CN102921961A - Method for producing metallic nanomaterials through femtosecond lasers - Google Patents
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims description 33
- 239000002184 metal Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 210000004877 mucosa Anatomy 0.000 claims description 14
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 13
- 229910052700 potassium Inorganic materials 0.000 claims description 13
- 239000011591 potassium Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- -1 gold potassium bromide Chemical compound 0.000 claims description 4
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 claims description 4
- ZHHGTDYVCLDHHV-UHFFFAOYSA-J potassium;gold(3+);tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Au+3] ZHHGTDYVCLDHHV-UHFFFAOYSA-J 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- VBWYZPGRKYRKNV-UHFFFAOYSA-N 3-propanoyl-1,3-benzoxazol-2-one Chemical compound C1=CC=C2OC(=O)N(C(=O)CC)C2=C1 VBWYZPGRKYRKNV-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 3
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940071536 silver acetate Drugs 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 238000001069 Raman spectroscopy Methods 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 230000002787 reinforcement Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 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 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000003760 hair shine Effects 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000007540 photo-reduction reaction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
The invention discloses a method for producing metallic nanomaterials through femtosecond lasers. According to the method, the lasers are used for directly irradiating metallic salt solution, thus obtaining the metallic nanomaterials with different shapes, wherein the time for laser irradiation is 1-3600 seconds, the average power of the incoming lasers is 5mW-400mW, and the concentration of the metallic salt solution is 1m mol/L-1mol/L. The method is simple and convenient, and does not need any reducing agent or surface active agent; and moreover, reaction conditions are simple and easy to control and are environment-friendly. The shapes and sizes of the produced metallic nanomaterials can be controlled, and the produced metallic nanomaterials can be applied to the fields of catalysis, electrochemistry, surface raman reinforcement or biomedicines and the like.
Description
Technical field
The present invention relates to the metal nano material technical field, be specifically related to the method that a kind of femtosecond laser prepares metal nano material.
Background technology
Along with the development of nearly decades, nano science has become one of scientific research field of current hot topic.And metal nanoparticle becomes the emphasis of nano science research owing to character such as its distinctive skin effect, small-size effect, macro quanta tunnel effects.Corresponding metal nano material has been applied to the numerous areas such as bio-sensing, catalysis, electronics industry, optics.The current existing multiple method for preparing metal nano material is such as vapor phase method, chemical precipitation method, sol-gel process, chemical reduction method, heat drop solution, photoreduction met hod etc.Wherein photo-reduction ratio juris is the character that part metals has surface plasma body resonant vibration, can be under the visible region light absorbing energy.When having a certain specific light source that the solution that contains metal ion is shone, metal ion can be reduced.If control suitable reaction condition, just can access the metal nano material of different-shape and size.Compare with additive method, photoreduction met hod has simple to operate, reaction temperature and etc. advantage, therefore also become a kind of common method of preparation metal nano material.
Reported at present to prepare metal nano material with photoreduction met hod mainly be the aqueous solution that contains metal ion with UV-irradiation, obtain metal nano material.Also there is report to shine the liquor argenti nitratis ophthalmicus that contains reducing agent with the diode lights that can regulate optical wavelength, obtains the silver nano material of different-shape.But these light sources are because light intensity is lower, and the irradiation time that often needs to grow just can react completely very.If use the laser illumination that energy density is high, directionality is good, then can just can make the metal ion reduction within a short period of time, prepare metal nano material.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the purpose of this invention is to provide the method that a kind of femtosecond laser prepares metal nano material, it is had simple to operate, consuming time shorter, environmental friendliness, the characteristics such as pattern and size are controlled.Prepared metal nano material can be used for the fields such as catalysis, electrochemistry, surface Raman enhancement or biomedicine.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of femtosecond laser prepares the method for metal nano material: directly shine with the laser alignment metal salt solution, obtain the metal nano material of different-shape; Wherein, the time of Ear Mucosa Treated by He Ne Laser Irradiation is 1 ~ 3600s, and the mean power of incident laser is 5 ~ 400mW, and the concentration of metal salt solution is 1mmol/L ~ 1mol/L.
