CN107539961A - The preparation method of telluride tin nanometer rods and telluride tinbase binary metal tellurides nanometer rods - Google Patents
The preparation method of telluride tin nanometer rods and telluride tinbase binary metal tellurides nanometer rods Download PDFInfo
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Abstract
The invention provides a kind of method for preparing telluride tin nanometer rods, including：Tellurium source and surfactant are added in ethylene glycol, obtain the first mixture, wherein tellurium source is sodium tellurite or orthotelluric acid；First mixture is heated to above to 110 DEG C of the first temperature, and adds hydrazine hydrate, reaction obtains including the second mixture of tellurium nanometer rods；Tin source is added into the second mixture, the second mixture is heated to above to 170 DEG C of second temperature, reaction obtains telluride tin nanometer rods, and wherein tin source is the chloride or nitrate of tin.Present invention also offers a kind of method for preparing telluride tinbase binary metal tellurides nanometer rods, including the second source metal is added simultaneously with tin source in the above-mentioned methods.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to telluride tin nanometer rods and telluride tinbase binary metal
The preparation method of tellurides nanometer rods.
Background technology
《Materials chemistry magazine》(volume 21 page 12218 of Journal of Materials Chemistry.2011) is reported
It is a kind of using Continuous Heat injection reaction device sustained response to obtain the method for telluride tin nanometer rods.It is using trioctylphosphine telluride phosphine as tellurium
Source, stannous chloride are tin source, react and obtain in oleic acid and tri octyl phosphine mixed liquor is the systems of solvent.Gained nanorod diameter
In 20 ± 5nm, for length in 60 ± 10nm, overall uniformity is fine, but draw ratio is relatively low, and post-processing is made using oil phase environment
It is a kind of poisonous solvent into certain influence and tri octyl phosphine, need to carefully uses.
《JACS》(Journal of the American Chemical Society.2015 volumes 137
Page 15074) report a kind of method that different telluride tin patterns are synthesized based on solution.Unlike, it selects oleyl amine and three pungent
Amine reacts 30 minutes as system environment, first addition stannous iodide at 100 DEG C, then pungent by injecting three at different temperatures
Base telluride phosphine and follow-up different reaction temperature control gained telluride tin pattern, (160 DEG C of injection temperature, reaction temperature during high temperature
240 DEG C of degree) obtain it is cubic, during low temperature (injection temperature is less than 120 DEG C, 180 DEG C of reaction temperature) obtain bar-shaped.And it can lead to
Overregulating different injection temperature (40~120 DEG C) can adjust to obtain the telluride tin nanometer rods of different draw ratios, overall synthesis
It is relatively simple, it can control to obtain different-shape, the product of draw ratio, but select oil phase environment and trioctylamine, tri octyl phosphine
Use, can also produce puzzlement same as mentioned above.
For environment-friendly and simply to manufacture telluride tin nanometer rods and telluride tinbase binary metal tellurides nanometer rods special
It is not the method with larger diameter and the nanometer rods compared with high length-diameter ratio, there are still needs.
The content of the invention
The present invention provides following technical scheme, to solve the above problems.
The present invention provides a kind of method for preparing telluride tin nanometer rods, and methods described includes：
Tellurium source and surfactant are added in ethylene glycol, obtain the first mixture, wherein the tellurium source is tellurous acid
Sodium or orthotelluric acid；
First mixture is heated to above to 110 DEG C of the first temperature, and adds hydrazine hydrate, reaction obtains including tellurium
Second mixture of nanometer rods；
Tin source is added into second mixture, the second mixture is heated to above to 170 DEG C of second temperature, reacted
To telluride tin nanometer rods, wherein the tin source is the chloride or nitrate of tin.
The present invention also provides a kind of method for preparing telluride tinbase binary metal tellurides nanometer rods, and methods described includes：
Tellurium source and surfactant are added in ethylene glycol, obtain the first mixture, wherein the tellurium source is tellurous acid
Sodium or orthotelluric acid；
First mixture is heated to above to 110 DEG C of the first temperature, and adds hydrazine hydrate, reaction obtains including tellurium
Second mixture of nanometer rods；
Tin source and the second source metal are added into second mixture, the second mixture is heated to above the of 170 DEG C
Two temperature, reaction obtains telluride tinbase binary metal tellurides nanometer rods, wherein the tin source is the chloride or nitrate of tin,
Second source metal is bimetallic chloride or nitrate.
