CN104018189B - A kind of preparation method of nano-silver thread - Google Patents
A kind of preparation method of nano-silver thread Download PDFInfo
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- CN104018189B CN104018189B CN201410247264.7A CN201410247264A CN104018189B CN 104018189 B CN104018189 B CN 104018189B CN 201410247264 A CN201410247264 A CN 201410247264A CN 104018189 B CN104018189 B CN 104018189B
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Abstract
The preparation method who the invention discloses a kind of nano-silver thread, comprising: get silver salt or argent-amine complex, add dissolution with solvents to obtain A liquid; Get organic substance, add dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid, be stirred to completely and dissolve; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, cell reaction 1～30min under the condition that is 1～50V at voltage; Reacted cathode plate is clean with distilled water flushing, at room temperature natural drying, obtain nano-silver thread. The present invention can control thickness and the draw ratio of nano-silver thread easily by electric field, realize the controllable growth to nanostructured, by adjusting current density, voltage and reaction time, make the nano-silver thread pattern of generation controlled, the nano-silver thread that can be 1～50nm by diameter, nanometer rods are synthesized, preparation technology of the present invention is simple, and cost is low, and the efficiency of synthesizing nano-silver line and nano-bar is higher.
Description
Technical field
The present invention relates to the preparation method of a kind of novel preparation technology of nano-noble metal structure, particularly a kind of nano-silver thread.
Background technology
The particle diameter of nanoparticle is minimum, and specific surface is very big, thereby performance optical, electrical, the magnetic property and the chemical property that make new advances. OrderBefore, the new material being made up of nanoparticle is at catalysis, luminescent material, magnetic material, semi-conducting material and fine ceramics materialBe widely applied in field. Nano Silver is as the important component part of noble metal nanometer material, except possessing common metalOutside the character such as skin effect, quantum size effect, bulk effect and the macro quanta tunnel effect of nano material, it is special also to haveSurface plasmon resonance effect, therefore, Nano Silver is used widely in fields such as catalysis, antibacterial, photoelectricity and superconductions.
In numerous metals, because silver has best conductive and heat-conductive effect, the nano silver wire of one dimension or nanometer bundle are in nanometer circuitHave broad application prospects. Bearing capacity by the resistance to nano silver wire and electric current is carried out system research, found that diameterFor the resistance of the nano-silver thread of 20nm is only 2 times of block silver. Present stage is prepared the method for silver nano material, is mainly divided intoPhysical and the large class of chemical method two, wherein chemical method because its technique is simple, economical, low for equipment requirements, easy scale etc. is excellentThereby gesture is able to fast development, generally chemical method can be divided into substantially to following a few class: template, wet chemistry method and polyalcohol method.
(1) template: refer to based on additional template, make nano material backed stamper plate hole road system by nano pore restrictionA kind of standby method, first the method needs to prepare as requested corresponding template in preparation process, as polymer template, oxidationAluminum alloy pattern plate, biomolecule (as protein dna) template etc., also need to carry out high-temperature calcination, and will carry out complicated later stage placeReason, thereby nano-silver thread complex process, cost prepared by this method are higher, and also the activity of nano-silver thread is lower, and growth is slowSlowly, pore distribution is inhomogeneous.
(2) wet chemistry method: be the general name of many different chemical methodes, its common feature is that reaction system is that liquid phase is (manyFor water), adopt organic matter or inorganic ions as stabilizing agent or derivant, conventionally also there is reducing agent, its critical process existsIn the reduction reaction initial stage, stabilizing agent just Already in system, plays restriction inhibition to the metal cluster in growth. ThisMethod is general only reacts in extremely dilute solution, and concentration improves just need to add stabilizing agent; Due to anti-with redox in course of reactionShould be main, thereby nanometer product deposition velocity is very fast, and deposition do not have directionality (generally taking spherical or block product asMain).
