CN100404411C - Method for preparing nano powder of elementary substance by using reducing agent to reduce oxide - Google Patents
Method for preparing nano powder of elementary substance by using reducing agent to reduce oxide Download PDFInfo
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- CN100404411C CN100404411C CNB2005100258300A CN200510025830A CN100404411C CN 100404411 C CN100404411 C CN 100404411C CN B2005100258300 A CNB2005100258300 A CN B2005100258300A CN 200510025830 A CN200510025830 A CN 200510025830A CN 100404411 C CN100404411 C CN 100404411C
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Abstract
The present invention provides a method for preparing nanometer micro powder of simple substance tellurium, selenium, silver, etc., by reducing oxide with a reducing agent. The preparation process is characterized in that oxide of a simple substance to be prepared is used as raw materials, one of polyvinylpyrrolidone, pyrrole or polyethylene glycol is used a reducing agent and a surface active agent, and the agent and the raw materials are mixed into suspension liquid or a uniform solution at room temperature; the suspension liquid or the uniform solution is arranged in a reaction vessel for carrying out a hydrothermal reaction in a temperature range of 120 to 220 DEG C. After the reaction, the producing matter is separated, washed and dried, and thus, corresponding simple substance nanometer micro powder is obtained. Through changing preparation conditions such as hydrothermal reaction temperature, time, density of reactants, pH value of the solution, etc., nanometer micro powder of tellurium, selenium, or silver, etc. which has different shapes and sizes can be obtained. The present invention has the characteristics that the raw materials are cheap, the technology is simple, the operation is convenient, the shape is controllable, etc.
Description
Technical field
The present invention relates to a kind of preparation method of simple substance nano powder, more precisely relate to by a kind of method for preparing simple substance nano powders such as tellurium, selenium and silver for the reductive agent reduced oxide in polyvinylpyrrolidone, pyrroles or the polyoxyethylene glycol, belong to field of nano material preparation.
Background technology
Precious metal such as silver and semi-conductor such as selenium, tellurium nano material have characteristics such as excellent light, electricity, magnetic, and it is with a wide range of applications in a lot of fields.Precious metal material itself just has excellent catalytic activity, if the nano material of being made into, its specific surface area will increase greatly, thereby increases the catalytic activity of noble metal nano particles.The noble metal nano particulate is very responsive to the heat in the environment, light, humidity and temperature, so transmitter also is one of the most promising Application Areas of noble metal nano particles.Noble metal nanometer material can also be as hydrogen storage material and optical material or the like simultaneously.Some compound of selenium, tellurium and selenium, tellurium is the semiconductor material of knowing.The unilateral conduction of selenium and outstanding photoelectric characteristic are applied to make rectifier and photocell already.Glass, pottery, enamel and pigment industry are the second largest consumer fields of selenium and tellurium, are used for producing ruby, palm fibre, indigo plant and black glass and enamel.Selenium and tellurium also can be used as rubber-reinforced dose, can improve heat-resisting, the anti-oxidant and solidity to corrosion of rubber.Selenium and tellurium can also can improve the machinability of metal and don't lower its corrosion stability as the additive of metal.
But the existing method for preparing nano materials such as selenium, tellurium and silver not only needs to introduce reductive agent usually, as hydrazine hydrate (H.Zhang, D.R.Yang, Y.J.Ji, X.Y.Ma, J.Xu, D.L.Que, J.Phys.Chem.B 2004,108,1179), sodium borohydride (R.B.Zheng, W.L.Cheng, E.K.Wang, S.J.Dong, Chem.Phys.Lett.2004,395,302; U.K.Gautam, M.Nath, C.N.R.Rao, J.Mater.Chem.2003,13,2845), xitix (J.Zhang, S.Y.Zhang, H.Y.Chen, Chem.Lett.2004,33,1054) etc., also need to introduce tensio-active agent or other inorganic salt such as sodium-chlor (Z.H.Wang, J.W.Liu simultaneously, X.Y.Chen, J.X.Wan, Y.T.Qian, Chem.Eur.J.2005,11,160) to prepare the simple substance nanometer material of different-shape.The present invention's polyvinylpyrrolidone, any one in pyrroles or the polyoxyethylene glycol need not add other reductive agent or tensio-active agent simultaneously as reductive agent and tensio-active agent, can simplify preparation technology.Simultaneously, water can reduce cost greatly as reaction solvent, has important practical significance in suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide the simple method for preparing cheaply of nano powders such as a kind of simple substance tellurium, selenium and silver.The present invention is a raw material by the corresponding oxide compound with the simple substance of desire preparation, with distilled water or deionized water is solvent, with polyvinylpyrrolidone, a kind of in pyrroles or the polyoxyethylene glycol is reductive agent and tensio-active agent, be mixed with suspension or uniform solution, again suspension or uniform solution carried out hydrothermal treatment consists and can obtain simple substance nano powders such as tellurium, selenium and silver.The method that is provided is simple, and is easy to operate, and used raw material is cheap and easy to get, is a kind of preparation method who is suitable for suitability for industrialized production.
