CN1994625A - Nano Au particle evenly coated carbon nanotube compound in-situ solution preparation method - Google Patents
Nano Au particle evenly coated carbon nanotube compound in-situ solution preparation method Download PDFInfo
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- CN1994625A CN1994625A CN 200610155580 CN200610155580A CN1994625A CN 1994625 A CN1994625 A CN 1994625A CN 200610155580 CN200610155580 CN 200610155580 CN 200610155580 A CN200610155580 A CN 200610155580A CN 1994625 A CN1994625 A CN 1994625A
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- 239000002245 particle Substances 0.000 title claims abstract description 46
- 239000002041 carbon nanotube Substances 0.000 title claims description 28
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims description 28
- -1 carbon nanotube compound Chemical class 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title claims description 15
- 238000011065 in-situ storage Methods 0.000 title claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 9
- 125000003118 aryl group Chemical group 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- KJOLVZJFMDVPGB-UHFFFAOYSA-N perylenediimide Chemical compound C=12C3=CC=C(C(NC4=O)=O)C2=C4C=CC=1C1=CC=C2C(=O)NC(=O)C4=CC=C3C1=C42 KJOLVZJFMDVPGB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000010931 gold Substances 0.000 abstract description 38
- 238000000034 method Methods 0.000 abstract description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 3
- 229910052737 gold Inorganic materials 0.000 abstract 3
- 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 abstract 2
- 239000012190 activator Substances 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 19
- 229920000642 polymer Polymers 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 238000005289 physical deposition Methods 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 description 1
- TYAMCPIKMIGMQC-UHFFFAOYSA-N 2-perylen-1-ylethanethiol Chemical group SCCC1=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45 TYAMCPIKMIGMQC-UHFFFAOYSA-N 0.000 description 1
- RMMXTBMQSGEXHJ-UHFFFAOYSA-N Aminophenazone Chemical compound O=C1C(N(C)C)=C(C)N(C)N1C1=CC=CC=C1 RMMXTBMQSGEXHJ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229910000071 diazene Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000013047 polymeric layer Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 229940113124 polysorbate 60 Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
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Abstract
The invention relates to an original solution prepare method of carbon nanometer tube composite uniformly packed by nanometer gold particles at high density, wherein said method comprises that: dispersing the carbon nanometer tube treated by mixed acid into the water solution with surface activator, to react with chlorauric acid solution, to obtain the nanometer composite NH2 packed by nanometer gold particles at high density; or, dispersing the carbon nanometer tube treated by mixed acid into water, adding organic molecule with aromatic ring and chlorauric acid solution, to obtain the nanometer composite NH3 uniformly packed by nanometer gold particles at high density, the inventive nanometer composite has better dissolve property and stability, with wide application.
Description
Technical field
The present invention relates to the in-situ solution preparation method of nano Au particle coated carbon nanotube compound, specifically, relate in solution made acid-stable in situ nano Au particle enveloped carbon nanometer tube compound process, add organic molecule with the formation that promotes nano Au particle coated carbon nanotube compound and make the compound of preparation in water and other various organic solvents, have dissolubility and stability preferably.