(3) polyalcohol method: be the one of wet chemistry method, but because it is preparing unique advantage in metal nano material, at presentIn known method, the pattern of its metal nano material obtaining is the abundantest, but also can be widely used in different goldBelong to, therefore cause various places researcher's very big interest. Because the solvent the most often using in polyalcohol method is ethylene glycol, its dielectric is normalNumber higher, except dissolving plurality of inorganic salt, can also dissolve part macromolecule (as polyvinylpyrrolidone,PVP), thereby many seminar all introduce PVP in polyalcohol method as stabilizing agent and derivant, and slaine is presoma,React and prepare metal nano material by adjusting. The method needs additional protective agent and reducing agent, the nano-metal particle shape of preparationLooks are larger.
Although above-mentioned several method can be prepared nano silver powder, it all can not realize the effective control to nanostructured,Such as particle size, club-shaped material pattern etc., and the method having need to be carried out high temperature sintering or under hydrothermal condition, be carried out anti-Should, thereby greatly increase preparation cost and difficulty.
Summary of the invention
The object of the invention is to, a kind of preparation method of nano-silver thread is provided, it can effectively solve and to exist in prior artThe problem that problem, especially complex process, cost be higher, can not realize the effective control to nanostructured.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of preparation method of nano-silver thread, comprise withLower step: get silver salt or argent-amine complex, add dissolution with solvents to obtain A liquid; Get organic substance, add dissolution with solvents to obtain BLiquid; A liquid is mixed with B liquid, be stirred to completely and dissolve; Add complexing agent again, stir, stratification, obtains CLiquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, at voltage isCell reaction 1～30min under the condition of 1～50V; Reacted cathode plate is clean with distilled water flushing, at room temperature certainlySo dry, obtain nano-silver thread.
Preferably, comprise the following steps: get silver salt or argent-amine complex, add dissolution with solvents to obtain A liquid; Get organic substance,Add dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid, be stirred to completely and dissolve; Add again complexing agent, stir,Stratification, obtains C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyteOil reservoir is that 25～35V, temperature are cell reaction 1～5min under the condition of 0～50 DEG C at voltage; By the reacted negative electrode utmost pointPlate is clean with distilled water flushing, at room temperature natural drying, obtains nano-silver thread. Draw ratio can be prepared with this understanding largeIn 10, even more tiny nano-silver thread, thereby the nanoscale of controlled silver-colored line.
Preferred, comprise the following steps: get silver salt or argent-amine complex, add dissolution with solvents to obtain A liquid; Get organic matterMatter, adds dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid, be stirred to completely and dissolve; Add again complexing agent, stir allEven, stratification, obtains C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electricitySeparate liquid oil reservoir, slowly increase voltage from 0V, when being increased to 31.5V generation current, being controlled at voltage is that 31.5V, temperature areCell reaction 1～5min under the condition of 25 DEG C; Reacted cathode plate is clean with distilled water flushing, at room temperature naturally dryDry, obtain nano-silver thread. Can prepare with this understanding draw ratio and be greater than 10, even more tiny nano-silver thread, withTime this nano-silver thread stable appearance and pattern best.
In the preparation method of aforesaid nano-silver thread, described solvent is distilled water, methyl alcohol, ethanol, propyl alcohol, n-butanol, twoOne or more in the tertiary alcohol, thus can ensure that the pattern of nano-silver thread is controlled in the scope of 1～50nm.
In the preparation method of aforesaid nano-silver thread, described silver salt is one or more in soluble silver salt.
Preferably, described silver salt is one or more in silver nitrate, silver sulfate, silver carboxylate, thereby can effectively reduce productionCost.
In the preparation method of aforesaid nano-silver thread, described organic substance is one or more in organic amine; Or high-carbonOne or more in alcohols.
Preferably, described organic substance is one or more in dodecyl amine, tridecyl amine, tetradecylamine; Or positive fourthOne or both in alcohol, n-amyl alcohol. Adopt this organic substance can additional protective agent and reducing agent, and this organic substanceNon-toxic, with low cost.
The concentration (being the concentration of A liquid) of the silver salt described in the present invention is 0.1～10mol/L; The concentration of organic substance (The concentration of B liquid) be 0.1～10mol/L. Concentration difference, the nanoscale of the silver-colored line of preparation and pattern i.e. difference to some extent, andIn this concentration range, all can prepare desired nano-silver thread, if exceed this scope, nano-silver thread will be grown into silver soNanometer bulk product.
