation, washing "
Journey, 120 DEG C of drying, then 550 DEG C of calcinings remove impurity, the mesoporous Au SiO for being purified in 5 hours2Compound particle.
In the present invention, by the alcohol water ratio in regulation system, the mesoporous Au SiO with different covered effects can be obtained2
Compound particle, when volume ratio of alcohol to water from 1：15 are increased to 3：When 13, covered effect coats gradually transition for multinuclear is coated from monokaryon；
The reaction time of golden core is prepared by changing, the shell thickness of product can be changed, nucleation time is more long, the shell of final product is thick
Degree it is smaller, when nucleation time from increase to 15 minutes within 4 minutes when, the shell thickness of final product falls below 10nm from 35nm；It is logical
The consumption of CTAB is overregulated, mesopore size can be changed, CTAB consumptions are more, and the meso-hole structure of shell is also more clear.
Beneficial effect：
Because the method for the present invention is only with a kind of reagent (i.e. choline), while reduction gold chloride and catalysis TEOS works can be played
With additionally, whole course of reaction is completed all in one pot, 80 DEG C of heating complete golden core and prepare and follow-up SiO2The cladding of shell,
Only measured and the nucleation reaction time by regulating and controlling alcohol/water volume ratio, CTAB, so that it may prepare with different covered effects, mesoporous chi
Very little and shell thickness Au@SiO2Compound particle.Therefore, this prepares mesoporous Au@SiO2The method of compound particle is more simple and effective,
Control measures and regulating effect are also more preferable.
Brief description of the drawings
Fig. 1 compares 1 for the embodiment of the present invention 1 by alcohol water：The Au@SiO that 15 condition is obtained2The transmitted electron of compound particle shows
Micro mirror (TEM) image.
Fig. 2 compares 2 for the embodiment of the present invention 1 by alcohol water：The Au@SiO that 14 condition is obtained2The transmitted electron of compound particle shows
Micro mirror (TEM) image.
Fig. 3 compares 3 for the embodiment of the present invention 1 by alcohol water：The Au@SiO that 13 condition is obtained2The transmitted electron of compound particle shows
Micro mirror (TEM) image.
Fig. 4 is the Au@SiO that the embodiment of the present invention 2 is obtained when the consumption of CTAB is 0.05g2The transmission electricity of compound particle
Sub- microscope (TEM) image.
Fig. 5 is the Au@SiO that the embodiment of the present invention 2 is obtained when the consumption of CTAB is 0.07g2The transmission electricity of compound particle
Sub- microscope (TEM) image.
Fig. 6 is the Au@SiO that the embodiment of the present invention 2 is obtained when the consumption of CTAB is 0.09g2The transmission electricity of compound particle
Sub- microscope (TEM) image.
Fig. 7 is the Au@SiO obtained under conditions of the embodiment of the present invention 3 is 4 minutes in the nucleation reaction time2Compound particle
Saturating electron microscope (TEM) image.
Fig. 8 is the Au@SiO obtained under conditions of the embodiment of the present invention 3 is 8 minutes in the nucleation reaction time2Compound particle
Saturating electron microscope (TEM) image.
Fig. 9 is the Au@SiO obtained under conditions of the embodiment of the present invention 3 is 15 minutes in the nucleation reaction time2Compound particle
Saturating electron microscope (TEM) image.
Specific embodiment
The following is the basic condition that embodiments of the invention are used, but the scope that the present invention can be implemented is not limited to these
Part, is also not necessarily limited to these embodiments：
25 DEG C of environment temperature, 1 atmospheric pressure；
Ethanol, density 0.79g/mL, molecular weight 46g/mol；
Water, density 1g/mL, molecular weight 18g/mol；
Choline, density 1.06g/mL, mass fraction 48~50%, molecular weight 121.25g/mol；
Cetyl trimethylammonium bromide (CTAB), molecular weight 364.45g/mol；
Gold chloride (HAuCl4), molar concentration 8.14mM；
TEOS, density 0.931g/mL, molecular weight 208.33g/mol.
Embodiment 1：The preparation of the silicon gold filled core-shell nano of different covered effects
First, 41mL, 38mL and 35mL water are first separately added into three three-necked bottles, then are separately added into 3mL, 6mL and 9mL
Ethanol；Afterwards, the aqueous choline base solution that 2mL mass concentrations are 0.01g/mL is separately added into three systems, 0.05g is added
CTAB, control temperature is constant to after 80 DEG C, adds 2mL 8.14mM HAuCl4The aqueous solution, is configured to water, ethanol volume ratio difference
For：15:1、14:2 and 13:3 three reaction systems；4~5min is reacted at 80 DEG C, then is separately added into 0.1mL TEOS
(0.45mmol), continues under 80 DEG C of steady temperatures, stirring reaction 0.5h.Twice of centrifugation, washing after three system reactions, first
120 DEG C of drying, afterwards 550 DEG C of calcinings remove impurity in 5 hours, obtain the mesoporous Au SiO with different covered effects2Compound grain
Son, transition is coated for multinuclear is coated from monokaryon, sees Fig. 1~3.