Background technology
Since CNT in 1991 since (Carbon Nanotubes) be found, because it has unique mechanical, electricity, optics, magnetic property and in every field, such as nano electron device, biology sensor, detector, afm tip, fortifying fibre etc., the potential application that exists causes the extensive concern of scientific circles and industrial quarters.Yet the chemical inertness of CNT itself has limited its application in every field.Therefore, adopting physics or chemical method that it is carried out modification is a kind of means that improve effectively and optimize its application.The more important thing is that CNT can be as constructing the basic material (Building Block) of other nano material.Nano composite material (Nano-Hybrid) based on CNT and metal nanoparticle, owing to have excellent catalytic activity, better electric conductivity, good fluorescent characteristic and a series of interesting and be different from the physical property of their intrinsics to the specific sensibility of hydrogen etc., be considered to a kind of in electricity, optics, catalysis, magnetics, senser element, the material that fields such as biological fluorescent labelling have wide application prospects.Various physics and chemical method are used as the compound for preparing CNT and metal nanoparticle such as physical deposition, heat deposition, electroless deposition, chemical modification, polymer support hydridization etc.Adopt aqueous process to prepare nano Au particle enveloped carbon nanometer tube compound though reported some at present, as adopt previously prepared nano Au particle and compound this compound that obtains of CNT, but the size that these methods can't the direct regulation and control nano Au particle, and preparation process is comparatively complicated; Also the handlebar polymer overmold is in carbon nano tube surface, interaction by polymer and nano Au particle forms this compound, but since make a little less than the interaction of polymer and CNT its coating effect inhomogeneous and polymer and nano Au particle active force a little less than, cause nano Au particle inhomogeneous and formed stable composite is relatively poor in the coating of carbon nano tube surface; On the other hand, thicker polymeric layer is potential to have limited electric charge and the energy transferance that exists between nano Au particle and the CNT, promptly may limit even lose distinctive optics of compound and electric property, has limited its range of application thus.Therefore, how to prepare the even coated carbon nanotube compound of nano Au particle and become one of focus of scientific worker's concern.
Summary of the invention
The invention provides the in-situ solution preparation method of the even coated carbon nanotube compound of a kind of nano Au particle, when pointing out the nano-complex of the even enveloped carbon nanometer tube of solution made acid-stable in situ nano Au particle, must add carboxyl itself that have organo-functional group such as grafting in organic molecule or the CNT, hydroxyl, amino, sulfydryl etc. and could form such compound.
The in-situ solution preparation method of the even coated carbon nanotube compound of a kind of nano Au particle may further comprise the steps:
1. CNT is added in the strong acid solution, under ultrasound condition, carry out purification process, obtain in water, having certain deliquescent carbon nano-tube solution;
2. surfactant is joined step 1. in the carbon nano-tube solution that obtains of purifying, ultrasonic dispersion adds the aqueous solution of chloraurate that concentration is 0.1～100m mol/l then, normal temperature stirred 1 minute～24 hours down, obtained carbon mano-tube composite; Described surfactant is sodium alkyl sulfonate or tween series of surfactants, is 100% in the quality of carbon nano-tube solution, and the consumption of surfactant is 0.01%-10%;
3. the 2. middle compound for preparing of step is come out with the supercentrifuge centrifugation.
2. the step of this preparation method also can be: the organic molecule that has aromatic ring is dissolved in the organic solvent, join step 1. in the carbon nano-tube solution that obtains of purifying, stir or ultrasonic a period of time; Add the aqueous solution of chloraurate that concentration is 0.1～100m mol/l then, normal temperature stirred 1 minute-24 hours down, obtained carbon mano-tube composite.The wherein said organic molecule that has aromatic ring is to contain sulfydryl to replace the De perylene diimide, contain the amino De of replacement perylene diimide, contain the pyrene that sulfydryl replaces or contain the organic molecule of band aromatic group such as the amino pyrene that replaces, and the consumption of organic molecule is 0.01～10mg/ml solvent.Described organic solvent is N, N '-dimethyl formamide, ethanol, methyl alcohol or water.
The present invention is raw material with the aqueous solution of chloraurate, adopts the even coated carbon nanotube compound of method in-situ preparing nano Au particle high density of solution, and the compound that makes has that the nano Au particle particle diameter is evenly distributed, characteristics such as reunion do not take place nano Au particle.The present invention implements under the aqueous solution and normal temperature, and preparation condition is extremely gentle, and the organic molecule that uses is as surfactant and aromatic ring molecule commonly used in the commerce, and is simply cheap; Can regulate the amount that adds gold chloride and CNT by selecting different organic molecules for use, prepare that particle diameter evenly distributes and the controlled nano Au particle and the nano-complex of the even enveloped carbon nanometer tube of nano Au particle high density; The more important thing is, compare with other method, as physical deposition and heat deposition etc., the cost of material that this method adopts is low, preparation process is simple, and can simply and effectively the nano-complex that makes be separated by methods such as centrifugations from the aqueous solution, conveniently is applied to each occasion.