Preferably, the concentration of described silver salt is 0.5mol/L; The concentration of organic substance is 0.5mol/L.
A liquid described in the present invention mixes by injection device with B liquid, described injection device be syringe pump, buret,One or more in syringe needle, mixing rate is 0.1 μ l/min～100ml/min. Because mixing velocity directly affects Nano SilverThe pattern of line, mixing rate is too fast, and pattern is grown up wayward, and speed is too small, and production efficiency is lower, and adopts in the present inventionState after mixing rate, not only can make the pattern of nano-silver thread controlled, and production efficiency is also higher.
Preferably, described mixing rate is 1ml/min, thereby can make the pattern of nano-silver thread controlled, and simultaneously production efficiencyHigh.
In order to ensure effect of the present invention, the applicant has carried out series of experiments and has screened the preparation technology bar of Novel nanometer silver linePart, to ensure its science, reasonable, feasible. Conclusion is as follows:
First, when applied voltage is during lower than 1V, cannot there is cell reaction in corresponding electrolyte, and during higher than 50V, electrolysisToo fast, substantially can not get nano-silver thread; Only having the applied voltage of working as is 1～50V, can obtain nano-silver thread, and changes voltageCondition, the pattern that can control nano-silver thread is changed into bar-shaped by line style; In the time that applied voltage is 25～35V, can be prepared into lengthFootpath is than the nano-silver thread that is greater than 10; When increasing voltage from 0V, when being increased to 31.5V generation current, being controlled at voltage and beingWhen 31.5V, can prepare draw ratio and be greater than 10, even more tiny nano-silver thread, the pattern of this nano-silver thread is steady simultaneouslyFixed and pattern is best.
Secondly, with the prolongation of electrolysis time, the nano-silver thread of preparation is grown up, and specific area reduces to some extent, when the cell reaction timeWhile being less than 1min, the not moulding of nano-silver thread of preparation, in the time that the cell reaction time is greater than 30min, the complexion of nano-silver thread withoutChange, electrolysis completes substantially; Only have in the time that the cell reaction time is 1～30min, can prepare the controlled Nano Silver of patternLine; And in the time that the cell reaction time is 1～5min, can prepares draw ratio and be greater than 10, even more tiny Nano SilverLine, the stable appearance of this nano-silver thread and pattern are best simultaneously.
Again, the temperature of cell reaction is also the key factor that affects nano-silver thread effect, when cell reaction temperature is lower than 0 DEG CTime, cannot there is cell reaction; When cell reaction temperature is during higher than 50 DEG C, react too fast, and nano-silver thread is oxidized, goes outShow oxidation shape pattern; In addition, when temperature is higher than 50 DEG C, also can increase energy consumption and cost; And only have when cell reaction temperature be0～50 DEG C time, can prepare the controlled nano-silver thread of pattern, nano-silver thread non-oxidation shape pattern occurs simultaneously; And work as electrolysisWhen reaction temperature is 25 DEG C, can prepares draw ratio and be greater than 10, even more tiny nano-silver thread, simultaneously this Nano SilverStable appearance and the pattern of line are best, and also non-oxidation shape pattern occurs.
In addition, the impact of the pattern of the concentration of silver salt and organic substance on nano-silver thread is also comparatively remarkable, when silver salt and organic substanceConcentration while being greater than 10mol/L, reaction speed is too fast, easily forms fine granularity nanometer silver granuel; When silver salt and organic substanceConcentration while being less than 0.1mol/L, reacted slow, and the pattern of the nano-silver thread forming changes also little; When silver salt and organicWhen the concentration of material is 0.1～10mol/L, reaction speed is moderate, can prepare the controlled nano-silver thread of pattern; And work asWhen the concentration of silver salt and organic substance is 0.5mol/L, can prepares draw ratio and be greater than 10, even more tiny Nano SilverLine, the stable appearance of this nano-silver thread and pattern are best simultaneously.