In the method for telluride tin nanometer rods or telluride tinbase binary metal tellurides nanometer rods is prepared：
Preferably, tin source is two hydrated stannous chlorides；
Preferably, the first temperature is between 120 DEG C to 160 DEG C；
Preferably, surfactant is PVP.
In the method for preparing telluride tinbase binary metal tellurides nanometer rods：
Preferably, the second metal is bismuth, and telluride tinbase binary metal tellurides nanometer rods are telluride tin-bismuth telluride nanometers
Rod；It is highly preferred that the second source metal is five nitric hydrate bismuths；
Preferably, the second metal is copper, and telluride tinbase binary metal tellurides nanometer rods are telluride tin-cuprous telluride nanometers
Rod；It is highly preferred that the second source metal is Copper dichloride dihydrate；
Preferably, second metal is cadmium, and the telluride tinbase binary metal tellurides nanometer rods are telluride tin-telluride
Cadmium nanometer rods；It is highly preferred that the second source metal is four nitric hydrate cadmiums.
The invention provides environment-friendly and simply manufacture telluride tin nanometer rods or telluride tinbase binary metal tellurides
The method of nanometer rods, telluride tin nanometer rods or telluride tinbase binary metal with larger diameter and compared with high length-diameter ratio can be manufactured
Tellurides nanometer rods.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of the telluride tin nanometer rods prepared in the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscopic picture of the telluride tin nanometer rods prepared in the embodiment of the present invention 2；
Fig. 3 is the scanning electron microscopic picture of the telluride tin nanometer rods prepared in the embodiment of the present invention 3；
Fig. 4 is the x-ray diffractogram of powder spectrum of the telluride tin nanometer rods prepared in the embodiment of the present invention 1 to 3；
Fig. 5 is the scanning electron microscopic picture of the telluride tin-bismuth telluride nanometer rods prepared in the embodiment of the present invention 4；
Fig. 6 is the x-ray diffractogram of powder spectrum of the telluride tin-bismuth telluride nanometer rods prepared in the embodiment of the present invention 4；
Fig. 7 is the scanning electron microscopic picture of the telluride tin-cuprous telluride nanometer rods prepared in the embodiment of the present invention 5；
Fig. 8 is the x-ray diffractogram of powder spectrum of the telluride tin-cuprous telluride nanometer rods prepared in the embodiment of the present invention 5；
Fig. 9 is the transmission electron microscope picture of the telluride tin-cadmium telluride nanometer rods prepared in the embodiment of the present invention 6；
Figure 10 is the x-ray diffractogram of powder spectrum of the telluride tin-cadmium telluride nanometer rods prepared in the embodiment of the present invention 6；
Figure 11 is the transmission electron microscope picture of the telluride tin nanometer rods prepared in the embodiment of the present invention 7；
Figure 12 is the x-ray diffractogram of powder spectrum of the telluride tin nanometer rods prepared in the embodiment of the present invention 7；
Embodiment
The present invention proposes a kind of preparation for preparing telluride tin nanometer rods or telluride tinbase binary metal tellurides nanometer rods
Method.
In the present invention, term " telluride tinbase binary metal tellurides " refers to a kind of binary metal tellurides, wherein
A kind of metal is tin.That is, telluride tinbase binary metal tellurides can be expressed as the metal telluride of telluride tin-the second.
" the second metal " refers to the metal in addition to metallic tin.Specifically, the second metal can be bismuth, copper, cadmium etc., corresponding telluride
Tinbase binary metal tellurides can be such as telluride tin-bismuth telluride, telluride tin-cuprous telluride, telluride tin-cadmium telluride.Should
When it is noted that although the binary metal tellurides in the present invention is referred to as " telluride tinbase ", but this is not intended to mean that two
Tin is main in kind metal.Term " telluride tinbase " only represents that a kind of metal in the binary metal tellurides is tin.Two
In first metal telluride nanometer rods, the molar content of tin can be higher than bimetallic molar content；But, the molar content of tin
Technical scheme less than the second metal molar content is also within the scope of the present invention.
The preparation method of the present invention is using ethylene glycol in the system of solvent, directly to be synthesized by simple chemical transformation
Obtain target product.
