CN104018189A - Preparation method for novel nano-silver wire - Google Patents
Preparation method for novel nano-silver wire Download PDFInfo
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- CN104018189A CN104018189A CN201410247264.7A CN201410247264A CN104018189A CN 104018189 A CN104018189 A CN 104018189A CN 201410247264 A CN201410247264 A CN 201410247264A CN 104018189 A CN104018189 A CN 104018189A
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Abstract
The invention discloses a preparation method for a novel nano-silver wire. The preparation method comprises the following steps: taking a sliver salt or silver amide complex, adding a solvent for dissolving to obtain liquor A; taking organic substances, adding the solvent for dissolving to obtain liquor B; mixing the liquor A with the liquor B, stirring until dissolving completely; adding a complexing agent, uniformly stirring, stewing and layering to obtain liquor C; taking the liquor C as an electrolyte, inserting an anode to a water layer of the electrolyte, inserting a cathode to an oil layer of the electrolyte, carrying out electrolytic reaction for 1-30 minutes under the condition that voltage is 1-50V; flushing the reacted cathode polar plate by distilled water, naturally drying at the room temperature to obtain the nano-silver wire. The thickness and slenderness ratio of the nano-silver wire can be conveniently controlled by electric fields, so that the controllable growth of a nano structure is realized; morphology of the generated nano-sliver wire is controllable by regulating the current density, voltage and reaction time, and the novel nano-silver wire can be synthesized by a nano-silver wire with the diameter of 1-50nm and a nano rod. The preparation process is simple and low in cost, and efficiency for synthesizing the nano-sliver wire and the nano rod is higher.
Description
Technical field
The present invention relates to a kind of novel preparation technology of nano-noble metal structure, particularly a kind of preparation method of Novel nanometer silver line.
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.At present, the type material being comprised of nanoparticle is widely applied in fields such as catalysis, luminescent material, magneticsubstance, semiconductor material and fine ceramics materials.Nanometer silver is as the important component part of noble metal nanometer material, except possessing the character such as surface effects, quantum size effect, volume effect and macro quanta tunnel effect of common metal nano material, also there is special surface plasma resonance effect, therefore, nanometer 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 have broad application prospects in nanometer circuit.By the supporting capacity of the resistance of nano silver wire and electric current is carried out to systematic study, found that diameter is that 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; mainly be divided into Physical and the large class of chemical method two; wherein chemical method, because thereby the advantages such as its technique is simple, economic, low for equipment requirements, easy mass-producing are able to fast development, generally can be divided into chemical method following a few class: template, wet chemistry method and polyvalent alcohol method substantially.
(1) template: refer to based on additional template, a kind of method that nano material backed stamper plate hole road is prepared by nano pore restriction, first the method needs to prepare as requested corresponding template in preparation process, as polymer template, alumina formwork, biomolecules (as protein dna) template etc., also need to carry out high-temperature calcination, and to carry out complicated post-processed, thereby nano-silver thread complex process, cost prepared by this method are higher, and the activity of nano-silver thread is lower, poor growth, pore distribution is inhomogeneous.
(2) wet chemistry method: the general name that is many different chemical processes; its common feature is that reaction system is liquid phase (mostly being water); adopt organism or mineral ion as stablizer or inductor; conventionally also there is reductive agent; its critical process is the reduction reaction initial stage; stablizer just Already in system, plays restriction inhibition to the metal cluster in growth.This method is general only reacts in extremely dilute solution, and concentration improves just need to add stablizer; Owing to take redox reaction in reaction process as main, thereby nanometer product sedimentation velocity is very fast, and deposition does not have directivity (generally take spherical or block product as main).
(3) polyvalent alcohol method: be a kind of of wet chemistry method, but due to its unique advantage in preparing metal nano material, in at present known method, the pattern of the metal nano material that it obtains is the abundantest, but also can be widely used in different metals, therefore cause various places researchist's very big interest.Because the solvent the most often using in polyvalent alcohol method is ethylene glycol, its specific inductivity is higher, except can dissolving plurality of inorganic salt, can also dissolve part polymer (as polyvinylpyrrolidone, PVP), thereby many study group all introduce PVP in polyvalent alcohol method as stablizer and inductor, metal-salt is presoma, by adjusting, is reacted and is prepared metal nano material.The method needs additional protective material and reductive agent, and the nano-metal particle pattern of preparation is larger.