Concrete technology comprises preparation, the hydrothermal treatment consists of reaction system, separation, washing and the drying process of product as shown in Figure 1, it is characterized in that concrete steps are as follows:
1, the preparation of liquid-phase reaction system:
(1) the corresponding oxide compound with the simple substance of desire preparation is a raw material, is solvent with distilled water or deionized water, adds a kind of reductive agent, prepares reaction system according to the simple substance kind of preparation, obtains suspension or uniform solution by stirring under the room temperature;
(2) or according to the pH value that need change reaction system of preparation with mineral acid or mineral alkali;
2, suspension or the uniform solution of preparing above is transferred in the reactor, carries out hydrothermal treatment consists at 120～220 ℃, the hydrothermal treatment consists time is 5～72 hours.Concrete temperature and time is determined according to the reductive agent of simple substance kind for preparing and use.The compactedness of reactor is 50-80%.
3, the product in the liquid-phase reaction system after the hydrothermal treatment consists is separated.Isolating method comprises centrifugation, filters or staticly settles etc.Separated products is washed and drying treatment, promptly get the nano powder of simple substance such as tellurium, selenium or silver.
Described oxide compound as reactant comprises the oxide compound of precious metals such as tellurium oxide, selenium oxide and silver.The concentration of oxide compound is 0.01～5.0 mol, and the concentration of reductive agent is 0.01～5.0 mol.
Described reductive agent comprises polyvinylpyrrolidone, a kind of in pyrroles or the polyoxyethylene glycol.Polyvinylpyrrolidone in the reaction process, pyrroles or polyoxyethylene glycol also play the effect of tensio-active agent simultaneously.
Described mineral acid is a kind of in hydrochloric acid, nitric acid or the sulfuric acid; Described mineral alkali is a kind of in sodium hydroxide, potassium hydroxide or the ammoniacal liquor.
The washing of described separated product is used dehydrated alcohol and distilled water wash respectively 2-4 time, 60 ℃ of-80 ℃ of vacuum-dryings.
The preparation method of simple substance provided by the invention (tellurium, selenium and silver etc.) nano powder has the following advantages:
(1) Zhi Bei simple substance (tellurium, selenium and silver etc.) nano powder advantages of good crystallization.
(2), can make simple substance (tellurium, selenium and the silver etc.) nano powder of different-shape and size by the suitable preparation condition of control.
(3) polyvinylpyrrolidone, pyrroles or polyoxyethylene glycol play the effect of reductive agent and tensio-active agent simultaneously in reaction process, do not need to add in addition other tensio-active agent in the reaction process, and this can simplify production process greatly, reduces cost.
(4) raw material is cheap and easy to get, easy to operate, is easy to realize suitability for industrialized production.
(5) preparation technology is simple, does not need cost and complex equipment.
Description of drawings
Preparation technology's schema of Fig. 1 simple substance (tellurium, selenium and silver etc.) nano powder.
The X-ray diffraction spectrogram of Fig. 2 tellurium nanotube.
Tellurium nanotube transmission electron microscope photo (a) and electron scanning micrograph (b) that Fig. 3 obtained 220 ℃ of hydro-thermals in 24 hours.What insert (a) is the selected area electron diffraction of single nanometer rod.
The transmission electron microscope photo (a) and the high resolution photo (b) of the tellurium nanometer rod that Fig. 4 obtained 180 ℃ of hydro-thermals in 24 hours.What insert (b) is the selected area electron diffraction of single nanometer rod.
Fig. 5 is at the transmission electron microscope photo of 180 ℃ of hydro-thermals (a) 48 hours and the tellurium nano-wire that (b) obtained in 72 hours.
Fig. 6 silver nano-grain transmission electron microscope photo.
Fig. 7 adds 2mL hydrochloric acid (36%) makes solution become strongly-acid, the transmission electron microscope photo of the tellurium nano-wire of the different amplification that obtained in 24 hours 180 ℃ of hydro-thermals.(b) be inserted as the selected area electron diffraction of single nano-wire in.