Compared with prior art, thus the present invention by utilizing electric field can control easily thickness and the draw ratio of nano-silver thread,Realize the controllable growth to nanostructured, further, by adjusting voltage and the reaction time of electric field, thereby make to generateNano-silver thread pattern controlled, can be that nano-silver thread in a big way of 1～50nm, nanometer rods are synthetic by diameter, and thisBright preparation technology is simple, easy to operate, has greatly saved preparation cost, has improved the effect of synthesizing nano-silver line and nano-barRate. In addition, preparation method of the present invention does not need through high-temperature calcination or hydro-thermal reaction, does not need to add reduction protection agent, canUnder normal pressure, directly from solution, preparing diameter is the nano-silver thread that 10～30nm, draw ratio are greater than 10. In addition phase of the present invention,For template, can under normal temperature condition, prepare without the corresponding template of preparation the nano-silver thread that draw ratio is greater than 10,Also without carrying out high-temperature calcination, thereby avoid complicated post-processed process, kept high activity, and the Nano Silver of preparationLine duct is more, is evenly distributed; For existing preparation method, the present invention, without additional reducing agent, has simplified workSkill, can avoid the reunion of noble metal, make whole preparation process more easy to operate and control. With respect to wet chemistry method, institute of the present inventionThe concentration range of the silver salt adopting can reach 0.1～10mol/L; The concentration range of organic substance is 0.1～10mol/L, greatlyExpand the scope of solution concentration, and can deposit at normal temperatures nano-silver thread, and can be by controlling electrolysis time and pressure, in factExisting prepared nano-silver thread pattern is controlled.
Brief description of the drawings
Fig. 1 is the SEM figure that reacts the nano-silver thread after 1min in embodiment 1;
Fig. 2 is the SEM figure that reacts the nano-silver thread after 5min in embodiment 1;
Fig. 3 is the energy spectrogram of the nano-silver thread described in embodiment 1;
Fig. 4 is the silver ion complexation schematic diagram described in embodiment 1;
Fig. 5 is the SEM figure that reacts the nano-silver thread after 1min in embodiment 2;
Fig. 6 is the SEM figure that reacts the nano-silver thread after 5min in embodiment 2;
Fig. 7 is the SEM photo of the nano-Ag particles described in embodiment 3.
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
Detailed description of the invention
Embodiments of the invention 1: a kind of preparation method of nano-silver thread, comprises the following steps: get silver nitrate, be dissolved in distillationIn water, obtaining concentration is the A liquid of 0.5mol/L; Get dodecyl amine, be dissolved in ethanolic solution, obtaining concentration is 0.5mol/L'sB liquid; By syringe pump, A liquid is transferred in reactor and is mixed with B liquid, mixing rate is 1ml/min, stirs with glass barTo dissolving completely; Pipette in the distilled water that 1mL ammoniacal liquor is added to 88mL as complexing agent with liquid-transfering gun, this complexing agent is addedEnter in the mixed solution of A liquid and B liquid, stir with glass bar, stratification, obtains C liquid; Get C liquid as electrolysisLiquid, is inserted into anode the water layer of electrolyte, and negative electrode is inserted into the oil reservoir of electrolyte; Slowly increase voltage from 0V, work as increaseTo 31.5V generation current, be controlled at voltage and be 31.5V, temperature and be cell reaction 1～5min under the condition of 25 DEG C; To reactAfter cathode plate clean with distilled water flushing, natural drying under room temperature, obtain nano-silver thread. SEM shows to react after 1minProduct pattern is that diameter is about the nano wire that 10nm, length are 500nm, as shown in Figure 1. Reaction 5min afterproduct shapeLooks are that diameter is about the nano wire that 20nm, length are 300nm, as shown in Figure 2. Can spectrogram as shown in Figure 3, silver ionComplexing schematic diagram as shown in Figure 4.