Although above-mentioned several method can be prepared nano silver powder, but it all can not realize the effective control to nanostructure, such as size, club-shaped material pattern etc., and some methods need to be carried out high temperature sintering or be reacted under hydrothermal condition, thereby have greatly increased preparation cost and difficulty.
Summary of the invention
The object of the invention is to, a kind of preparation method of Novel nanometer silver line is provided, it can effectively solve problems of the prior art, especially complex process, cost higher, can not realize the problem to effective control of nanostructure.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of preparation method of Novel nanometer silver line, comprises 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 complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 1～30min under the condition that is 1～50V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains 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 complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, at voltage, is that 25～35V, temperature are electrolytic reaction 1～5min under the condition of 0～50 ℃; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.Can prepare with this understanding length-to-diameter ratio and be greater than 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 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 electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, from 0V, slowly increases voltage, when being increased to 31.5V generation current, is controlled at voltage and is 31.5V, temperature and be electrolytic reaction 1～5min under the condition of 25 ℃; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.Can prepare with this understanding length-to-diameter ratio and be greater than 10, even more tiny nano-silver thread, the stable appearance of this nano-silver thread and pattern are best simultaneously.
In the preparation method of aforesaid Novel nanometer silver line, described solvent is one or more in distilled water, methyl alcohol, ethanol, propyl alcohol, propyl carbinol, two tertiary alcohols, thereby the morphology control that can guarantee nano-silver thread is in the scope of 1～50nm.
In the preparation method of aforesaid Novel nanometer silver line, described silver salt is one or more in soluble silver salt.
Preferably, described silver salt is one or more in Silver Nitrate, Sulfuric acid disilver salt, silver carboxylate, thereby can effectively reduce production costs.
In the preparation method of aforesaid Novel nanometer silver line, described organic substance is one or more in organic amine; Or one or more in high-carbon alcohols.
Preferably, described organic substance is one or more in n-Laurylamine, tridecyl amine, tetradecylamine; Or one or both in propyl carbinol, Pentyl alcohol.Adopt this organic substance can additional protective material and reductive agent, and this organic substance nontoxicity, with low cost.
The concentration of the silver salt described in the present invention (being the concentration of A liquid) is 0.1～10mol/L; The concentration of organic substance (being the concentration of B liquid) is 0.1～10mol/L.Concentration is different, and the nanoscale of the silver-colored line of preparation and pattern i.e. difference to some extent, and in this concentration range, all can prepare desired nano-silver thread, if surpass this scope, nano-silver thread will be grown into silver nanoparticle bulk product so.
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, and described injection device is one or more in syringe pump, drop-burette, syringe needle, and mixing rate is 0.1 μ l/min～100ml/min.Because mixing velocity directly affects the pattern of nano-silver thread, mixing rate is too fast, and pattern is grown up wayward, speed is too small, and production efficiency is lower, and adopts after the above-mentioned mixing rate of the present invention, 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 production efficiency is the highest simultaneously.
In order to ensure effect of the present invention, the applicant has carried out the preparation process condition that series of experiments screens Novel nanometer silver line, guaranteeing its science, reasonable, feasible.Conclusion is as follows:
First, when impressed voltage is during lower than 1V, cannot there is electrolytic reaction in corresponding electrolytic solution, and during higher than 50V, electrolysis is too fast, substantially can not get nano-silver thread; Only having the impressed voltage of working as is 1～50V, can obtain nano-silver thread, and changes voltage conditions, and the pattern that can control nano-silver thread is changed into bar-shaped by line style; When impressed voltage is 25～35V, can be prepared into the nano-silver thread that length-to-diameter ratio is greater than 10; When increasing voltage from 0V, when being increased to 31.5V generation current, when being controlled at voltage and being 31.5V, can preparing length-to-diameter ratio and be greater than 10, even more tiny nano-silver thread, the stable appearance of this nano-silver thread and pattern are best simultaneously.