Embodiment
Further specify embodiment and effect with following indefiniteness embodiment:
Embodiment 1. polyvinylpyrrolidones are that reductive agent prepares the tellurium nanotube
At room temperature, 50mg tellurium oxide and 500mg polyvinylpyrrolidone are joined in the 30mL distilled water, stirring at room 30 minutes obtains homodisperse suspension.Suspension is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 220 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the centrifuging separated product, isolating product respectively washs 2 times with dehydrated alcohol and distilled water respectively, 60 ℃ of vacuum-dryings.Fig. 2 is the X-ray diffraction spectrogram of the tellurium nanotube of present embodiment preparation, does not find the diffraction peak of any impurity in the spectrogram, and the single-phase tellurium nanotube of gained is described.Fig. 3 is its transmission electron microscope photo and electron scanning micrograph, clearly finds out tubular structure.The prepared nanotube of high resolution photo explanation that inserts among the figure has single crystal structure.
Embodiment 2. usefulness polyvinylpyrrolidones are that reductive agent prepares the tellurium nanometer rod
At room temperature, 50mg tellurium oxide and 500mg polyvinylpyrrolidone are joined in the 30mL distilled water, stirring at room 30 minutes obtains homodisperse suspension.Suspension is changed in the back-pressure still, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the centrifuging separated product, isolating product is used dehydrated alcohol and distilled water wash respectively 2 times, and 60 ℃ of vacuum-dryings promptly get the tellurium nanometer rod.Fig. 4 shows that for the transmission electron microscope photo of the tellurium nanometer rod of present embodiment preparation its diameter is about 50nm, and length is about 2 μ m.The prepared tellurium nanometer rod of inserting among the figure of selected area electron diffraction photo explanation has single crystal structure.The direction of growth of high-resolution electron microscopy photo explanation tellurium nano-wire has only defective seldom along the C axle of lattice, and this is consistent to the result of tellurium nanometer rod single crystal structure with transmission electron microscope observing.
Embodiment 3. usefulness polyvinylpyrrolidones are that reductive agent prepares tellurium nano-wire
At room temperature, 50mg tellurium oxide and 500mg polyvinylpyrrolidone are joined in the 30mL distilled water, stirring at room 30 minutes obtains homodisperse suspension.Solution is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 72 hours.After reactor naturally cools to room temperature, take out product, use the intermediate processing separated product, isolating product is used dehydrated alcohol and distilled water wash respectively 4 times, and 60 ℃ of vacuum-dryings promptly get tellurium nano-wire.Fig. 5 (b) shows that for the transmission electron microscope photo of the tellurium nano-wire of present embodiment preparation its diameter is about 80nm, and length is about 10 μ m.
Embodiment 4. usefulness polyethylene glycol 6000s are that reductive agent prepares tellurium nano-wire
At room temperature, 50mg tellurium oxide and 500mg polyethylene glycol 6000 are joined in the 30mL distilled water, stirring at room 30 minutes obtains homodisperse suspension.Suspension is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the filter method separated product, isolating product respectively washs 2 times with dehydrated alcohol and distilled water respectively, and 80 ℃ of vacuum-dryings promptly obtain tellurium nano-wire.
Embodiment 5. usefulness polyvinylpyrrolidones are that reductive agent prepares silver nano-grain
At room temperature, 30mg silver suboxide and 500mg polyvinylpyrrolidone are joined in the 30mL distilled water, stirring at room 30 minutes obtains homodisperse suspension.Suspension is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the centrifuging separated product, isolating product is used dehydrated alcohol and distilled water wash respectively 2 times, and 60 ℃ of vacuum-dryings promptly obtain silver nano-grain.Fig. 6 shows that for the transmission electron microscope photo of the silver nano-grain of present embodiment preparation product is polygonal Nano silver grain, and mean diameter is less than 100nm.
Embodiment 6. usefulness polyvinylpyrrolidones are that reductive agent prepares the selenium linear structure
At room temperature, 37mg selenium oxide and 500mg polyvinylpyrrolidone are joined in the 30mL distilled water, stirring at room 30 minutes obtains the clear solution of homogeneous.Clear solution is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the intermediate processing separated product, isolating product is used dehydrated alcohol and distilled water wash respectively respectively 2 times, and 60 ℃ of vacuum-dryings promptly obtain the selenium linear structure.