The basic process of method of the present invention is：First, in appropriate environmental system, tellurium source and surface-active are added
Agent, the first mixture is formed, and the heating of the first mixture is reacted, it is mixed to prepare second comprising homogeneous tellurium nanometer rods
Compound.Then, the tin source as presoma and the second optional source metal are added into the second mixture, then is elevated above 170
DEG C reaction temperature reaction a period of time, you can obtain corresponding metal telluride nanorod structure.
The overall reaction mechanism of method of the present invention is：Tellurium source is reduced to simple substance tellurium, and this time control under hydrazine hydrate effect
The synthesis of nanometer rods pattern processed；Then, add corresponding metal ion, its by hydrazine hydrate reduction into elemental metallic atom, just
With simple substance tellurium rod the corresponding metal telluride of combination reaction generation occurs for the metallic atom of the high activity of generation.
Tellurium source is sodium tellurite and orthotelluric acid in the preparation method of the present invention.Tellurium source can be gone back in the presence of reducing agent
Originally it was tellurium simple substance.Compared with sodium tellurite, it can obtain that draw ratio is higher and even size distribution using orthotelluric acid as tellurium source
The higher nanometer rods of property.
Reducing agent in the preparation method of the present invention is hydrazine hydrate.The effect of hydrazine hydrate in the present invention is：First, as
Reducing agent, corresponding tellurium source, source metal are reduced to corresponding simple substance；Second, there is provided the weakly alkaline environment of whole system：If system
For acidity, then the high activity metal atom just generated first may react with H+；If system is strong basicity environment, the tellurium list of generation
Disproportionated reaction may occur for matter, and two kinds of situations can influence subsequent reactions.It can also reach 2 points of effects of the above from sodium borohydride
Fruit, but in real process, it is good to be far from hydrazine hydrate using the effect of sodium borohydride.Importantly, final product also with
The formation of nano particle, it is impossible to be advantageously controlled the formation of nanometer rods.
In order to form the nanometer rods of desired shape, surfactant is needed to use when forming tellurium nanometer rods.Live on surface
Property agent example include polyvinylpyrrolidone, polyethylene glycol, cetyl trimethylammonium bromide etc..Wherein, polyvinyl pyrrole
Alkanone is most common, effect is also best.Although polyethylene glycol, cetyl trimethylammonium bromide can also as an alternative,
But effect is far short of what is expected.
Selected environmental system is ethylene glycol solvent environment in the preparation method of the present invention.In the preparation process in accordance with the present invention,
It is from the reason for ethylene glycol, on the one hand, reaction temperature can be higher than 170 DEG C, and the in general aqueous solution is unable to reach；The opposing party
Face, ethylene glycol modest viscosity, each material mixing can be made uniformly with sustained response.In the method for the invention, reaction environment is viscous
Spend extremely important, the too high and too low formation for being unfavorable for the desired nanometer rods with high length-diameter ratio of the present invention of viscosity.For example,
When from substitute of the glycerine as ethylene glycol, because its viscosity is excessive so that stirring difficulty, be unfavorable for the equal of each material
It is even scattered, cause finally prepd product that there is more particle.In addition, ethylene glycol is very cheap, economy is high.
Source metal is the corresponding chloride (i.e. hydrochloride) or nitrate of metal in the preparation method of the present invention.That is,
Tin source is the chloride or nitrate of tin.Second source metal is bimetallic chloride or nitrate.Nodeless mesh water
Source metal and source metal effect containing the crystallization water are more or less the same, but consider from cheap and ready availability angle, from containing the crystallization water
Source metal is preferred.In order to facilitate reaction, source metal can be first dissolved in a small amount of ethylene glycol, be then added to the second mixing
In thing.
First reaction temperature of the first mixture of tellurium source, PVP and ethylene glycol composition is higher than 110 DEG C,
And preferably 120 to 160 degrees Celsius.First temperature is higher, and tellurium nanorod length is longer, but diameter is basically unchanged.Add metal
The second reaction temperature behind source is higher than 170 DEG C, preferably at about 180 DEG C.
Nanometer rods made from the method for the present invention have one-dimensional nano structure, and have higher diameter, particularly have
There is high length-diameter ratio.Its diameter can be 30 to 60nm, such as 40 to 50nm；Draw ratio can be more than 5, more than 6, more than 8, or even greatly
In 10；Length can be more than 150nm, more than 250nm, even greater than 500nm.
It is optionally possible to washing, drying by washing, alcohol, the post processing such as mill, the production as corresponding solid powder is obtained
Thing.
