CN107892282A - Lead telluride nanometer rods, the preparation method and applications of a kind of size uniformity - Google Patents
Lead telluride nanometer rods, the preparation method and applications of a kind of size uniformity Download PDFInfo
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- CN107892282A CN107892282A CN201810005926.8A CN201810005926A CN107892282A CN 107892282 A CN107892282 A CN 107892282A CN 201810005926 A CN201810005926 A CN 201810005926A CN 107892282 A CN107892282 A CN 107892282A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention discloses lead telluride nanometer rods, the preparation method and applications of a kind of size uniformity.Lead presoma is combined to form using trans 2 decylenic acid of short chain organic acid and lead oxide, three（Diethylin）Phosphine combines to form tellurium presoma with simple substance tellurium, by regulating and controlling reaction temperature, the ratio of two kinds of presomas of lead tellurium, hot injecting method is used again, synthesis obtains a kind of lead telluride nanometer rods of size uniformity, its a diameter of 2~5 nanometers, length is 10~60 nanometers, and its electronic band is in anisotropy, has extremely strong quantum confined effect.Lead telluride nanometer rods provided by the invention have good dissolubility in n-hexane solvent, and application field is more extensive, easy to use.The lead telluride nanometer rods that the logical present invention synthesizes UV, visible light near-infrared absorption spectrum in characteristic absorption peak between 400~550 nm, with special optical property, be advantageous to lead telluride nanometer rods applied in the photoelectricity such as solar cell, photodetector and thermo-electric device.
Description
Technical field
The invention belongs to technical field of nano material, is related to a kind of lead telluride nanometer rods, preparation method and applications, is carried
The lead telluride nanometer rods size uniformity of confession, dissolubility are preferable, have extremely strong quantum confined effect.
Background technology
Lead telluride in narrow band gap lead chalcogen semiconductor material（PbTe）With very big Bohr radius（46 nanometers）, and
Electronics is smaller than hole mass in lead telluride, the space of its size, pattern adjustability is compared lead selenide（PbSe）Bigger, this makes
Its quantum confined effect is particularly significant, while it has dielectric constant height, thermoelectric figure of merit coefficient（ZT）The high, property such as energy level is adjustable
Matter.In addition, the distinctive anisotropic electron band structure of lead telluride promotees to make it have special photoelectric properties.Therefore lead telluride this
Class material has in the photoelectricity such as solar cell, photodetector and thermo-electric device is applied even more extensively prospect.And one
The nanocrystalline of dimension structure has the transmission of more effective electric charge, excellent thermoelectric figure of merit coefficient compared to its zero-dimension structural, make its
The more excellent performance of the device saliency such as photoelectricity, thermoelectricity.2010, " a kind of simple preparation method was by lead telluride nanometer for document
Crystalline substance is changed into club shaped structure from point-like "（Chemical material）Two step colloid methods synthesis lead telluride is reported by point-like to bar-shaped transformation,
In text using the lead salt aqueous solution and sodium hydrogen telluride respectively as lead, tellurium presoma in more than 200 DEG C crystal growths of reaction temperature extremely
Few 2 it is small in the case of grow up to lead telluride nanometer rods（DOI: 10.1021/cm100636b）.2015, Neil C.
Greenham et al. is reported first to be surpassed based on the outer quantum yield of lead telluride materials for solar cells more than 120%, interior quantum yield
Cross 150%, it was demonstrated that telluride lead material has very excellent more exciton multiplier effects（Referring to document：Lead telluride quantum dot solar
The outer quantum yield of battery is more than 120%, nanometer bulletin, DOI: 10.1021/acs.nanolett.5b03161）.
However, it is currently based on low temperature（Less than 200 DEG C）Under the conditions of synthesize lead telluride nanometer rods simple method for preparing not yet
Someone studies report.Because lead telluride has the face-centered cubic crystal structure of high degree of symmetry so that prepare anisotropic growth
There is certain technical barrier in lead telluride nanometer rods, especially synthesize the lead telluride nanometer of size uniformity, diameter less than 5 nanometers
Rod.Once this problem is addressed, it will help people study the potential optical specificity energy of lead telluride nanometer rods, will also have
Help the material to be applied even more extensively in photoelectricity, thermo-electric device.But it is current, using under hot injecting method cryogenic conditions（150
Below DEG C）Synthesis size uniformity, dissolubility are preferably and the lead telluride nanometer rods with extremely strong quantum confined effect have not been reported.
