CN105921768A - Preparation method for metal, metal nanoparticles and ink - Google Patents

Preparation method for metal, metal nanoparticles and ink Download PDF

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Publication number
CN105921768A
CN105921768A CN201610532681.5A CN201610532681A CN105921768A CN 105921768 A CN105921768 A CN 105921768A CN 201610532681 A CN201610532681 A CN 201610532681A CN 105921768 A CN105921768 A CN 105921768A
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metal
solution
ink
mixed liquor
slaine
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Inventor
周虎
黄良辉
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GUANGDONG NANHAI ETEB TECHNOLOGY Co Ltd
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GUANGDONG NANHAI ETEB TECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/0003Metallic powders per se; Mixtures of metallic powders; Metallic powders mixed with a lubricating or binding agent
    • B22F1/0007Metallic powder characterised by its shape or structure, e.g. fibre structure
    • B22F1/0011Metallic powder characterised by size or surface area only
    • B22F1/0018Nanometer sized particles
    • B22F1/0022Dispersions or suspensions thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks

Abstract

The invention discloses a preparation method for metal, metal nanoparticles and ink. The preparation method includes the following steps that a metal salt-alcohol solution or a metal salt-water solution or a metal salt-alcohol water solution with the concentration ranging from 0.1 mol/L to 1.00 mol/L is prepared and stirred at the room temperature to be dissolved; the prepared metal salt solution is heated to 40 DEG C to 80 DEG C, then molten organic amine or organic acid or organic thiol or a mixture of organic amine, organic acid and organic thiol is injected dropwise, stirring is conducted for 30 min to 60 min till the mixture is dissolved; and the solution prepared through the steps mentioned above is subjected to vacuum-assisted heating and spray drying or filtering, and an intermediate is obtained. By the adoption of the intermediate, different metals and metal nanoparticle ink can be obtained through different technological paths; and furthermore, a precipitator is added, and pure nanoparticle solids can be obtained through filtering. By the adoption of the preparation method, preparation is easy, quality is reliable, the particle size of the metal and the metal nanoparticles can be expanded to 5 nm to 100 nm, different production requirements can be met, and the preparation method is widely applied to preparation methods of metals, metal nanoparticles and ink.

Description

A kind of metal and alloy nano particle thereof and the preparation method of ink
Technical field
The invention belongs to chemical field, be specifically related to the preparation method of a kind of metal and alloy nano particle thereof, especially relate to And a kind of metal forming mean diameter about 5-30nm and the method for alloy nano particle thereof, and can be directly synthesized and obtain phase Answer nanoparticle inks.
Background technology
Nanoparticle generally refers to the particle diameter particle at 1-100nm, is in cluster and the transitional region of macro object boundary, is A kind of typical mesoscopic systems, has special skin effect, small-size effect and macro quanta tunnel effect.Work as macro object After being subdivided into nanoparticle, the character in terms of its optics, calorifics, electricity, magnetics, mechanics and chemistry will have and significantly change Become, can be widely applied to the various fields such as electronics, medicine, chemical industry, military affairs, Aero-Space.
The current preparation method of nanoparticle mainly has vapour deposition, mechanical lapping and electronation three paths.Vapour deposition process It is by high density energy sources such as heat, electron beam, laser beams, melted for raw material evaporation or reaction to be decomposed, then makes it condense formation Nano-powder.Micro-powder is generally pulverized as nanometer grade powder by mechanical milling method in the mode of high-energy ball milling.Chemical reduction method is By various precursor solutions, it is reduced into nanoparticle with reducing agent.
The method of above-mentioned acquisition nanoparticle, the nano silver particles size dispersion that vapour deposition process obtains big (generally up to 1-200nm), Easily assembling, to prepare stable dispersion liquid be a challenge greatly for follow-up;The nano-particles size that mechanical milling method obtains is relatively Greatly (generally > 100nm), easily assemble, be not suitable for preparing nanometer ink;Chemical reduction method can obtain in size 1-100nm And the nanoparticle of uniform particle diameter, and its equipment the feature such as is simple and convenient to operate and becomes the main preparation methods of current nanoparticle. But most chemical methods need to introduce more chemical reagent, have that production cost is higher, Organic substance in system is difficult to remove, It is likely to be of the problems such as certain environmental pollution.