Described slaine comprises silver nitrate, silver acetate, gold chloride, sodium chloraurate, potassium chloroaurate, auribromohydric acid, sodium terabomoaurate, gold potassium bromide, iodo-auric acid, Potassium Tetraiodoaurate, chloroplatinic acid, platinic sodium chloride, potassium chloroplatinate, bromoplatinic acid, potassium bromoplatinate, potassium bromoplatinate, platinic sulfate, platinum nitrate, copper sulphate, copper nitrate, copper chloride, copper bromide, and any molar mixture of gold chloride and chloroplatinic acid.
The solvent of described metal salt solution comprises water, methyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, oxolane, DMF, DMAc, and, the mixing of the arbitrary volume ratio of one or more among water and methyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, oxolane, DMF, the DMAc.
The concentration of described metal salt solution is preferably 10 ~ 100mmol/L.
The time of described Ear Mucosa Treated by He Ne Laser Irradiation, be preferably 600 ~ 1200s.
The mean power of described incident laser is preferably 20 ~ 50mW.
Described Ear Mucosa Treated by He Ne Laser Irradiation sample has rays pass through lens to focus on rear irradiation and direct irradiation dual mode.
Used light source is femto-second laser among the present invention, and the laser of its generation has the advantages that the pulse duration is short, peak power is high.In the situation that gross output is less, femto-second laser also can provide enough energy for the chemical reaction that some needs very high-energy could occur.And therefore femtosecond laser gross output and little can not cause material to be burnt.
Beneficial effect: compared with prior art, advantage of the present invention comprises: the present invention adopts above-mentioned process, and is simple and convenient, need not to add any reducing agent or surfactant, and reaction condition is simple and easy to control, environmental friendliness.Prepared metal nano material pattern and size are controlled, can be applicable to the fields such as catalysis, electrochemistry, surface Raman enhancement or biomedicine.
Description of drawings
Fig. 1 is that femtosecond laser prepares metal nano material experiment index path;
Fig. 2 is AgNO
3The transmission electron microscope photo of the nano particle that forms behind the process Ear Mucosa Treated by He Ne Laser Irradiation;
Fig. 3 is the transmission electron microscope photo that chlorauric acid solution passes through the nanometer rods that forms behind the Ear Mucosa Treated by He Ne Laser Irradiation;
Fig. 4 is the transmission electron microscope photo that chlorauric acid solution passes through the hexagonal nanosheet that forms behind the Ear Mucosa Treated by He Ne Laser Irradiation;
Fig. 5 is the transmission electron microscope photo that gold chloride and chloroplatinic acid mixed solution pass through the nanometer rods that forms behind the Ear Mucosa Treated by He Ne Laser Irradiation;
The specific embodiment
The present invention is described further below in conjunction with specific embodiment.
Embodiment 1
As shown in Figure 1, used laser instrument is the Legend Elite femto-second laser of Coherent company.Debugging laser makes the light path of laser aim at the plane of incidence of sample cell.Use the lens on light line focus, the position of focus is at the center of sample cell inside.Then the power with laser transfers to 20mW, and the silver nitrate aqueous solution of the 10mmol/L for preparing is added in the sample cell, shines after leaving standstill 5min again.Behind the irradiation 600s, sample is detected.AgNO
3Through the nano particle that forms behind the Ear Mucosa Treated by He Ne Laser Irradiation, as shown in Figure 2.
Embodiment 2
Replace silver nitrate with silver acetate, other conditions are with embodiment 1.
Embodiment 3
Debugging laser takes off lens, the hot spot of laser is aimed at the plane of incidence of sample cell.Then the power with laser transfers to 400mW, and the chlorauric acid solution of the 1mmol/L for preparing is added in the sample cell, shines after leaving standstill 5min again.Behind the irradiation 1s, sample is detected.The nanometer rods of gold chloride through forming behind the Ear Mucosa Treated by He Ne Laser Irradiation, as shown in Figure 3.After shining 2 min, sample is detected.The hexagonal nanosheet of chlorauric acid solution through forming behind the Ear Mucosa Treated by He Ne Laser Irradiation, as shown in Figure 4.
Embodiment 4
Replace gold chloride with sodium chloraurate, potassium chloroaurate, auribromohydric acid, sodium terabomoaurate, gold potassium bromide, iodo-auric acid, Potassium Tetraiodoaurate respectively, other conditions are with embodiment 3.