Embodiment 2: a kind of preparation method of nano-silver thread, comprises the following steps: take 1.02g silver nitrate, be dissolved in 10mlAbsolute ethyl alcohol in, obtain A liquid (concentration is 6mol/L); Take in the ethanolic solution that 5g dodecyl amine is dissolved in 30mL,B liquid (concentration is 0.9mol/L); By buret, A liquid is transferred in reactor and is mixed with B liquid, mixing rate is100ml/min, is stirred to completely and dissolves with glass bar; Pipette in the distilled water that 1mL ethylenediamine joins 80mL with liquid-transfering gunAs complexing agent, this complexing agent is added in the mixed solution of A liquid and B liquid, stir with glass bar, stratification,Obtain C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into the oil reservoir of electrolyte; ?Voltage is that 30V, temperature are cell reaction 1～5min under the condition of 50 DEG C; Reacted cathode plate is dry with distilled water flushingOnly, natural drying under room temperature, obtain nano-silver thread. SEM shows: reaction 1min afterproduct pattern is diameter 10nm, lengthThe nano wire of degree 200nm, as shown in Figure 5, reaction 5min afterproduct pattern is receiving of diameter 20nm, length 100nmRice noodles, as shown in Figure 6.
Embodiment 3: a kind of preparation method of nano-silver thread, comprises the following steps: take 2.10g silver nitrate, be dissolved in 30mlAbsolute ethyl alcohol in, obtain A liquid (concentration is 0.4mol/L); Take the ethanolic solution that 10g dodecyl amine is dissolved in 50mLIn, obtain B liquid (concentration is 1.1mol/L); By syringe needle, A liquid is transferred in reactor and is mixed with B liquid, mixing rate is0.1 μ l/min, is stirred to completely and dissolves with glass bar; Pipette in the distilled water that 1ml salicylide joins 20mL with liquid-transfering gunAs complexing agent, this complexing agent is added in the mixed solution of A liquid and B liquid, stir with glass bar, stratification,Obtain C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into the oil reservoir of electrolyte; ?Voltage is that 25V, temperature are cell reaction 5min under the condition of 25 DEG C; Reacted cathode plate is dry with distilled water flushingOnly, natural drying under room temperature, obtain nano-silver thread. SEM shows: reaction 5min afterproduct pattern is receiving of diameter 20nmRice grain, as shown in Figure 7.
Can be found out by embodiment 1～embodiment 3: under the condition of embodiment 1, can prepare draw ratio and be greater than 10 receiveThe silver-colored line of rice, and can find out from the scanning electron microscope (SEM) photograph of Fig. 1, the nano-silver thread of preparation is tiny evenly, and morphology characterization is complete, nanometerIn silver line, specific area and the larger hole of relative appropriateness are there is, the nano-silver thread that visible the present invention is prepared with respect to prior art, all have at aspect product pattern and functional aspect significantly and promote. In addition, along with decomposition voltage and concentration of electrolyteChange (being that decomposition voltage and the concentration of electrolyte numerical value in embodiment 1 becomes the numerical value in embodiment 2), can make preparationNano-silver thread is grown along crystal face, and pattern good evenness, and the direction of growth is controlled, as shown in Figure 2. And with respect to embodiment 2With the condition in embodiment 3, the specific area of the nano-silver thread that embodiment 1 prepares and relevant hole maximum, major diameterThan also maximum, nano-silver thread is the most tiny evenly simultaneously, and therefore, the preparation condition in the embodiment of the present invention 1 is optimum.
Embodiment 4: a kind of preparation method of nano-silver thread, comprises the following steps: get silver carboxylate, add methyl alcohol to dissolve to obtain concentrationFor the A liquid of 0.1mol/L; Get tetradecylamine, add propyl alcohol to dissolve to obtain the concentration B liquid that is 0.2mol/L; By A liquid and BLiquid mixes, and is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electricitySeparate liquid, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, electrolysis under the condition that is 35V at voltageReaction 3min; Reacted cathode plate is clean with distilled water flushing, at room temperature natural drying, obtain nano-silver thread.