Secondly, with the prolongation of electrolysis time, the nano-silver thread of preparation is grown up, specific surface area reduces to some extent, when the electrolytic reaction time is less than 1min, and the not moulding of nano-silver thread of preparation, when the electrolytic reaction time is greater than 30min, the complexion of nano-silver thread is without change, and electrolysis completes substantially; Only have when the electrolytic reaction time is 1～30min, can prepare the controlled nano-silver thread of pattern; And when the electrolytic reaction time is 1～5min, can prepares length-to-diameter ratio and be greater than 10, even more tiny nano-silver thread, the stable appearance of this nano-silver thread and pattern are best simultaneously.
Again, the temperature of electrolytic reaction is also the important factor that affects nano-silver thread effect, when electrolytic reaction temperature is during lower than 0 ℃, electrolytic reaction cannot occur; When electrolytic reaction temperature is during higher than 50 ℃, react too fast, and nano-silver thread is oxidized, there is oxidation shape pattern; When in addition, temperature is higher than 50 ℃, also can increase energy consumption and cost; And only have when electrolytic reaction temperature is 0～50 ℃, can prepare the controlled nano-silver thread of pattern, nano-silver thread non-oxidation shape pattern occurs simultaneously; And when electrolytic reaction temperature is 25 ℃, can prepares length-to-diameter ratio and be greater than 10, even more tiny nano-silver thread, the stable appearance of this nano-silver thread and pattern are best simultaneously, and also non-oxidation shape pattern occurs.
In addition, the concentration of silver salt and organic substance is also comparatively remarkable on the impact of the pattern of nano-silver thread, and when the concentration of silver salt and organic substance is greater than 10mol/L, speed of response is too fast, easily forms fine granularity nanometer silver granuel; When the concentration of silver salt and organic substance is less than 0.1mol/L, reacted slow, and the morphology change of the nano-silver thread forming is also little; When the concentration of silver salt and organic substance is 0.1～10mol/L, speed of response is moderate, can prepare the controlled nano-silver thread of pattern; And when the concentration of silver salt and organic substance is 0.5mol/L, can prepares length-to-diameter ratio and be greater than 10, even more tiny nano-silver thread, the stable appearance of this nano-silver thread and pattern are best simultaneously.
Compared with prior art, thereby the present invention is by utilizing electric field can control easily thickness and the length-to-diameter ratio of nano-silver thread, the controllable growth of realization to nanostructure, further, by adjusting voltage and the reaction times of electric field, thereby make the nano-silver thread pattern of generation controlled, can be that 1～50nm nano-silver thread, nanometer rod is in a big way synthetic by diameter, and preparation technology of the present invention is simple, easy to operate, greatly save preparation cost, improved the efficiency of synthesizing nano-silver line and nano-bar.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, and can under normal pressure, directly from solution, prepare diameter is the nano-silver thread that 10～30nm, length-to-diameter ratio are greater than 10.In addition, the present invention is for template, without the corresponding template of preparation, can under normal temperature condition, prepare the nano-silver thread that length-to-diameter ratio is greater than 10, also without carrying out high-temperature calcination, thereby avoided complicated post-processed process, kept high reactivity, and the nano-silver thread duct of preparation is more, is evenly distributed; For existing preparation method, the present invention, without additional reducing agent, has simplified technique, can avoid the reunion of precious metal, makes whole preparation process more easy to operate and control.With respect to wet chemistry method, the concentration range of silver salt of the present invention can reach 0.1～10mol/L; The concentration range of organic substance is 0.1～10mol/L, has greatly expanded the scope of strength of solution, and can deposit at normal temperatures nano-silver thread, and can, by controlling electrolysis time and pressure, realize prepared nano-silver thread pattern controlled.
Accompanying drawing explanation
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.
