CN102267718A - Synthesis method of tin dioxide nanometer material - Google Patents

Abstract

The invention relates to a synthesis method of a tin dioxide nanometer material. The method comprises the following specific steps: weighting tin sulfate (SnSO4) and trisodium citrate dehydrate (Na3C6H5O7.2H2O) which are used as raw materials, according to a molar ratio of 2:(5-4); adding the raw materials into a mixed solution of absolute alcohol and deionized water of which the volume ratio is 1:(9-9), quickly stirring for 1-2 hours, putting the mixture into a high-pressure reaction kettle to react at 120-200 DEG C for 2-48 hours, cooling, washing with deionized water and ethanol several times, and drying to obtain the tin dioxide nanometer material. The synthesis method has the advantages of simple process and good repeatability and can be used for batch production. The particle size of the product-tin dioxide nanospheres is about 50nm and the product has good monodispersity.

Description

The synthetic method of stannic oxide nanometer material

Technical field

The present invention relates to a kind of stannic oxide nanometer preparation methods, belong to inorganic chemistry and field of material synthesis technology.

Background technology

Tindioxide (SnO ₂) be a kind of conductor oxidate material of excellent performance, it has wide band gap (3.6 eV), low resistivity (10 ^-4~ 10 ⁶Ω cm) and high light transmittance.In addition, it also have reliability height, physicochemical property stable, to advantages such as gas detection are reversible, with low cost, be widely used in gas sensing property transmitter, lithium ion battery, glass coating, photochemical catalysis, and field such as solar cell.

In recent years, along with the development of nanoscale science and technology, people have prepared the various stannic oxide nanometer material of pattern, as nano particle, and nano core-shell, nanometer ball, nano wire, nanotube, nanometer sheet etc.In these materials, the stannic oxide nanometer ball is because its unique pattern and synthesis condition gentleness, the great interest that caused people.Bibliographical information mainly contains vacuum condensation method about the stannic oxide nanometer preparation methods, vapour deposition process, sol-gel method, the precipitator method, microemulsion method etc. at present.But all inevitably there are some problems in above these methods, and to the having relatively high expectations of equipment, the product purity of precipitator method preparation is low as vacuum condensation method and vapour deposition process, and particle radius is big etc.Except above-mentioned method, hydrothermal synthesis method is simple to operate because of having, characteristics such as products obtained therefrom particle purity height, good dispersity and looked at by investigator's parent.It is called hydrothermal method again, is meant to be solvent with water etc. in the pressurized vessel of sealing, the chemical reaction that carries out under the condition of High Temperature High Pressure.

Summary of the invention

The purpose of this invention is to provide a kind of stannic oxide nanometer preparation methods.

The present invention is with stannous sulfate (SnSO ₄) be Xi Yuan, two hydration trisodium citrate (Na ₃C ₆H ₅O ₇2H ₂O) as sequestrant, fast magnetic agitation makes SnSO in this process ₄Fully hydrolysis utilizes Na again ₃C ₆H ₅O ₇2H ₂The sequestering action of O in solution system and the reaction system of High Temperature High Pressure have finally formed the comparatively stannic oxide nanometer material of the small particle size of homogeneous of pattern.

According to above-mentioned design, the present invention adopts following technical scheme:

A kind of stannic oxide nanometer preparation methods is characterized in that the concrete steps of this method are:

A. the volume ratio according to (1: 9 ~ 9) mixes dehydrated alcohol and deionized water, forms mixed solution;

B. the mol ratio according to (2: 5 ~ 4) takes by weighing stannous sulfate and two hydration trisodium citrates respectively, and joins in the step a gained mixed solution, stirs 1 ~ 2 hour;

C. step b gained mixed solution was reacted 2 ~ 48 hours down at 120 ~ 200 ℃, use deionized water and absolute ethanol washing after filtering, promptly obtain the stannic oxide nanometer material after the oven dry then.

Characteristics of the present invention and mechanism are described below: in the process of the present invention with SnSO ₄And Na ₃C ₆H ₅O ₇2H ₂O is dissolved in the mixed solution of second alcohol and water composition simultaneously;

The stannic oxide nanometer material particle size that the present invention adopts hydro-thermal synthetic method to prepare is little, monodispersity good.And the pattern homogeneous is having good prospects for application aspect gas sensing property transmitter and the electrochemistry, can produce in batches, and this is fit to industrial applications very much.

Technology of the present invention is simple, the preparation condition gentleness, and good reproducibility, and product yield is higher, can realize large-scale mass production, and this is very beneficial for its industrial applications.

Description of drawings

Fig. 1 is products therefrom SnO among the embodiment 1 among the present invention ₂X-ray diffraction (XRD) spectrogram.

Fig. 2 is gained SnO among the embodiment 1 among the present invention ₂Scanning electronic microscope (SEM) photo figure.

Fig. 3 is gained SnO among the embodiment 1 among the present invention ₂Transmission electron microscope (TEM) photo figure.