Embodiment 2：The preparation of the silicon gold filled core-shell nano of different mesopore sizes
First, first distinguish in three three-necked bottles and all add 41mL water and 3mL ethanol；Afterwards, it is separately added into 2mL mass dense
The aqueous choline base solution for 1% is spent, then is separately added into 0.05g, 0.07g and 0.09g CTAB, controlling reaction temperature is constant to 80 DEG C
Afterwards, 2mL 8.14mM HAuCl are added4The aqueous solution, it is 15 to be made into water, ethanol volume ratio:1, but CTAB contents different three are anti-
Answer system；After three reaction systems react 4~5min at 80 DEG C, then 0.1mL TEOS (0.45mmol) are separately added into, continued
Under 80 DEG C of steady temperatures, stirring reaction 0.5h.Twice of centrifugation, washing, first 120 DEG C of drying, afterwards 550 DEG C after three sample synthesis
Calcining removes impurity in 5 hours, obtains the Au SiO with different mesopore sizes2Compound particle, CTAB measures higher, the mesoporous knot of shell
Structure is more clear, sees Fig. 4~6.
Embodiment 3：The mesoporous Au@SiO of different shell thicknesses2The preparation of compound particle
First, first distinguish in three three-necked bottles and all add 41mL water and 3mL ethanol；Afterwards, it is separately added into 2mL mass dense
The aqueous choline base solution for 1% is spent, then is separately added into 0.07g CTAB, control reaction is constant to after 80 DEG C, is separately added into 2mL
8.14mM HAuCl4The aqueous solution, it is 15 to be made into water, ethanol volume ratio:1 reaction system；Three individualities tie up to 80 DEG C and react respectively
After 4min, 8min and 15min, 0.1mL TEOS (0.45mmol) is added, continued under 80 DEG C of steady temperatures, stirring reaction
0.5h.Twice of centrifugation, washing after sample synthesis, afterwards 550 DEG C of calcinings remove impurity in 5 hours, and respectively obtaining shell thickness is
The mesoporous Au@SiO of 35nm, 23nm, 10nm2Compound particle, such as Fig. 7~9.
Claims (6)
1. one kind prepares mesoporous Au@SiO2The method of compound particle, first in alcohol-water system, with cetyl trimethyl bromination
Ammonium, using choline as reducing agent, reduces HAuCl as golden core stabilizer and the template of shell meso-hole structure4Prepare gold
Core；In golden karyomorphism into rear addition tetraethyl orthosilicate, tetraethyl orthosilicate is catalyzed by the choline in reaction system, hydrolysis, in gold
Core surface deposition growing SiO2, it is purified after obtain mesoporous Au@SiO2Compound particle.
2. one kind according to claim 1 prepares mesoporous Au@SiO2The method of compound particle, it is characterised in that Loading sequence
For：Water, ethanol, choline, cetyl trimethylammonium bromide, gold chloride, are eventually adding tetraethyl orthosilicate.
3. one kind according to claim 1 prepares mesoporous Au@SiO2The method of compound particle, it is characterised in that prepare golden core
Process and deposition growing SiO2During, reaction temperature is 80 DEG C.
4. one kind according to claim 1 prepares mesoporous Au@SiO2The method of compound particle, it is characterised in that preparing gold
In the reaction of core, after all reactants all mix, the relation with contents of each reactant is in system：Volume ratio of alcohol to water is 1:15~
3:13, the concentration of choline is 4.17 × 10-4G/mL, the concentration of cetyl trimethylammonium bromide is 1.0 × 10-3~1.9 × 10-3G/mL, the concentration of gold chloride is 0.339mM；In golden core surface deposition growing SiO2Reaction in, add tetraethyl orthosilicate
Afterwards, concentration of the tetraethyl orthosilicate in system is 1.9 × 10-3g/mL。
5. one kind according to claim 1 prepares mesoporous Au@SiO2The method of compound particle, it is characterised in that described carries
It is pure to concretely comprise the following steps：The product that obtains will be reacted carries out twice process of " centrifugation, washing ", and 120 DEG C dry, and afterwards 550
DEG C calcining 5 hours remove impurity.
6. mesoporous Au@SiO are prepared according to any described one kind of Claims 1 to 52The method of compound particle, it is characterised in that
Specific step is：First, it is the aqueous choline base solution of 0.01g/mL mass concentration to be added in alcohol-water system, adds hexadecane
Base trimethylammonium bromide, the temperature of reaction system is constant to after 80 DEG C, and it is the HAuCl of 8.14mM to add molar concentration4It is water-soluble
Liquid, the relation of the amount of each reactant is in mixed system：The volume ratio of alcohol water is 1：15~3：13, the concentration of choline is
4.17×10-4G/mL, the concentration of cetyl trimethylammonium bromide is 1.0 × 10-3~1.9 × 10-3G/mL, HAuCl4Concentration
It is 0.339mM, after whole reaction system is reacted 4~15 minutes at 80 DEG C, adds tetraethyl orthosilicate, the use of tetraethyl orthosilicate
Measure and be：The concentration of tetraethyl orthosilicate is 1.9 × 10 in system after adding tetraethyl orthosilicate-3G/mL, continuation is stirred at 80 DEG C
Reaction 0.5 hour is mixed, will react the product for obtaining carries out twice process of " centrifugation, washing ", and 120 DEG C dry, then 550 DEG C
Calcining removes impurity, the mesoporous Au SiO for being purified in 5 hours2Compound particle.
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