The reaction process of this preparation method is simple, and selected reagent is also readily available and nontoxic.To end-product nanometer rods
The regulation of draw ratio can both be adjusted by reaction temperature, can also be adjusted by changing sodium tellurite into orthotelluric acid；Both tellurium can be synthesized
Change tin, can also synthesize telluride tinbase binary metal tellurides.Preferably, using two hydrated stannous chlorides as tin source, tellurium is prepared
Change tin nanometer rods.Preferably, using two hydrated stannous chlorides and five nitric hydrate bismuths as source metal, telluride tin-telluride is prepared
Bismuth nanometer rods.Preferably, using two hydrated stannous chlorides and Copper dichloride dihydrate as source metal, it is sub- to prepare telluride tin-telluride
Copper nanometer rods.Preferably, using two hydrated stannous chlorides and four nitric hydrate cadmiums as source metal, telluride tin-cadmium telluride is prepared
Nanometer rods.
Tellurides nanometer rods synthesized by the present invention have larger diameter and suitable big L/D ratio, can extensive use
In fields such as thermoelectric conversion, photodetection, galvanomagnetic-effects.
The present invention is more fully described by the following examples.It should be appreciated that embodiment is provided exclusively for the purposes of illustration,
And the invention is not restricted to these embodiments.
Agents useful for same is commercially available in the present invention, is also synthesized using known method in laboratory.
Embodiment 1
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 120 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Two hydrated stannous chloride 0.2257g (1mmol) being first dissolved in advance in a small amount of ethylene glycol are then added, are warming up to 180
DEG C, 2h is reacted, is washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying 12h.
This nanometer rods scanning electron microscopic picture is shown in Fig. 1, and XRD data are shown in Fig. 4.Now nanorod length is about 280 to 300nm,
Diameter is about 50nm.
Embodiment 2
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 140 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Two hydrated stannous chloride 0.2257g (1mmol) being first dissolved in advance in a small amount of ethylene glycol are then added, are warming up to 180
DEG C, 2h is reacted, is washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying 12h.
This nanometer rods scanning electron microscopic picture is shown in Fig. 2, and XRD data are shown in Fig. 4.Now nanorod length is about 360 to 420nm,
Diameter is about 50nm.
Embodiment 3
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 160 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Two hydrated stannous chloride 0.2257g (1mmol) being first dissolved in advance in a small amount of ethylene glycol are then added, are warming up to 180
DEG C, 2h is reacted, is washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying 12h.
This nanometer rods scanning electron microscopic picture is shown in Fig. 3, and XRD data are shown in Fig. 4.Now nanorod length is about 480 to 600nm,
Diameter is about 50nm.
From embodiment 1 to 3, with the raising of tellurium rod growth temperature, its length significantly improves, but its diameter is very steady
It is fixed.
Embodiment 4
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 120 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Then add the hydrations of two hydrated stannous chloride 0.0564g (0.25mmol) being first dissolved in advance in a small amount of ethylene glycol and five
Bismuth nitrate 0.2426g (0.5mmol), 180 DEG C are warming up to, react 2h, washed 1 time after cooling, ethanol is washed twice, and 60 DEG C of vacuum are done
Dry 12h.
This nanometer rods scanning electron microscopic picture is shown in Fig. 5, and XRD data are shown in Fig. 6.Now nanorod length is about 300 to 400nm,
Diameter is about 50nm.
Embodiment 5
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 120 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Then add the hydration chlorine of two hydrated stannous chloride 0.1129g (0.5mmol) being first dissolved in advance in a small amount of ethylene glycol and two
Change copper 0.1705g (1mmol), be warming up to 180 DEG C, react 2h, washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying
12h。
This nanometer rods scanning electron microscopic picture is shown in Fig. 7, and XRD data are shown in Fig. 8.Now nanorod length is about 250 to 600nm,
Diameter is about 40 to 50nm.
Embodiment 6
Take 50mL three-necked flasks, wherein add 0.2216g (1mmol) sodium tellurite, 1g polyvinylpyrrolidones and
30mL ethylene glycol, it is passed through argon gas and protects and be heated to 120 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, instead
Answer 2h.Then add the two hydrated stannous chloride 0.2257g (1mmol) and four nitric hydrates being first dissolved in advance in a small amount of ethylene glycol
Cadmium 0.1542g (0.5mmol), 180 DEG C are warming up to, react 2h, washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying
12h。
This nanometer rods transmission electron microscope picture is shown in Fig. 9, and XRD data are shown in Figure 10.Now nanorod length is about 250 to 600nm,
Diameter is about 35 to 45nm.