Description of drawings
Fig. 1 a, Fig. 1 b, Fig. 1 c are the Electronic Speculum figure of nano Au particle enveloped carbon nanometer tube compound NH1.
Fig. 2 a, Fig. 2 b, Fig. 2 c are the Electronic Speculum figure of nano Au particle enveloped carbon nanometer tube compound NH2.
Fig. 3 a, Fig. 3 b, Fig. 3 c are the Electronic Speculum figure of nano Au particle enveloped carbon nanometer tube compound NH3.
Fig. 4 a, Fig. 4 b are sulfydryl Qu Dai perylene diimide molecules, the molecular structural formula figure of An base Qu Dai perylene diimide.
The specific embodiment
Comparative Examples 1:
1) to CNT purification process under the ultrasound condition in strong acid solution, the high-purity carbon nano tube that obtains in water, having certain dispersiveness;
2) directly be the aqueous solution of chloraurate adding 1 of 1m mol/l to concentration) in, normal temperature stirred 6 hours down, obtain nano Au particle enveloped carbon nanometer tube compound NH1, find out by Fig. 1, nano Au particle mainly is coated on the wall place and the defective locations of CNT, and it is not very even that nano particle diameter distributes.
Embodiment 1:
1) CNT is carried out ultrasonic purification process, the high-purity carbon nano tube that obtains having certain dispersiveness in water in strong acid solution;
2) the surfactant neopelex of 0.1% (mass ratio) is joined 1) the aqueous solution in, ultrasonic dispersion 30min; Add the aqueous solution of chloraurate that concentration is 1m mol/l then, normal temperature stirred 6 hours down, obtained nano Au particle enveloped carbon nanometer tube compound NH2.Found out that by Fig. 2 a in the NH2 compound that obtains, nano Au particle is coated on carbon nano tube surface in a large number, nano Au particle has particle diameter distribution preferably.
Embodiment 2:
1) CNT is carried out ultrasonic purification process, the high-purity carbon nano tube that obtains having certain dispersiveness in water in strong acid solution;
2) the surfactant polysorbate60 of 0.1% (mass ratio) is joined 1) the aqueous solution in, ultrasonic dispersion 30min; Add the aqueous solution of chloraurate that concentration is 1m mol/l then, normal temperature stirred 6 hours down, obtained nano Au particle enveloped carbon nanometer tube compound NH2.By Fig. 2 b, 2c finds out that in the NH2 compound that obtains, nano Au particle is coated on carbon nano tube surface in a large number, and nano Au particle has particle diameter distribution preferably.
Embodiment 3:
1) CNT is carried out ultrasonic purification process, the high-purity carbon nano tube that obtains having certain dispersiveness in water in strong acid solution;
2) N of institute, in the aqueous solution of N '-two (2-mercaptoethyl) perylene diimide (Fig. 4) is dissolved in N, forms saturated solution in N '-dimethyl formamide, joins 1), normal temperature stirs 30min down; Add the aqueous solution of chloraurate that concentration is 1m mol/l then, normal temperature stirred 6 hours down, obtained nano Au particle enveloped carbon nanometer tube compound NH3 (Fig. 3).In the NH3 compound, the nano Au particle high density is coated on carbon nano tube surface, and nano Au particle has very uniformly that particle diameter distributes, and particle diameter is very little, nearly all between 1-5nm, and does not reunite between the nano Au particle.This compound has fine solubility and stable preferably in water and various organic solvent.