Summary of the invention
For the deficiencies in the prior art, it is desirable to provide a kind of particle diameter 5-30nm metal and alloy nano particle thereof are (expansible To produce particle diameter 5-100nm nanoparticle) new preparation method, the method can synthesize the metals such as gold, platinum, copper, palladium And the nanoparticle of alloy, preparation is simple, beneficially large-scale industrial production, and the present invention has following steps:
A kind of metal and alloy nano particle thereof and the preparation method of ink, comprise the following steps:
1) the slaine-ol solution of compound concentration 0.1 1.00mol/L, slaine-ol water or slaine-aqueous solution, Stirring and dissolving under room temperature, obtains slaine mixed liquor;
2) described slaine mixed liquor is heated to 40-80 DEG C, then drips the organic amine of fusing, organic acid, organic mercaptan Or its mixture, described slaine mixed liquor and organic amine, organic acid, organic mercaptan or the mol ratio of its mixture For 1:2--1:6, drip continuation stirring 30-60min;Obtain secondary mixed liquor.
Above-mentioned slaine mixed liquor includes gold, platinum, copper, the alcohol-soluble of palladium metal, water solublity and ammonia dissolubility salt and mixture thereof; Described alcoholic solution is methanol, ethanol, propanol, isopropanol, butanol;Described organic amine be carbon chain lengths 8-30 chain alkyl or Aralkylamine, described organic acid is chain alkyl or the aralkyl acid of carbon chain lengths 2-18;Described organic mercaptan is carbon chain lengths The chain alkyl of 8-30 or aromatic alkyl thioalcohol.
When the solvent of above-mentioned slaine mixed liquor is described alcoholic solution, secondary mixed liquor is heated to 60-80 DEG C, and assists evacuation, I.e. can get thick shape intermediate, described thick shape intermediate is continued to be heated to 150-400 DEG C, keep 10-60min, obtain oily Solution;After cooling, adding the precipitant of 3-5 times of volume, stir 5-15min, sucking filtration i.e. obtains nanoparticle solid.
Above-mentioned precipitant is one or more mixture in water, methanol, ethanol, acetone.
When the solvent of above-mentioned slaine mixed liquor is described alcohol water, then secondary mixed liquor is spray-dried and i.e. can get powdery intermediate; Described powdery intermediate is joined in ethylene glycol, glycerol, low molecular poly high-boiling point alcohol, stirs at 60-150 DEG C Mix dissolving reaction 30-120min and obtain three mixed liquors;By described three mixed liquors and toluene, benzene, hexamethylene, normal hexane, ring The alkane such as heptane, normal heptane or aromatic hydrocarbons mixing, volume ratio is 1:0.5-3, and stratification after stirring 30min, upper strata is for containing The oil phase of nanoparticle, lower floor is high boiling point alcohol phase, and isolated oily liquid can use directly as ink;Or further In the oily liquid obtained, add the precipitant of 3-5 times of volume, stir 5-10min, filter and i.e. obtain nanoparticle solid.
When the solvent of above-mentioned slaine mixed liquor is described aqueous solution, then secondary mixed liquor is filtered to obtain viscous shape intermediate, Described viscous shape intermediate is joined in toluene, hexamethylene alkane or aromatic solvent, at 30-80 DEG C, dissolves 60-240min, obtain Obtain solid content 1.0-10.0wt% solution;Preparation 5.0-20.0wt% reducing agent aqueous solution;Reducing agent aqueous solution is added dropwise to above-mentioned molten Liquid, volume ratio 1:0.5-3, to react 60-300min, stand split-phase, upper strata is the oil phase containing nanoparticle, and lower floor is water Phase, isolated oily liquid can use directly as ink;Or in the oily liquid obtained, add 3-5 times of volume further Precipitant, stir 5-15min, sucking filtration i.e. obtains nanoparticle solid.
Above-mentioned reducing agent is the compound of hydrazine or hydrazine, sodium borohydride, hexamethylenetetramine.
Due to technique scheme, the invention has the beneficial effects as follows: equipment is simple, operating process is convenient, and production cost is the highest, Organic substance in system is removed at all, is not had the problems such as environmental pollution, and oiliness nanoparticle can be extended to particle diameter 5-100nm, adapts to different Production requirements;Can be directly synthesized and obtain nanoparticle inks, convenient application.