From embodiment 4 to 6, by converting source metal, corresponding binary metal tellurides nanometer rods can be formed, and
And still there is larger diameter and high length-diameter ratio.
Embodiment 7
50mL three-necked flasks are taken, add 0.2296g (1mmol) orthotelluric acid, 1g polyvinylpyrrolidones and 30mL wherein
Ethylene glycol, it is passed through argon gas and protects and be heated to 120 DEG C under magnetic stirring, be now added immediately 2mL98% hydrazine hydrates, react
2h.Two hydrated stannous chloride 0.2257g (1mmol) being first dissolved in advance in a small amount of ethylene glycol are then added, are warming up to 180 DEG C,
2h is reacted, is washed 1 time after cooling, ethanol is washed twice, 60 DEG C of vacuum drying 12h.
This nanometer rods transmission electron microscope picture is shown in Figure 11, and XRD data are shown in Figure 12.Now nanorod length be about 800 to
850nm, diameter are about 40nm.
As can be seen that when changing tellurium source into orthotelluric acid by sodium tellurite, its draw ratio significantly improves, and even size distribution
Property can also improve.
Claims (11)
1. a kind of method for preparing telluride tin nanometer rods, methods described include：
Tellurium source and surfactant are added in ethylene glycol, obtain the first mixture, wherein the tellurium source be sodium tellurite or
Orthotelluric acid；
First mixture is heated to above to 110 DEG C of the first temperature, and adds hydrazine hydrate, reaction obtains including tellurium nanometer
Second mixture of rod；
Tin source is added into second mixture, the second mixture is heated to above to 170 DEG C of second temperature, reaction obtains tellurium
Change tin nanometer rods, wherein the tin source is the chloride or nitrate of tin.
2. a kind of method for preparing telluride tinbase binary metal tellurides nanometer rods, methods described include：
Tellurium source and surfactant are added in ethylene glycol, obtain the first mixture, wherein the tellurium source be sodium tellurite or
Orthotelluric acid；
First mixture is heated to above to 110 DEG C of the first temperature, and adds hydrazine hydrate, reaction obtains including tellurium nanometer
Second mixture of rod；
Tin source and the second source metal are added into second mixture, the second mixture is heated to above to 170 DEG C of the second temperature
Degree, reaction obtains telluride tinbase binary metal tellurides nanometer rods, wherein the tin source is the chloride or nitrate of tin, it is described
Second source metal is bimetallic chloride or nitrate.
3. method according to claim 1 or 2, wherein the tin source is two hydrated stannous chlorides.
4. method according to claim 1 or 2, wherein first temperature is between 120 DEG C to 160 DEG C.
5. method according to claim 1 or 2, wherein the surfactant is PVP.
6. according to the method for claim 2, wherein second metal is bismuth, the telluride tinbase binary metal tellurides
Nanometer rods are telluride tin-bismuth telluride nanometer rods.
7. according to the method for claim 2, wherein second source metal is five nitric hydrate bismuths.
8. according to the method for claim 2, wherein second metal is copper, the telluride tinbase binary metal tellurides
Nanometer rods are telluride tin-cuprous telluride nanometer rods.
9. according to the method for claim 2, wherein second source metal is Copper dichloride dihydrate.
10. according to the method for claim 2, wherein second metal is cadmium, the telluride tinbase binary metal telluride
Thing nanometer rods are telluride tin-cadmium telluride nanometer rods.
11. according to the method for claim 2, wherein second source metal is four nitric hydrate cadmiums.
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| CN112875654A (en) * | 2021-01-12 | 2021-06-01 | 青岛大学 | Tin telluride nanobelt and preparation method and application thereof |
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| CN1384047A (en) * | 2002-06-07 | 2002-12-11 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112573490A (en) * | 2020-11-09 | 2021-03-30 | 青海大学 | Method for macro-preparation of uniform single crystal cadmium telluride nanorods |
| CN112875654A (en) * | 2021-01-12 | 2021-06-01 | 青岛大学 | Tin telluride nanobelt and preparation method and application thereof |
| CN112875654B (en) * | 2021-01-12 | 2023-04-21 | 青岛大学 | Tin telluride nano belt and preparation method and application thereof |
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Application publication date: 20180105 |