Embodiment 5: a kind of preparation method of nano-silver thread, comprises the following steps: get silver sulfate, add n-butanol to dissolve denselyDegree is the A liquid of 1mol/L; Get tridecyl amine, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 2mol/L; By A liquid and BLiquid mixes, and mixing rate is 10ml/min, is stirred to completely and dissolves; Add again complexing agent, stir, stratification,C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, at voltage isCell reaction 5～30min under the condition of 15V; Reacted cathode plate is clean with distilled water flushing, at room temperature natureDry, obtain nano-silver thread.
Embodiment 6: a kind of preparation method of nano-silver thread, comprises the following steps: get argent-amine complex, add butanols to dissolveA liquid; Get tridecyl amine, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 5mol/L; A liquid is mixed with B liquid, mix speedRate is 50ml/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquidAs electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, the condition that is 25V at voltageLower cell reaction 7min; Reacted cathode plate is clean with distilled water flushing, at room temperature natural drying, obtain nanometerSilver line.
Embodiment 7: a kind of preparation method of nano-silver thread, comprises the following steps: get silver sulfate, add n-butanol to dissolve denselyDegree is the A liquid of 10mol/L; Get n-butanol, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 10mol/L; By A liquid and BLiquid mixes, and mixing rate is 80ml/min, is stirred to completely and dissolves; Add again complexing agent, stir, stratification,C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, at voltage isCell reaction 1min under the condition of 50V; Reacted cathode plate is clean with distilled water flushing, at room temperature naturally dryDry, obtain nano-silver thread.
Embodiment 8: a kind of preparation method of nano-silver thread, comprises the following steps: get silver sulfate, add n-butanol to dissolve denselyDegree is the A liquid of 0.5mol/L; Get n-amyl alcohol, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 0.5mol/L; By A liquid and BLiquid mixes, and mixing rate is 1ml/min, is stirred to completely and dissolves; Add again complexing agent, stir, stratification,C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electrolyte oil reservoir, at voltage isCell reaction 5min under the condition of 31.5V; Reacted cathode plate is clean with distilled water flushing, at room temperature naturally dryDry, obtain nano-silver thread.
Embodiment 9: a kind of preparation method of nano-silver thread, comprises the following steps: get silver sulfate, add n-butanol to dissolve denselyDegree is the A liquid of 0.5mol/L; Get tridecyl amine and tetradecylamine, add two tertiary alcohols to dissolve to obtain the concentration B that is 0.1mol/LLiquid; A liquid is mixed with B liquid, and mixing rate is 10 μ l/min, is stirred to completely and dissolves; Add again complexing agent, stir allEven, stratification, obtains C liquid; Get C liquid as electrolyte, anode is inserted into the water layer of electrolyte, negative electrode is inserted into electricitySeparating liquid oil reservoir, is that 1V, temperature are cell reaction 30min under the condition of 0 DEG C at voltage; By distillation for reacted cathode plateWater is rinsed well, at room temperature natural drying, obtains nano-silver thread.
The nano particle pattern of mentioning in the present invention is particle, is now than the pattern that is easier to realize; Nano wire and nanometer rodsThe main distinction be draw ratio difference, the basic pattern of the nano-silver thread that the inventive method is produced can be grown to by hair shape littleThe bar-shaped granule that even becomes, nano-silver thread pattern prepared by this kind of complexing method, for forefathers do not prepare, is a kind of completeNew complexing method.
Claims (6)
1. a preparation method for nano-silver thread, is characterized in that, comprises the following steps: get silver salt or argent-amine complex, add moltenA liquid is dissolved to obtain in agent; Get organic substance, add dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid, be stirred to completely moltenSeparate; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolyte, anode is inserted into electricitySeparate the water layer of liquid, negative electrode is inserted into the oil reservoir of electrolyte, is that 1～50V, temperature are electrolysis under the condition of 0～50 DEG C at voltageReaction 1～30min; Reacted cathode plate is clean with distilled water flushing, at room temperature natural drying, obtain Nano SilverLine; Described solvent is one or more in distilled water, methyl alcohol, ethanol, propyl alcohol, n-butanol, two tertiary alcohols; Silver salt is canOne or more in dissolubility silver salt; Organic substance is one or more in dodecyl amine, tridecyl amine, tetradecylamine; OrOne or both in person's n-butanol, n-amyl alcohol; Complexing agent is added in distilled water and is obtained by ammoniacal liquor, ethylenediamine or salicylide; InstituteThe concentration of the silver salt of stating is 0.1～10mol/L; The concentration of organic substance is 0.1～10mol/L; Described A liquid and B liquidMixing rate is 0.1 μ l/min～100ml/min.