Due to above-mentioned beneficial effect, the present invention is widely used in the preparation method of metal and alloy nano particle thereof and its ink.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
1) Cu (NO of compound concentration 1.0mol/L3)2-aqueous solution, stirring and dissolving under room temperature;
2) lauric acid/dodecanoic acid is added heat fusing at 60 DEG C;
3) by above-mentioned steps 1) solution that obtains is heated to 50 DEG C, and drip by the lauric acid/dodecanoic acid of fusing, stir 60 minutes, Mantoquita is 1:4 with the mol ratio of lauric acid/dodecanoic acid;
4) by above-mentioned steps 3) solution that obtains is cooled to room temperature, and form turbid solution, filter and i.e. obtain thick shape intermediate;
5) thick shape intermediate is heated to 250 DEG C, keeps 30 minutes, obtain oily liquids;
6) adding the methanol extraction nanometer copper particle of 3 times of volumes, sucking filtration i.e. obtains nanometer copper particle solid.
Embodiment 2:
1) PdCl of compound concentration 0.2mol/L2-ethanol solution, stirring and dissolving under room temperature;
2) 18-amine. is added heat fusing at 60 DEG C;
3) by above-mentioned steps 1) solution that obtains is heated to 50 DEG C, and drip by the 18-amine. of fusing, stir 60 minutes, Palladium salt is 1:3 with the mol ratio of 18-amine.;
4) at 50 DEG C, evacuation removes ethanol, obtains thick shape intermediate;
5) thick shape intermediate is heated to 300 DEG C, keeps 45 minutes, obtain oily liquids;
6) adding the acetone precipitation palladium nanoparticles of 3 times of volumes, sucking filtration i.e. obtains palladium nanoparticles solid.
Above-mentioned two embodiment, i.e. embodiment 1 and embodiment 2 are for " solvent of described slaine mixed liquor is that described alcohol is molten During liquid " time being expanded on further of preparation method path, concrete corresponding technical scheme is:
1) the slaine-ol solution of compound concentration 0.1 1.00mol/L, slaine-ol water or slaine-aqueous solution, Stirring and dissolving under room temperature, obtains slaine mixed liquor;
2) described slaine mixed liquor is heated to 40-80 DEG C, then drips the organic amine of fusing, organic acid, organic mercaptan Or its mixture, described slaine mixed liquor is 1 with the mol ratio of organic amine, organic acid, organic mercaptan or its mixture: 2--1:6, drips continuation stirring 30-60min, obtains secondary mixed liquor.
When the solvent of above-mentioned slaine mixed liquor is described alcoholic solution, secondary mixed liquor is heated to 60-80 DEG C, and assists evacuation, I.e. can get thick shape intermediate, described thick shape intermediate is continued to be heated to 150-400 DEG C, keep 10-60min, obtain oily Solution;After cooling, adding the precipitant of 3-5 times of volume, stir 5-15min, sucking filtration i.e. obtains nanoparticle solid.
Embodiment 3:
1) PtCl of compound concentration 0.4mol/L2-ammonia spirit, stirring and dissolving under room temperature;
2) stearylmercaptan is added heat fusing at 40 DEG C;
3) by above-mentioned steps 1) solution that obtains is heated to 50 DEG C, and drip by the stearylmercaptan of fusing, stir 60 minutes, Platinum salt is 1:2 with the mol ratio of stearylmercaptan;
4) by above-mentioned steps 3) solution that obtains is cooled to room temperature, and form turbid solution, filter and i.e. obtain thick shape intermediate;
5) above-mentioned thick shape intermediate is joined in ethylene glycol, dissolve at 150 DEG C and form concentration 10.0wt% solution, continue anti- Answer 120 minutes;
6) it being cooled to room temperature, by step 5) solution that obtains mixes with hexamethylene, and volume ratio is 1:1, stirs 30 minutes Rear stratification, upper strata is the oil phase containing Platinum Nanoparticles, can use directly as ink;
7) for obtaining nanoparticle solid, to above-mentioned steps 6) oily liquids that obtains adds the ethanol of 5 times of volumes, stir Mix 5-10 minute, filter and i.e. obtain nanoparticle solid.