Embodiment
Embodiments of the invention 1: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get Silver Nitrate, be dissolved in distilled water, obtaining concentration is the A liquid of 0.5mol/L; Get n-Laurylamine, be dissolved in ethanolic soln, obtaining concentration is the B liquid of 0.5mol/L; By syringe pump, A liquid is transferred in reactor and is mixed with B liquid, mixing rate is 1ml/min, with glass stick, is stirred to completely and dissolves; With liquid-transfering gun, pipette in the distilled water that 1mL ammoniacal liquor is added to 88mL as complexing agent, this complexing agent is added in the mixing solutions of A liquid and B liquid, with glass stick, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into the oil reservoir of electrolytic solution; From 0V, slowly increase voltage, when being increased to 31.5V generation current, be controlled at voltage and be 31.5V, temperature and be electrolytic reaction 1～5min under the condition of 25 ℃; Reacted cathode plate is clean with distilled water flushing, and seasoning under room temperature, obtains nano-silver thread.It is that diameter is about the nano wire that 10nm, length are 500nm that SEM shows to react 1min after product pattern, as shown in Figure 1.Reaction 5min after product pattern is that diameter is about the nano wire that 20nm, length are 300nm, as shown in Figure 2.As shown in Figure 3, silver ion complexation schematic diagram as shown in Figure 4 for energy spectrogram.
Embodiment 2: a kind of preparation method of Novel nanometer silver line, comprises the following steps: take 1.02g Silver Nitrate, be dissolved in the dehydrated alcohol of 10ml, obtain A liquid (concentration is 6mol/L); Take in the ethanolic soln that 5g n-Laurylamine is dissolved in 30mL, obtain B liquid (concentration is 0.9mol/L); By drop-burette, A liquid is transferred in reactor and is mixed with B liquid, mixing rate is 100ml/min, with glass stick, is stirred to completely and dissolves; With liquid-transfering gun, pipette in the distilled water that 1mL quadrol joins 80mL as complexing agent, this complexing agent is added in the mixing solutions of A liquid and B liquid, with glass stick, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into the oil reservoir of electrolytic solution; At voltage, be that 30V, temperature are electrolytic reaction 1～5min under the condition of 50 ℃; Reacted cathode plate is clean with distilled water flushing, and seasoning under room temperature, obtains nano-silver thread.SEM shows: reaction 1min after product pattern is the nano wire of diameter 10nm, length 200nm, and as shown in Figure 5, reaction 5min after product pattern is the nano wire of diameter 20nm, length 100nm, as shown in Figure 6.
Embodiment 3: a kind of preparation method of Novel nanometer silver line, comprises the following steps: take 2.10g Silver Nitrate, be dissolved in the dehydrated alcohol of 30ml, obtain A liquid (concentration is 0.4mol/L); Take in the ethanolic soln that 10g n-Laurylamine is dissolved in 50mL, 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 is 0.1 μ l/min, with glass stick, is stirred to completely and dissolves; With liquid-transfering gun, pipette in the distilled water that 1ml salicylic aldehyde joins 20mL as complexing agent, this complexing agent is added in the mixing solutions of A liquid and B liquid, with glass stick, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into the oil reservoir of electrolytic solution; At voltage, be that 25V, temperature are electrolytic reaction 5min under the condition of 25 ℃; Reacted cathode plate is clean with distilled water flushing, and seasoning under room temperature, obtains nano-silver thread.SEM shows: reaction 5min after product pattern is the nano particle of diameter 20nm, as shown in Figure 7.
By embodiment 1～embodiment 3, can be found out: under the condition of embodiment 1, can prepare the nano-silver thread that length-to-diameter ratio is greater than 10, and can find out from the scanning electron microscope (SEM) photograph of Fig. 1, the nano-silver thread of preparation is tiny evenly, morphology characterization is complete, in nano-silver thread, there is specific surface area and the larger hole of relative appropriateness, for the nano-silver thread that visible the present invention is prepared with respect to prior art, at aspect product pattern and functional aspect, all had significantly and promote.In addition, along with the change (being that electrolysis voltage and the concentration of electrolyte numerical value in embodiment 1 becomes the numerical value in embodiment 2) of electrolysis voltage and concentration of electrolyte, can make the nano-silver thread of preparation grow along crystal face, and pattern good evenness, the direction of growth is controlled, as shown in Figure 2.And for the condition in embodiment 2 and embodiment 3, the specific surface area of the nano-silver thread that embodiment 1 prepares and relevant hole are maximum, and length-to-diameter ratio is also maximum, and nano-silver thread is the most tiny evenly simultaneously, therefore, the preparation condition in the embodiment of the present invention 1 is optimum.