Embodiment

All embodiment all operate by the operation steps of technique scheme.

Embodiment 1:

Preparation process and step in the present embodiment are as described below:

1. measure 10 mL dehydrated alcohol (CH respectively with graduated cylinder ₃CH ₂OH) and the deionized water of 90 mL, pour in the beaker, mix;

2. take by weighing the stannous sulfate (SnSO of 1.0738 g (5 mmol) with electronic balance ₄) and the two hydration trisodium citrate (Na of 4.4115 g (15 mmol) ₃C ₆H ₅O ₇2H ₂O);

3. the SnSO of weighing ₄And Na ₃C ₆H ₅O ₇2H ₂O joins in the above-mentioned solution in the lump, and magnetic agitation is 1 hour fast;

4. above-mentioned mixing solutions is packed in the autoclave, reaction is 12 hours in 160 ℃ baking oven;

5. will react products therefrom cooling back wash 3 times respectively with deionized water and dehydrated alcohol after 80 ℃ of dryings 12 hours down, promptly obtain the stannic oxide nanometer material.

The particle diameter of gained stannic oxide nanometer material is in 40 ~ 60 nm scopes, and monodispersity is good.

Embodiment 2:

Implementation process except for the following differences, other are all identical with embodiment 1

1. measure 20 mL dehydrated alcohol (CH respectively with graduated cylinder ₃CH ₂OH) and the deionized water of 80 mL, pour in the beaker, mix;

4. above-mentioned mixing solutions is packed in the autoclave, reaction is 36 hours in 120 ℃ baking oven;

The particle diameter of gained stannic oxide nanometer material is in 40 ~ 200 nm scopes.

 

Embodiment 3:

Implementation process except for the following differences, other are all identical with embodiment 1

2. take by weighing the stannous sulfate (SnSO of 1.0738 g (5 mmol) with electronic balance ₄) and the two hydration trisodium citrate (Na of 0.7353 (2.5 mmol) ₃C ₆H ₅O ₇2H ₂O);

4. above-mentioned mixing solutions is packed in the autoclave, reaction is 24 hours in 140 ℃ baking oven;

The particle diameter of gained stannic oxide nanometer material but has a large amount of block SnO in 40 ~ 100 nm scopes ₂Generate.

 

Embodiment 4:

Implementation process except for the following differences, other are all identical with embodiment 1

2. take by weighing the stannous sulfate (SnSO of 1.0738 g (5 mmol) with electronic balance ₄);

3. the SnSO of weighing ₄Join in the solution, magnetic agitation is 2 hours fast;

4. above-mentioned mixing solutions is packed in the autoclave, reaction is 2 hours in 200 ℃ baking oven;

But there is certain agglomeration in the particle diameter of gained stannic oxide nanometer material in 40 ~ 60 nm scopes.

 

Above embodiment products therefrom is SnO ₂Nano material all has similar XRD spectra, just some difference on the pattern.

Referring to accompanying drawing, Fig. 1 is products therefrom SnO in the embodiment of the invention 1 ₂X-ray diffraction (XRD) spectrogram, XRD analysis: on Japanese RigaKu D/max-2550 type X-ray diffractometer, carry out Cu-K α diffraction.As can be seen from Figure 1, SnO ₂The position of diffraction peak consistent with standard card (JCPDS card No.41-1445), and do not have other tangible stray crystals and occur mutually, the SnO that has successfully synthesized pure phase by this method proved with rutile structure ₂Nano material.

Referring to accompanying drawing, Fig. 2 is gained SnO among the embodiment 1 among the present invention ₂Scanning electronic microscope (SEM) photo figure., sem analysis: adopt the Japanese JEOL JSM-6700F of company type sem observation material pattern.As shown in Figure 2, the SnO that synthesizes ₂Spherical pattern with homogeneous.

Referring to accompanying drawing, Fig. 3 is gained SnO among the embodiment 1 among the present invention ₂Transmission electron microscope (TEM) photo figure.Tem analysis: adopt the Japanese JEOL JEM-200CX of company type transmission electron microscope observation material pattern.From the TEM picture as can be seen, the SnO that adopts this method to synthesize ₂The feature that presents porous material, its particle diameter is about 50 nm, and monodispersity is very good.

Claims (1)

1. stannic oxide nanometer preparation methods is characterized in that the concrete steps of this method are:

A. the volume ratio according to (1: 9 ~ 9) mixes dehydrated alcohol and deionized water, forms mixed solution;

B. the mol ratio according to (2: 5 ~ 4) takes by weighing stannous sulfate and two hydration trisodium citrates respectively, and joins in the step a gained mixed solution, stirs 1 ~ 2 hour;

C. step b gained mixed solution was reacted 2 ~ 48 hours down at 120 ~ 200 ℃, use deionized water and absolute ethanol washing after filtering, promptly obtain the stannic oxide nanometer material after the oven dry then.

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