Embodiment 4:
1) AuCl of compound concentration 0.5mol/L3-ethanol solution, stirring and dissolving under room temperature;
2) stearylmercaptan is added heat fusing at 40 DEG C;
3) by above-mentioned steps 1) solution that obtains is heated to 45 DEG C, and drip by the stearylmercaptan of fusing, stir 45 points Clock, gold salt is 1:3 with the mol ratio of stearylmercaptan;
4) at 50 DEG C, evacuation removes ethanol, obtains thick shape intermediate;
5) above-mentioned thick shape intermediate is joined in PEG-4000, dissolves at 150 DEG C and form concentration 5.0wt% solution, Continue reaction 120 minutes;
6) it being cooled to room temperature, by step 5) solution that obtains mixes with toluene, and volume ratio is 1:2, stirs 30 minutes Rear stratification, upper strata is the oil phase containing nanometer gold, can use directly as ink;
7) for obtaining nanoparticle solid, to above-mentioned steps 6) oily liquids that obtains adds the acetone of 2 times of volumes, Stir 5-10 minute, filter and i.e. obtain nanoparticle solid.
Above-mentioned two embodiment, i.e. embodiment 3 and embodiment 4 are for " solvent of described slaine mixed liquor is described During alcohol water " time being expanded on further of preparation method path, concrete corresponding technical scheme is:
1) the slaine-ol solution of compound concentration 0.1 1.00mol/L, slaine-ol water or slaine-aqueous solution, It is stirred at room temperature dissolving, obtains slaine mixed liquor;
2) described slaine mixed liquor is heated to 40-80 DEG C, then drips the organic amine of fusing, organic acid, organic mercaptan Or its mixture, described slaine mixed liquor with the mol ratio of organic amine, organic acid, organic mercaptan or its mixture is 1:2--1:6, drips continuation stirring 30-60min, obtains secondary mixed liquor.
When the solvent of described slaine mixed liquor is described alcohol water, then secondary mixed liquor i.e. be can get powder by being spray-dried Shape intermediate;Described powdery intermediate is joined in ethylene glycol, glycerol, low molecular poly high-boiling point alcohol, At 60-150 DEG C, stirring and dissolving reaction 30-120min obtains three mixed liquors;By described three mixed liquors and toluene, benzene, The alkane such as hexamethylene, normal hexane, cycloheptane, normal heptane or aromatic hydrocarbons mixing, volume ratio is 1:0.5-3, stirs 30min Rear stratification, upper strata is the oil phase containing nanoparticle, and lower floor is high boiling point alcohol phase, isolated oily liquid Use directly as ink;Or in the oily liquid obtained, add the precipitant of 3-5 times of volume, stirring further 5-10min, filters and i.e. obtains nanoparticle solid.
Embodiment 5:
1) PtCl of compound concentration 0.5mol/L2-ammonia spirit, stirring and dissolving under room temperature;
2) CuCl of compound concentration 0.5mol/L2-ethanol solution, stirring and dissolving under room temperature;
3) 18-amine. is added heat fusing at 60 DEG C;
4) by above-mentioned PtCl2-ammonia spirit is heated to 60 DEG C, 18-amine. dropping is entered, and stirs reaction 60 minutes, platinum Salt is 1:3 with the mol ratio of 18-amine.;
5) by above-mentioned steps 4) solution that obtains is cooled to room temperature, and form turbid solution, filter and i.e. obtain viscous shape intermediate A;
6) by above-mentioned CuCl2-ethanol solution is heated to 60 DEG C, 18-amine. dropping is entered, and stirs reaction 30 minutes, copper Salt is 1:4 with the mol ratio of 18-amine.;
7) by above-mentioned steps 6) solution that obtains is warmed up to 60 DEG C, evacuation, obtains viscous shape intermediate B;
8) weigh 2.00g thick shape intermediate B and 0.10g thick shape intermediate A, under stirring, add 40mL toluene, be heated to 40 DEG C, keep 180 minutes;
9) prepare 10% hydrazine-aqueous solution, and take 20mL, at 40 DEG C, dropwise add to above-mentioned steps 8) solution that obtains, stirring After reacting 120 minutes, it is layered to obtain oily solution, can use as ink;
10) for obtaining nanoparticle solid, to above-mentioned steps 9) oily liquids that obtains adds the acetone of 4 times of volumes, Stirring 5-15min, sucking filtration PtCux(x=5-20) nanoparticle solid.