Embodiment 4: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get silver carboxylate, add dissolve with methanol to obtain the A liquid that concentration is 0.1mol/L; Get tetradecylamine, add propyl alcohol to dissolve to obtain the concentration B liquid that is 0.2mol/L; 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 electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 3min under the condition that is 35V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
Embodiment 5: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get Sulfuric acid disilver salt, add propyl carbinol to dissolve to obtain the concentration A liquid that is 1mol/L; Get tridecyl amine, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 2mol/L; A liquid is mixed with B liquid, and mixing rate is 10ml/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 5～30min under the condition that is 15V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
Embodiment 6: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get argent-amine complex, add butanols to dissolve to obtain A 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, and mixing rate is 50ml/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 7min under the condition that is 25V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
Embodiment 7: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get Sulfuric acid disilver salt, add propyl carbinol to dissolve to obtain the concentration A liquid that is 10mol/L; Get propyl carbinol, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 10mol/L; A liquid is mixed with B liquid, and mixing rate is 80ml/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 1min under the condition that is 50V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
Embodiment 8: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get Sulfuric acid disilver salt, add propyl carbinol to dissolve to obtain the concentration A liquid that is 0.5mol/L; Get Pentyl alcohol, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 0.5mol/L; A liquid is mixed with B liquid, and mixing rate is 1ml/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, electrolytic reaction 5min under the condition that is 31.5V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
Embodiment 9: a kind of preparation method of Novel nanometer silver line, comprises the following steps: get Sulfuric acid disilver salt, add propyl carbinol to dissolve to obtain the concentration A liquid that is 0.5mol/L; Get tridecyl amine and tetradecylamine, add two tertiary alcohols to dissolve to obtain the concentration B liquid that is 0.1mol/L; A liquid is mixed with B liquid, and mixing rate is 10 μ l/min, is stirred to completely and dissolves; Add complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, at voltage, is that 1V, temperature are electrolytic reaction 30min under the condition of 0 ℃; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, 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; The key distinction of nano wire and nanometer rod is that length-to-diameter ratio is different, the basic pattern of the nano-silver thread that the inventive method is produced can be grown to the little bar-shaped small-particle that even becomes by hair shape, nano-silver thread pattern prepared by this kind of complexing method does not prepare for forefathers, is a kind of brand-new complexing method.
Claims (10)
1. a preparation method for Novel nanometer silver line, is characterized in that, comprises 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 complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into the oil reservoir of electrolytic solution, electrolytic reaction 1～30min under the condition that is 1～50V at voltage; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
2. the preparation method of Novel nanometer silver line according to claim 1, is characterized in that, comprises 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 complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, at voltage, is that 25～35V, temperature are electrolytic reaction 1～5min under the condition of 0～50 ℃; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
3. the preparation method of Novel nanometer silver line according to claim 2, is characterized in that, comprises 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 complexing agent again, stir, stratification, obtains C liquid; Get C liquid as electrolytic solution, anode is inserted into the water layer of electrolytic solution, negative electrode is inserted into electrolytic solution oil reservoir, from 0V, increases voltage, when being increased to 31.5V generation current, is controlled at voltage and is 31.5V, temperature and be electrolytic reaction 1～5min under the condition of 25 ℃; Reacted cathode plate is clean with distilled water flushing, and at room temperature seasoning, obtains nano-silver thread.
4. according to the preparation method of arbitrary described Novel nanometer silver line in claim 1～3, it is characterized in that, described solvent is one or more in distilled water, methyl alcohol, ethanol, propyl alcohol, propyl carbinol, two tertiary alcohols.
