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CN102502820B - One-dimensional and composite morphology Sb2O3 micro-nano powders prepared by one-step method - Google Patents

One-dimensional and composite morphology Sb2O3 micro-nano powders prepared by one-step method Download PDF

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CN102502820B
CN102502820B CN201110391114XA CN201110391114A CN102502820B CN 102502820 B CN102502820 B CN 102502820B CN 201110391114X A CN201110391114X A CN 201110391114XA CN 201110391114 A CN201110391114 A CN 201110391114A CN 102502820 B CN102502820 B CN 102502820B
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CN102502820A (en
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李宾杰
徐翔民
李志伟
赵彦保
张治军
吴志申
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Henan University
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Abstract

The invention belongs to the technical field of preparation of micro-nanometer materials, and particularly relates to a one-step method for preparing one-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder. Liquor with SbCl3 soluble in ethanol is added into alkali liquor to realize reaction, and one-dimensional Sb203 micro-nanometer powder and composite-morphological Sb203 micro-nanometer powder are obtained by means of filtering and drying. The method is simple, time-saving and labor-saving, is low in cost and environmental pollution, and saves energy, optional additives are omitted in a preparation procedure, and the one-step method has high industrial application potential.

Description

Single stage method prepares one dimension and compound pattern Sb thereof 2o 3micro-nano powder
Technical field
The invention belongs to technical field of micro nano material preparation, particularly a kind of single stage method prepares one dimension and compound pattern Sb thereof 2o 3the method of micro-nano powder.
Background technology
Because one dimension and composite structure micro Nano material thereof have the character such as some unique mechanics, optics, electromagnetism, thereby become the focus that material supply section educational circles pays close attention to.The method for preparing at present one dimension and composite structure micro-nano powder thereof mainly comprises vapour deposition process, water/solvent-thermal method, template and ultrasonic method etc.But aforesaid method preparation technology comparatively complexity, long reaction time, energy dissipation is serious and need add a large amount of additives, and contaminate environment, seriously restricted the micro Nano material applied research.So far, liquid phase method especially prepares one dimension and composite structure micro-nano granules thereof and is acknowledged as the simplest, feasible and the preparation method of prospects for commercial application arranged in water in research.But the polarity of water is large, nucleation, the fast growth that hydrolysis reaction generates oxide compound or oxyhydroxide occurs in metal ion therein, have large quantity of moisture on the nano grain surface prepared, these water moleculess can combine by the hydroxide radical on hydrogen bond and nano grain surface.When grain spacing from close to the time, lip-deep water molecules can be used as " bridge " molecule, very easily causes that in drying process between particle, hard aggregation grows up to macrobead, thereby makes quantum effect, the surface effects of nano particle, tunnel drills effect etc. and can't bring into play.
Summary of the invention
The object of the present invention is to provide a kind of single stage method to prepare one dimension and compound pattern Sb thereof 2o 3the method of micro-nano powder, overcome the easy hard aggregation of product that existing method prepares, thereby affect quantum effect, the surface effects of nano particle, and tunnel drills the defect that effect etc. can't be brought into play.
The technical solution used in the present invention is as follows:
Single stage method prepares one dimension and compound pattern Sb thereof 2o 3micro-nano powder, by SbCl under normal temperature 3ethanolic soln joins in alkaline solution and reacts, and filtration, drying obtain one dimension and compound pattern Sb thereof 2o 3micro-nano powder.
SbCl 3the concentration of ethanolic soln is 0.01-4.0 mol/L.
In described alkaline solution, the mass concentration of alkali is 0.02-30.0%.
The aqueous solution that described alkaline solution is sodium hydroxide, ammoniacal liquor, quadrol, diethanolamine.