Embodiment 6:
1) AuCl of compound concentration 0.5mol/L3-ethanol solution, stirring and dissolving under room temperature;
2) CuCl of compound concentration 0.5mol/L2-ethanol solution, stirring and dissolving under room temperature;
3) stearylmercaptan is added heat fusing at 40 DEG C;
4) by above-mentioned AuCl3-ethanol solution is heated to 40 DEG C, stearylmercaptan dropping is entered, stirring reaction 30 minutes, gold salt It is 1:3 with the mol ratio of stearylmercaptan;
5) by above-mentioned steps 4) solution that obtains is warmed up to 60 DEG C, evacuation, obtains viscous shape intermediate A;
6) by above-mentioned CuCl2-ethanol solution is heated to 40 DEG C, stearylmercaptan dropping is entered, stirring reaction 30 minutes, mantoquita It is 1:2 with the mol ratio of stearylmercaptan;
7) by above-mentioned steps 6) solution that obtains is warming up to 60 DEG C, evacuation, obtains viscous shape intermediate B;
8) weigh 2.00g intermediate B and 0.10g intermediate A, under stirring, add 40mL toluene, be heated to 40 DEG C, protect Hold 180 minutes;
9) prepare 20% sodium borohydride-aqueous solution, and take 20mL, at 40 DEG C, dropwise add to above-mentioned steps 8) solution that obtains, After stirring reaction 90 minutes, it is layered to obtain oily solution, can use as ink;
10) for obtaining nanoparticle solid, add the methanol of 3 times of volumes, stir 5-15min, sucking filtration, obtain AuCux (x=5-20) nanoparticle solid.
Above-mentioned two embodiment, i.e. embodiment 5 and embodiment 6 are for " solvent of described slaine mixed liquor is described water body When being " time being expanded on further of preparation method path, concrete corresponding technical scheme is:
1) the slaine-ol solution of compound concentration 0.1 1.00mol/L, slaine-ol water or slaine-aqueous solution, Stirring and dissolving under room temperature, obtains slaine mixed liquor;
2) described slaine mixed liquor is heated to 40-80 DEG C, then drip the organic amine of fusing, organic acid, organic mercaptan or Its mixture, described slaine mixed liquor is 1:2--1 with the mol ratio of organic amine, organic acid, organic mercaptan or its mixture: 6, drip continuation stirring 30-60min, obtain secondary mixed liquor.
When the solvent of described slaine mixed liquor is described aqueous solution, secondary mixed liquor is filtered to obtain viscous shape intermediate, Described viscous shape intermediate is joined in toluene, hexamethylene alkane or aromatic solvent, at 30-80 DEG C, dissolves 60-240min, obtain Obtain solid content 1.0-10.0wt% solution;Preparation 5.0-20.0wt% reducing agent aqueous solution;Reducing agent aqueous solution is added dropwise to above-mentioned molten Liquid, volume ratio 1:0.5-3, to react 60-300min, stand split-phase, upper strata is the oil phase containing nanoparticle, and lower floor is water Phase, isolated oily liquid can use directly as ink;Or in the oily liquid obtained, add 3-5 times of volume further Precipitant, stir 5-15min, sucking filtration i.e. obtains nanoparticle solid.

Claims (7)

1. metal and alloy nano particle thereof and a preparation method for ink, comprises the following steps:
1) the slaine-ol solution of compound concentration 0.1 1.00mol/L, slaine-ol aqueous solution or slaine-aqueous solution, It is stirred at room temperature dissolving, obtains slaine mixed liquor;
2) described slaine mixed liquor is heated to 40-80 DEG C, then drips the organic amine of fusing, organic acid, organic mercaptan Or its mixture, described slaine mixed liquor and organic amine, organic acid, organic mercaptan or the mol ratio of its mixture For 1:2--1:6, drip continuation stirring 30-60min, obtain secondary mixed liquor.