Embodiment 7. usefulness pyrroles are that reductive agent prepares the tellurium linear structure
At room temperature, 33mg tellurium oxide and 0.3mL pyrroles are gone in 19.7mL distilled water, add in NaOH, KOH or the ammoniacal liquor a kind ofly again, make solution become strong basicity, stirring at room 30 minutes obtains homodisperse solution.Solution is changed in the reactor, add distilled water to 50% of reactor volume, sealing.Reactor is put into baking oven, 120 ℃ of insulations 10 hours.After reactor naturally cools to room temperature, take out product, use the centrifuging separated product, isolating product respectively washs 2 times with dehydrated alcohol and distilled water respectively, and 60 ℃ of vacuum-dryings promptly obtain the tellurium linear structure.
Embodiment 8. usefulness polyvinylpyrrolidones are that reductive agent prepares tellurium nano-wire
At room temperature, 50mg tellurium oxide and 500mg polyvinylpyrrolidone are gone in 30mL distilled water, add 2mL hydrochloric acid (36%) or nitric acid again, sulfuric acid makes solution become strongly-acid.Stirring at room 30 minutes obtains uniform solution.Uniform solution is changed in the reactor, add distilled water to 75% of reactor volume, sealing.Reactor is put into baking oven, 180 ℃ of insulations 24 hours.After reactor naturally cools to room temperature, take out product, use the centrifuging separated product, isolating product respectively washs 2 times with dehydrated alcohol and distilled water respectively, and 60 ℃ of vacuum-dryings promptly obtain the tellurium linear structure.Fig. 7 shows that for the transmission electron microscope photo of the tellurium nanometer rod of present embodiment preparation its diameter is about 50nm.The prepared tellurium nanometer rod of inserting among the figure of selected area electron diffraction photo explanation has single crystal structure, and the direction of growth is along the C axle of lattice.
Claims (7)
1. one kind prepares the method for simple substance nano powder with the reductive agent reduced oxide, comprises preparation, the hydrothermal treatment consists of reaction system, separation, washing and the drying process of product, it is characterized in that concrete preparation process is as follows:
(1) corresponding oxide with the simple substance of desire preparation is a raw material, is solvent with distilled water or deionized water, adds a kind of reductive agent, stir under the room temperature, and be suspension or uniform solution according to the reaction system of the simple substance kind preparation of preparation; Described reductive agent is any one in polyvinylpyrrolidone, pyrroles or the polyoxyethylene glycol;
(2) prepared suspension of step (1) or solution are transferred in the hydrothermal reaction kettle, 120～220 ℃ are carried out hydrothermal treatment consists, and the time is 5～72 hours;
(3) product in the liquid-phase reaction system after the hydrothermal treatment consists is separated, then separated products is washed and drying treatment;
Described simple substance is tellurium, selenium or silver, and described raw material is tellurium oxide, selenium oxide or silver suboxide.
2. prepare the method for simple substance nano powder by claim 1 is described with the reductive agent reduced oxide, it is characterized in that in the effect of tensio-active agent of having held concurrently simultaneously of the reductive agent described in the reaction process.
3. by the described method for preparing the simple substance nano powder with the reductive agent reduced oxide of claim 1, the concentration that it is characterized in that described oxide compound is 0.01 mol～5.0 mol, the concentration of reductive agent is 0.01 mol～5.0 mol, and the compactedness of reactor is 50%～80%.
4. prepare the method for simple substance nano powder by claim 1 is described with the reductive agent reduced oxide, it is characterized in that described separation method is centrifugation, a kind of in filtering or staticly settling.
5. prepare the method for simple substance nano powder by claim 1 is described with the reductive agent reduced oxide, it is characterized in that the separated product washing uses dehydrated alcohol and distilled water wash respectively 2-4 time, 60-80 ℃ of vacuum-drying.
6. by any one describedly prepares the method for simple substance nano powder with the reductive agent reduced oxide among the claim 1-5, the pattern that it is characterized in that the nano powder of the simple substance for preparing is a kind of in nanometer rod, nano wire, nanotube or the nano particle.
7. by the described method for preparing the simple substance nano powder with the reductive agent reduced oxide of claim 1-5, the pH value of the reaction system of the simple substance kind preparation that it is characterized in that preparing is regulated with mineral acid or mineral alkali, and described mineral acid is a kind of in hydrochloric acid, nitric acid or the sulfuric acid; Described mineral alkali is a kind of in sodium hydroxide, potassium hydroxide or the ammoniacal liquor.
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| CN101898250A (en) * | 2010-07-20 | 2010-12-01 | 复旦大学 | Original ecology separation and redispersion method of nano metallic colloid |
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| CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
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