SbCl 3the volume ratio of ethanolic soln and alkaline solution is that 1:1 is to 1:20.
SbCl 3ethanolic soln dropwise adds or disposable pouring in alkaline solution.
Temperature of reaction is 5-85 ℃, and the time is 0.1-0.5 h, in the time of reaction, is stirred.
Stir as electric stirring or magnetic agitation.
Concrete, temperature of reaction is 50-60 ℃, in the ammonia soln that is 0.02-5% in mass concentration, obtains banded Sb 2o 3micro-nano crystal grain; Temperature of reaction is 40-70 ℃, in the aqueous sodium hydroxide solution that is 0.02-1% in mass concentration, obtains nearly flower-shaped Sb 2o 3micro-nano crystal grain; Temperature of reaction is 20-50 ℃, in the ammonia soln that is 0.02-10% in mass concentration, obtains being with pencil Sb 2o 3micro-nano crystal grain; Temperature of reaction is 50-85 ℃, in the ammonia soln that is 5-12% in mass concentration, obtains bowknot shape Sb 2o 3micro-nano crystal grain; Temperature of reaction is 10-20 ℃, in the ammonia soln that is 12-25% in mass concentration, obtains flower-shaped Sb 2o 3micro-nano crystal grain; Temperature of reaction is 40-80 ℃, in the diethanolamine aqueous solution that is 1-5% in mass concentration, obtains stratiform Sb 2o 3micro-nano crystal grain; Temperature of reaction is 30-70 ℃, in the ethylenediamine solution that is 2-5% in mass concentration, obtains stratiform Sb 2o 3micro-nano crystal grain.
The object of the invention is to make reactant SbCl by controlling different reaction conditionss 3one step generates the Sb of different-shape 2o 3micro-nano granules, and the particle generated is difficult for reuniting.At first use anhydrous alcohol solution SbCl under normal temperature condition 3, make inorganic metal salt SbCl 3generate therein alcohol solvent compound, SbCl like this can slow down 3hydrolysis generates oxidiferous nucleation and the speed of growth, according to incomplete oriented adsorption and Ostwarld slaking mechanism, is grown; In addition, a small amount of ethanol molecule existed in system can be adsorbed onto particle surface, reaches sterically hindered effect, has reduced between particle and has taken by water molecules the phenomenon that " bridge " grows up.By adjusting different reaction parameters, control the product pattern, prepare the Sb of one dimension and composite structure pattern thereof 2o 3micro-nano powder, as different-shapes such as banded, band pencil, bowknot shape, flower-shaped and stratiforms.The micro-nano granules prepared not only has comparatively regular pattern, and granule surface area is large, and what have also has a larger length-to-diameter ratio, and output is large, in fields such as fire-retardant, catalysis, electrochemistry, will have good application prospect.This method has that preparation is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, and the additive that does not add any control pattern in preparation process as tensio-active agent etc., is applicable to the requirements of the times of current low carbonization, has industrial applications potential.Present method also is expected to for the preparation of the micro Nano material of other kind and industrialization research.
The present invention, with respect to prior art, has following advantage:
Product particle that the present invention prepares is better dispersed, is not easy to occur hard aggregation, and method is simple, cost is low, time saving and energy saving, save energy, environmental pollution are little, does not add any additive in preparation process, has industrial applications potential.
The accompanying drawing explanation
The Sb that Fig. 1 is banded pattern 2o 3the SEM figure of micro-nano granules;
Fig. 2 is the Sb with the pencil pattern 2o 3the SEM figure of micro-nano granules;
The Sb that Fig. 3 is the bowknot shape pattern 2o 3the SEM figure of micro-nano granules;
The Sb that Fig. 4 is floriform appearance 2o 3the SEM figure of micro-nano granules;
The Sb that Fig. 5 is the stratiform pattern 2o 3the SEM figure of micron particle;
The Sb that Fig. 6 is banded pattern 2o 3the XRD figure of micro-nano granules.
Embodiment
Below with specific embodiment, technical scheme of the present invention is described, but protection scope of the present invention is not limited to this:
Embodiment 1
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L 3ethanolic soln is added drop-wise in the ammonia soln of 45 mL 3% (wt %), and magnetic agitation is reacted 0.2 h, the Sb then hydrolysis generated 2o 3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb 2o 3powdered sample.