A kind of metal the most according to claim 1 and alloy nano particle thereof and the preparation method of ink, it is characterised in that: Described slaine mixed liquor includes gold, platinum, copper, the alcohol-soluble of palladium metal, water solublity and ammonia dissolubility salt and mixture thereof;Institute Stating alcoholic solution is methanol, ethanol, propanol, isopropanol, butanol;Described organic amine is chain alkyl or the virtue of carbon chain lengths 8-30 Alkylamine, described organic acid is chain alkyl or the aralkyl acid of carbon chain lengths 2-18;Described organic mercaptan is carbon chain lengths 8-30 Chain alkyl or aromatic alkyl thioalcohol.
A kind of metal the most according to claim 1 and 2 and alloy nano particle thereof and the preparation method of ink, its feature exists In: the solvent of described slaine mixed liquor is described alcoholic solution, then described secondary mixed liquor is heated to 60-80 DEG C, and auxiliary is taken out Vacuum, i.e. can get thick shape intermediate, continues to be heated to 150-400 DEG C by described thick shape intermediate, keeps 10-60min, i.e. Obtain oily solution;After cooling, adding the precipitant of 3-5 times of volume, stir 5-15min, sucking filtration i.e. obtains nanoparticle solid.
A kind of metal the most according to claim 3 and alloy nano particle thereof and the preparation method of ink, it is characterised in that: Described precipitant is one or more mixture in water, methanol, ethanol, acetone.
A kind of metal the most according to claim 1 and 2 and alloy nano particle thereof and the preparation method of ink, its feature exists In: the solvent of described slaine mixed liquor is described alcohol-water solution, then described secondary mixed liquor is the most available by spray drying Powdery intermediate;Described powdery intermediate is joined in ethylene glycol, glycerol, low molecular poly high-boiling point alcohol, At 60-150 DEG C, stirring and dissolving reaction 30-120min obtains three mixed liquors;By described three mixed liquors and toluene, benzene, hexamethylene, The alkane such as normal hexane, cycloheptane, normal heptane or aromatic hydrocarbons mixing, volume ratio is 1:0.5-3, stratification after stirring 30min, Upper strata is the oil phase containing nanoparticle, and lower floor is high boiling point alcohol phase, and isolated oily liquid can use directly as ink; Or in the oily liquid obtained, add the precipitant of 3-5 times of volume further, stir 5-10min, filter and i.e. obtain nanoparticle Sub-solid.
A kind of metal the most according to claim 1 and 2 and alloy nano particle thereof and the preparation method of ink, its feature exists In: the solvent of described slaine mixed liquor is described aqueous solution, then described secondary mixed liquor is filtered in the middle of viscous shape Body, joins in toluene, hexamethylene alkane or aromatic solvent by described viscous shape intermediate, dissolves 60-240min at 30-80 DEG C, Obtain solid content 1.0-10.0wt% solution;Preparation 5.0-20.0wt% reducing agent aqueous solution;Reducing agent aqueous solution is added dropwise to above-mentioned Solution, volume ratio 1:0.5-3, to react 60-300min, stand split-phase, upper strata is the oil phase containing nanoparticle, and lower floor is Aqueous phase, isolated oily liquid can use directly as ink;Or in the oily liquid obtained, add 3-5 times of body further Long-pending precipitant, stirs 5-15min, and sucking filtration i.e. obtains nanoparticle solid.
A kind of metal the most according to claim 6 and alloy nano particle thereof and the preparation method of ink, it is characterised in that: Described reducing agent is the compound of hydrazine or hydrazine, sodium borohydride, hexamethylenetetramine.
CN201610532681.5A 2016-07-07 2016-07-07 Preparation method for metal, metal nanoparticles and ink Pending CN105921768A (en)

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CN108284232B (en) * 2018-01-26 2021-07-20 上海应用技术大学 Preparation method of silver nanoparticles
CN108971513A (en) * 2018-10-12 2018-12-11 圣戈莱(北京)科技有限公司 A kind of nano copper particle and its inexpensive environmentally protective preparation method
CN108971513B (en) * 2018-10-12 2021-09-21 圣戈莱(北京)科技有限公司 Nano copper particle and low-cost green and environment-friendly preparation method thereof

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