Embodiment 5
Debugging laser makes the light path of laser aim at the plane of incidence of sample cell.Use the lens on light line focus, the position of focus is at the center of sample cell.Then the power with laser transfers to 50mW, and the copper sulfate solution of the 1mol/L for preparing is added in the sample cell, shines after leaving standstill 5min again.Behind the irradiation 1200s, sample is detected.
Embodiment 6
Replace copper sulphate with copper nitrate, copper chloride, copper bromide respectively, other conditions are with embodiment 5.
Embodiment 7
Debugging laser makes the light path of laser aim at the plane of incidence of sample cell.Use the lens on light line focus, the position of focus is at the center of sample cell.Then the power with laser transfers to 5mW, and the gold chloride of the total concentration 100mmol/L for preparing and the aqueous solution of chloroplatinic acid mol ratio 1:1 are added in the sample cell, shines after leaving standstill 5min again.Behind the irradiation 3600s, sample is detected.Gold chloride and the chloroplatinic acid mixed solution nanometer rods through forming behind the Ear Mucosa Treated by He Ne Laser Irradiation, as shown in Figure 5.
Embodiment 8
Replace gold chloride with sodium chloraurate, potassium chloroaurate, auribromohydric acid, sodium terabomoaurate, gold potassium bromide, iodo-auric acid, Potassium Tetraiodoaurate respectively, replace chloroplatinic acid with platinic sodium chloride, potassium chloroplatinate, bromoplatinic acid, potassium bromoplatinate, potassium bromoplatinate, platinic sulfate, platinum nitrate respectively simultaneously, the two kinds of samples in front and back can be corresponding arbitrarily, and (other conditions are with embodiment 7.
Embodiment 9
Replace water among the embodiment 1 to 8 with the mixed solvent of methyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, oxolane, DMF, DMAc or water and above-mentioned solvent arbitrary volume ratio, other conditions are with embodiment 1 to 8.
Claims (7)
1. a femtosecond laser prepares the method for metal nano material, it is characterized in that: directly shine with the laser alignment metal salt solution, obtain the metal nano material of different-shape; Wherein, the time of Ear Mucosa Treated by He Ne Laser Irradiation is 1 ~ 3600s, and the mean power of incident laser is 5 ~ 400mW, and the concentration of metal salt solution is 1mmol/L ~ 1mol/L.
2. the method for preparing metal nano material according to claims 1 described femtosecond laser, it is characterized in that: described slaine comprises silver nitrate, silver acetate, gold chloride, sodium chloraurate, potassium chloroaurate, auribromohydric acid, sodium terabomoaurate, gold potassium bromide, iodo-auric acid, Potassium Tetraiodoaurate, chloroplatinic acid, platinic sodium chloride, potassium chloroplatinate, bromoplatinic acid, potassium bromoplatinate, potassium bromoplatinate, platinic sulfate, platinum nitrate, copper sulphate, copper nitrate, copper chloride, copper bromide, and any molar mixture of gold chloride and chloroplatinic acid.
3. the method for preparing metal nano material according to claims 1 described femtosecond laser, it is characterized in that: the solvent of described metal salt solution comprises water, methyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, oxolane, DMF, DMAc, and, the mixing of the arbitrary volume ratio of one or more among water and methyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, oxolane, DMF, the DMAc.
4. prepare the method for metal nano material according to claims 1 described femtosecond laser, it is characterized in that: the concentration of described metal salt solution is 10 ~ 100mmol/L.
5. prepare the method for metal nano material according to claims 1 described femtosecond laser, it is characterized in that: the time of described Ear Mucosa Treated by He Ne Laser Irradiation is 600 ~ 1200s.
6. prepare the method for metal nano material according to claims 1 described femtosecond laser, it is characterized in that: irradiation and two kinds of methods of direct irradiation after the method for described Ear Mucosa Treated by He Ne Laser Irradiation sample has rays pass through lens to focus on.
7. prepare the method for metal nano material according to claims 1 described femtosecond laser, it is characterized in that: the mean power of described incident laser is 20 ~ 50mW.
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