2. the preparation method of nano-silver thread according to claim 1, is characterized in that, comprises the following steps: get silver salt or silver-colored amineComplex compound, adds dissolution with solvents to obtain A liquid; Get organic substance, add dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid,Be stirred to completely and dissolve; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolyte, willAnode is inserted into the water layer of electrolyte, and negative electrode is inserted into electrolyte oil reservoir, is that 25～35V, temperature are 0～50 DEG C at voltageCell reaction 1～5min under condition; Reacted cathode plate is clean with distilled water flushing, at room temperature natural drying,Obtain nano-silver thread.
3. the preparation method of nano-silver thread according to claim 2, is characterized in that, comprises the following steps: get silver salt or silver-colored amineComplex compound, adds dissolution with solvents to obtain A liquid; Get organic substance, add dissolution with solvents to obtain B liquid; A liquid is mixed with B liquid,Be stirred to completely and dissolve; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolyte, willAnode is inserted into the water layer of electrolyte, and negative electrode is inserted into electrolyte oil reservoir, increases voltage from 0V, produces when being increased to 31.5VElectric current, is controlled at voltage and is 31.5V, temperature and be cell reaction 1～5min under the condition of 25 DEG C; By reacted cathode plateClean with distilled water flushing, at room temperature natural drying, obtain nano-silver thread.
4. the preparation method of nano-silver thread according to claim 1, is characterized in that, the concentration of described silver salt is0.5mol/L; The concentration of organic substance is 0.5mol/L.
5. the preparation method of nano-silver thread according to claim 1, is characterized in that, described A liquid and B liquid are by injectionDevice mixes, and described injection device is one or more in syringe pump, buret, syringe needle.
6. the preparation method of nano-silver thread according to claim 1, is characterized in that, mixing rate is 1ml/min.
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| CN105734613B (en) * | 2016-05-06 | 2018-01-16 | 上海应用技术学院 | A kind of method that liquid electrodeposition prepares nano-silver thread |
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| CN101314860A (en) * | 2008-07-14 | 2008-12-03 | 苏州大学 | Method for producing nano-silver powder or nano-gold powder |
| CN102267682A (en) * | 2010-06-03 | 2011-12-07 | 中国科学院合肥物质科学研究院 | Silver nanowire array electrode, preparation method and application thereof |
| CN102803128A (en) * | 2009-06-15 | 2012-11-28 | 阿莫绿色技术有限公司 | Method and apparatus for producing nano-sized silver particles using electrolysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101314860A (en) * | 2008-07-14 | 2008-12-03 | 苏州大学 | Method for producing nano-silver powder or nano-gold powder |
| CN102803128A (en) * | 2009-06-15 | 2012-11-28 | 阿莫绿色技术有限公司 | Method and apparatus for producing nano-sized silver particles using electrolysis |
| CN102267682A (en) * | 2010-06-03 | 2011-12-07 | 中国科学院合肥物质科学研究院 | Silver nanowire array electrode, preparation method and application thereof |
Non-Patent Citations (3)
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| Aqueous-Organic Phase-Transfer of Highly Stable Gold，Silver，and Platinum Nanoparticles and New Route for Fabrication of Gold Nanofilm at the Oil/Water Interface and on Solid Supports;Xingli Feng et al;《J.Phys.Chem.B》;20060606;第12311-12317页 * |
| Preparation of silver nanorods by electrochemical methods;Jun-Jie Zhu et al;《Materials Letters》;20010630;第91-95页 * |
| 银纳米材料的可控合成研究;张万忠 等;《稀有金属材料与工程》;20081115;第37卷(第11期);第2059-2064页 * |
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