By the Sb prepared on a small quantity 2o 3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 1.Particle as we can see from the figure is banded pattern, and length reaches 10-20 μ m, and the thickness of single nano belt is in the 100nm left and right.
Embodiment 2
In the time of 40 ℃, the SbCl of 20 mL 0.1 mol/L 3ethanolic soln splashes in the ammonia soln of 50 mL 5% (wt %), and magnetic agitation is reacted 0.5 h, the Sb then hydrolysis generated 2o 3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb 2o 3powdered sample.
By the Sb prepared on a small quantity 2o 3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 2.Particle as we can see from the figure is band pencil pattern, and length is in 20 μ m left and right, and the thickness of single nano belt is in 100 nm left and right, and the length of band bundle one side can reach 10 μ m.
Embodiment 3
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L 3ethanolic soln is poured in the ammonia soln of 45 mL 6% (wt %), and electric stirring reacts 0.1 h, the Sb then hydrolysis generated 2o 3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb 2o 3powdered sample.
By the Sb prepared on a small quantity 2o 3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 3.Particle as we can see from the figure is the bowknot shape pattern, and length is in 20 μ m left and right, and the thickness of the nano belt of composition bow-knot-double is in 100 nm left and right, and the length of bow-knot-double one side can reach 10 μ m.
Embodiment 4
In the time of 10 ℃, the SbCl of 5 mL 1.5 mol/L 3ethanolic soln is added drop-wise in the ammonia soln of 45 mL 14% (wt %), and magnetic agitation is reacted 0.5 h, the Sb then hydrolysis generated 2o 3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb 2o 3powdered sample.
By the Sb prepared on a small quantity 2o 3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 4.The absolutely large number of particle as we can see from the figure is floriform appearance, and the diameter of flower is about 5 μ m left and right, and the micro-nano popped rice is by from center, longer length is 2-3 μ m one by one, and thickness forms at the sheet of 100 nm left and right.
Embodiment 5
In the time of 60 ℃, the SbCl of 5 mL 0.5 mol/L 3ethanolic soln is added drop-wise in the ethylenediamine solution of 45 mL 2% (wt %), and electric stirring reacts 0.5 h, the Sb then hydrolysis generated 2o 3suspension filtered, washing, 60 ℃ of oven dryings obtain Sb 2o 3powdered sample.
By the Sb prepared on a small quantity 2o 3powdered sample directly adheres on the copper platform of conductive resin, after it is carried out to metal spraying, under scanning electron microscope, observes, and result as shown in Figure 5.Particle as we can see from the figure is the laminate structure pattern, and the thickness of every one deck is also nanometer scale, and the mutual cross of some laminate structures is similar to flower-shaped.
Embodiment 6
Changing temperature is 50 ℃, the aqueous sodium hydroxide solution that alkaline solution is 0.5% (wt %), and other obtain nearly flower-shaped Sb with embodiment 4 2o 3micro-nano crystal grain.
Embodiment 7
Changing temperature of reaction is 75 ℃, and alkaline solution is 1.5% (wt %) diethanolamine aqueous solution, and other obtain stratiform Sb with embodiment 5 2o 3micro-nano crystal grain.
Fig. 6 is the banded pattern Sb of embodiment 1 2o 3the X-ray powder diffraction of powdered sample.Can see multiple diffraction absorption peak from collection of illustrative plates, the peak position of absorption peak well with rhombic form Sb 2o 3(JCPDS, 71-0383) matches, and is illustrated as rhombic form Sb 2o 3, the stronger interpret sample of absorption peak strength has comparatively perfect crystalline structure.With Sb 2o 3standard diagram compare, the Sb obtained 2o 3the intensity of (110) of powdered sample and (200) face diffraction peak improves, and the strength decreased of (111) face diffraction peak (012), this just illustrates that the crystal growth for preparing sample has certain orientation, and this is corresponding with banded pattern well.Do not find other diffraction peak yet from diffracting spectrum, illustrate that to obtain sample purity fine.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and the change that other any the present invention of not deviating from does all should be equivalent substitute mode, within being included in protection scope of the present invention.