5. the preparation method of Novel nanometer silver line according to claim 4, is characterized in that, described silver salt is one or more in soluble silver salt.
6. the preparation method of Novel nanometer silver line according to claim 5, is characterized in that, described organic substance is one or more in organic amine; Or one or more in high-carbon alcohols.
7. according to the preparation method of arbitrary described Novel nanometer silver line in claim 1～3, it is characterized in that, the concentration of described silver salt is 0.1～10mol/L; The concentration of organic substance is 0.1～10mol/L.
8. the preparation method of Novel nanometer silver line according to claim 7, is characterized in that, the concentration of described silver salt is 0.5mol/L; The concentration of organic substance is 0.5mol/L.
9. the preparation method of Novel nanometer silver line according to claim 7, it is characterized in that, described A liquid mixes by injection device with B liquid, and described injection device is one or more in syringe pump, drop-burette, syringe needle, and mixing rate is 0.1 μ l/min～100ml/min.
10. the preparation method of Novel nanometer silver line according to claim 9, is characterized in that, mixing rate is 1ml/min.
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| CN106623977A (en) * | 2016-12-30 | 2017-05-10 | 西安交通大学青岛研究院 | Preparation method of gold nanowire |
| CN106825601A (en) * | 2016-12-30 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of preparation method of nano silver wire |
| CN106975754A (en) * | 2016-12-30 | 2017-07-25 | 西安交通大学青岛研究院 | A kind of preparation method of palladium nanometer wire |
| EP4180152A4 (en) * | 2020-07-08 | 2024-01-10 | Mitsui Mining & Smelting Co Ltd | Fine metal linear body |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2013234341A (en) * | 2012-05-07 | 2013-11-21 | Univ Of Shiga Prefecture | Method for producing silver nanowire, and the silver nanowire |
-
2014
- 2014-06-05 CN CN201410247264.7A patent/CN104018189B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2013234341A (en) * | 2012-05-07 | 2013-11-21 | Univ Of Shiga Prefecture | Method for producing silver nanowire, and the silver nanowire |
Non-Patent Citations (3)
| Title |
|---|
| JUN-JIE ZHU ET AL: "Preparation of silver nanorods by electrochemical methods", 《MATERIALS LETTERS》 * |
| XINGLI FENG ET AL: "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", 《J.PHYS.CHEM.B》 * |
| 张万忠 等: "银纳米材料的可控合成研究", 《稀有金属材料与工程》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105618787A (en) * | 2016-01-27 | 2016-06-01 | 东莞理工学院 | Preparation method of hydrophobic silver nanoparticles |
| CN105734613A (en) * | 2016-05-06 | 2016-07-06 | 上海应用技术学院 | Method for preparing nano silver wires by liquid phase electrodeposition |
| CN105908220A (en) * | 2016-05-06 | 2016-08-31 | 上海应用技术学院 | Method for manufacturing micro-nano-silver dendritic crystal through liquid-phase electrodeposition |
| 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 |
| CN105908220B (en) * | 2016-05-06 | 2018-03-30 | 上海应用技术学院 | A kind of method that liquid electrodeposition prepares micro-nano silver dendrite |
| CN106623977A (en) * | 2016-12-30 | 2017-05-10 | 西安交通大学青岛研究院 | Preparation method of gold nanowire |
| CN106825601A (en) * | 2016-12-30 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of preparation method of nano silver wire |
| CN106975754A (en) * | 2016-12-30 | 2017-07-25 | 西安交通大学青岛研究院 | A kind of preparation method of palladium nanometer wire |
| CN106623977B (en) * | 2016-12-30 | 2018-07-10 | 西安交通大学青岛研究院 | A kind of preparation method of nanowires of gold |
| CN106975754B (en) * | 2016-12-30 | 2019-08-30 | 杭州罗松贸易有限公司 | A kind of preparation method of palladium nanometer wire |
| EP4180152A4 (en) * | 2020-07-08 | 2024-01-10 | Mitsui Mining & Smelting Co Ltd | Fine metal linear body |
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