Claims (5)
1. the in-situ solution preparation method of a nano Au particle coated carbon nanotube compound may further comprise the steps:
1. CNT is added in the strong acid solution, under ultrasound condition, carry out purification process, obtain dispersed carbon nano tube solution;
2. surfactant is joined step 1. in the carbon nano-tube solution that obtains of purifying, ultrasonic dispersion certain hour adds the aqueous solution of chloraurate that concentration is 0.1～100mmol/l then, normal temperature stirred 1 minute～24 hours down, obtained carbon mano-tube composite;
3. the 2. middle carbon mano-tube composite for preparing of step is come out with the supercentrifuge centrifugation.
2. in-situ solution preparation method according to claim 1 is characterized in that:
1. CNT is added in the strong acid solution, under ultrasound condition, carry out purification process, obtain dispersed carbon nano tube solution;
2. the organic molecule that has aromatic ring is dissolved in the organic solvent, join step 1. in the carbon nano-tube solution that obtains of purifying, stir or ultrasonic certain hour; Add the aqueous solution of chloraurate that concentration is 0.1mmol/l～100mmol/l then, normal temperature stirred 1 minute-24 hours down, obtained carbon mano-tube composite;
3. the 2. middle carbon mano-tube composite for preparing of step is come out with the supercentrifuge centrifugation.
3. in-situ solution preparation method according to claim 1, it is characterized in that: described surfactant is sodium alkyl sulfonate or tween series of surfactants, quality in carbon nano-tube aqueous solutions is 100%, and the consumption of surfactant is 0.01%-10%.
4. in-situ solution preparation method according to claim 2, it is characterized in that: the described organic molecule that has aromatic ring is to contain the organic molecule that sulfydryl replaces the De perylene diimide, contains band aromatic group such as the amino De of replacement perylene diimide, and the consumption of organic molecule is 0.01～10mg/ml solvent.
5. in-situ solution preparation method according to claim 2 is characterized in that: described organic solvent is N, N '-dimethyl formamide, ethanol, methyl alcohol or water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101555807A CN100488668C (en) | 2006-12-29 | 2006-12-29 | Nano gold particle evenly coated carbon nanotube compound in-situ solution preparation method |
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| CNB2006101555807A CN100488668C (en) | 2006-12-29 | 2006-12-29 | Nano gold particle evenly coated carbon nanotube compound in-situ solution preparation method |
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| CN1994625A true CN1994625A (en) | 2007-07-11 |
| CN100488668C CN100488668C (en) | 2009-05-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254916B (en) * | 2008-04-11 | 2010-04-07 | 北京工业大学 | Method for in-situ synthesis of metal phthalocyanine/carbon nano-tube compound |
| CN102539754A (en) * | 2011-09-29 | 2012-07-04 | 中国科学院合肥物质科学研究院 | Biological immune sensor and detection method thereof |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN104630869A (en) * | 2015-01-22 | 2015-05-20 | 江南大学 | DNA sensor for detecting staphylococcus aureus as well as preparation method and application of DNA sensor |
-
2006
- 2006-12-29 CN CNB2006101555807A patent/CN100488668C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254916B (en) * | 2008-04-11 | 2010-04-07 | 北京工业大学 | Method for in-situ synthesis of metal phthalocyanine/carbon nano-tube compound |
| CN102539754A (en) * | 2011-09-29 | 2012-07-04 | 中国科学院合肥物质科学研究院 | Biological immune sensor and detection method thereof |
| CN102539754B (en) * | 2011-09-29 | 2014-03-12 | 中国科学院合肥物质科学研究院 | Biological immune sensor and detection method thereof |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN103884693B (en) * | 2012-12-20 | 2016-09-07 | 江南大学 | A kind of single dispersing for anaphylactogen detection, the preparation method of low bio-toxicity gold nanorods |
| CN104630869A (en) * | 2015-01-22 | 2015-05-20 | 江南大学 | DNA sensor for detecting staphylococcus aureus as well as preparation method and application of DNA sensor |
| CN104630869B (en) * | 2015-01-22 | 2017-07-14 | 江南大学 | A kind of DNA sensor for detecting staphylococcus aureus and its preparation and application |
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| CN100488668C (en) | 2009-05-20 |
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