Claims (8)

1.一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，将SbCl3乙醇溶液加入到碱溶液中发生反应，SbCl3乙醇溶液与碱溶液的体积比为1:1-20，过滤、干燥得到一维及其复合形貌Sb2O3微纳米粉体，一维及其复合形貌为带状、带束状、蝴蝶结状、花状、层状。1. One-dimensional and composite morphology Sb 2 O 3 micro-nano powders prepared by one-step method, characterized in that SbCl 3 ethanol solution is added to alkali solution to react, and the volume ratio of SbCl 3 ethanol solution to alkali solution is 1 :1-20, filtered and dried to obtain one-dimensional and its composite morphology Sb 2 O 3 micro-nano powder, the one-dimensional and its composite morphology are ribbon, ribbon, bow-knot, flower, and layered. 2.如权利要求1所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，反应温度为5-85℃，时间为 0.1-0.5 h，反应的同时进行搅拌。2. One-dimensional and composite morphology Sb 2 O 3 micronano powders prepared by one-step method as claimed in claim 1, characterized in that, the reaction temperature is 5-85°C, and the time is 0.1-0.5 h. Stir. 3.如权利要求1所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，SbCl3乙醇溶液的浓度为0.01-4.0 mol/L。3. The one-dimensional and composite morphology Sb 2 O 3 micro-nano powder prepared by one-step method as claimed in claim 1, characterized in that the concentration of the SbCl 3 ethanol solution is 0.01-4.0 mol/L. 4.如权利要求3所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，所述碱溶液中碱的质量浓度为0.02-30.0%。4. The one-dimensional and composite morphology Sb 2 O 3 micronano powder prepared by one-step method as claimed in claim 3, characterized in that the mass concentration of alkali in the alkali solution is 0.02-30.0%. 5.如权利要求4所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，所述碱溶液为氢氧化钠、氨水、乙二胺、二乙醇胺的水溶液。5. One-dimensional and composite morphology Sb 2 O 3 micro-nano powders prepared by one-step method as claimed in claim 4, it is characterized in that, the alkali solution is sodium hydroxide, ammoniacal liquor, ethylenediamine, diethanolamine aqueous solution. 6.如权利要求1所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，SbCl3乙醇溶液逐滴加入或一次性倒入碱溶液中。6. The one-dimensional and composite morphology Sb 2 O 3 micro-nano powder prepared by one-step method as claimed in claim 1, characterized in that the SbCl 3 ethanol solution is added dropwise or poured into the alkali solution at one time. 7.如权利要求2所述的一步法制备一维及其复合形貌Sb2O3微纳米粉体，其特征在于，搅拌为电动搅拌或磁力搅拌。7. The one-dimensional and composite morphology Sb 2 O 3 micro-nano powder prepared by one-step method as claimed in claim 2, characterized in that the stirring is electric stirring or magnetic stirring. 8.如权利要求1-7之一所述的一步法制备一维及其复合形貌 Sb2O3微纳米粉体，其特征在于，反应温度为50-60℃，在质量浓度为0.02-5%的氨水溶液中，得到带状Sb2O3微纳米晶体颗粒；反应温度为40-70℃，在质量浓度为0.02-1%的氢氧化钠水溶液中，得到近花状Sb2O3微纳米晶体颗粒；反应温度为20-50℃，在质量浓度为0.02-10%的氨水溶液中，得到带束状Sb2O3微纳米晶体颗粒；反应温度为 50-85℃，在质量浓度为5-12%的氨水溶液中，得到蝴蝶结状Sb2O3微纳米晶体颗粒；反应温度为10-20℃，在质量浓度为12-25%的氨水溶液中，得到花状Sb2O3微纳米晶体颗粒；反应温度为40-80℃，在质量浓度为1-5%的二乙醇胺水溶液中，得到层状Sb2O3微纳米晶体颗粒；反应温度为30-70℃，在质量浓度为2-5%的乙二胺溶液中，得到层状Sb2O3微纳米晶体颗粒。8. The one-dimensional and composite morphology Sb 2 O 3 micro-nano powder prepared by one-step method according to any one of claims 1-7, characterized in that, the reaction temperature is 50-60°C, and the mass concentration is 0.02- In 5% aqueous ammonia solution, ribbon-shaped Sb 2 O 3 micro-nano crystal particles are obtained; at a reaction temperature of 40-70°C, in an aqueous sodium hydroxide solution with a mass concentration of 0.02-1%, nearly flower-shaped Sb 2 O 3 is obtained Micro-nano crystal particles; the reaction temperature is 20-50°C, and in the ammonia solution with a mass concentration of 0.02-10%, the belt-like Sb 2 O 3 micro-nano crystal particles are obtained; the reaction temperature is 50-85°C, and at a mass concentration of In 5-12% ammonia solution, bow-tie-shaped Sb 2 O 3 micro-nano crystal particles are obtained; at a reaction temperature of 10-20°C, flower-shaped Sb 2 O 3 is obtained in an ammonia solution with a mass concentration of 12-25% Micro-nano crystal particles; the reaction temperature is 40-80°C, in the diethanolamine aqueous solution with a mass concentration of 1-5%, layered Sb 2 O 3 micro-nano crystal particles are obtained; the reaction temperature is 30-70°C, at a mass concentration of In a 2-5% ethylenediamine solution, layered Sb 2 O 3 micro-nano crystal particles are obtained.
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