The content of the invention
The present invention prepares size in view of the deficienciess of the prior art, providing under a kind of cryogenic conditions below 150 DEG C
Homogeneous, dissolubility is preferably and lead telluride nanometer rods, preparation method and applications with extremely strong quantum confined effect.
Realize that the technical scheme of the object of the invention is to provide a kind of lead telluride nanometer rods, its molecular formula is PbTe, diameter
For 2~5 nanometers, length is 10~60 nanometers, and the characteristic absorption peak position in UV, visible light-near-infrared absorption spectrum is 400
Between~550 nm.
Technical solution of the present invention also includes a kind of preparation method of lead telluride nanometer rods, and step is as follows：
1）The preparation of lead presoma：It is 1 by the mol ratio of lead oxide and trans unrighted acid under inert gas shielding:2
~6, lead oxide, trans unrighted acid and solvent octadecylene are added in reaction vessel, they are 100~150 DEG C in temperature
Stirring condition under, obtain clear shape solution；Vacuumized under conditions of being again 100~130 DEG C in temperature, except dereaction
After water and oxygen in container, lead presoma is obtained；
2）The preparation of tellurium presoma：By tellurium simple substance and three（Diethylin）Phosphine is configured to the mixed solution that concentration is 1 mole every liter,
Tellurium simple substance is continued stirring until to be completely dissolved；
3）Synthetic reaction：By step 2）Three (diethylin) phosphine mixed solutions of obtained tellurium are dissolved in three（Diethylin）Phosphine and
The in the mixed solvent of octadecylene, after being well mixed, then by the mol ratio of lead oxide and tellurium simple substance it is 1:0.15~5, it is placed in temperature
For 100~150 DEG C of step 1）In obtained lead presoma, reacted 10~90 minutes under stirring condition；
4）Post processing：By step 3）After obtained reactant is down to room temperature, n-hexane is injected into reaction vessel, adds isopropyl
Alcohol precipitates, until reaction solution becomes cloudy, upper liquid is discarded after centrifugal treating, solid vacuum is drained, a kind of lead telluride is obtained and receives
Rice rod.
Repeatable step 4）1~2 time, carry out purification processes.
Described inert gas is any one in nitrogen, helium, neon.
The mol ratio of the lead oxide and trans unrighted acid is 1:2.5.
Described trans unrighted acid is in trans -2- hexenoic acids, trans -2- octenoic acids, trans -2- decylenic acids
Any one.
Described octadecylene, n-hexane, isopropanol are through Non-aqueous processing.
A kind of lead telluride nanometer rods provided by the invention, are used as solar cell, the photoelectricity of field of photodetectors
And in thermo-electric device.
Compared with prior art, the invention has the advantages that：
1. the present invention is using trans unrighted acid as lead presoma, three（Diethylin）Phosphine is combined into tellurium forerunner with tellurium simple substance
Body, a kind of lead telluride nanometer rods are prepared, Size Distribution is homogeneous, and its electronic band is in anisotropy, and has extremely strong quantum confinement
Effect.
2. using a diameter of 2~5 nanometers of lead telluride nanometer rods provided by the invention, length is 10~60 nanometers,
Characteristic absorption peak position is 400~550 nanometers in visible region in UV, visible light-near-infrared absorption spectrum, can be used as the sun
Can battery, field of photodetectors photoelectricity and thermo-electric device in.
3. lead telluride nanometer rods provided by the invention have good dissolubility in n-hexane solvent, clarification is presented in solution
Pellucidity, the preparation technology for making it be applied in electronic device are easier.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture for the lead telluride nanometer rods that the embodiment of the present invention 1 synthesizes at a temperature of 100 DEG C；
Fig. 2 is the photo of the hexane solution for the lead telluride nanometer rods that the embodiment of the present invention 1 provides；
Fig. 3 is the transmission electron microscope picture for the lead telluride nanometer rods that the embodiment of the present invention 2 synthesizes at a temperature of 120 DEG C；
Fig. 4 is the transmission electron microscope picture for the lead telluride nanometer rods that the embodiment of the present invention 3 synthesizes at a temperature of 140 DEG C；
Fig. 5 is the X-ray diffraction spectrogram of lead telluride nanometer rods provided in an embodiment of the present invention；
Fig. 6 be various embodiments of the present invention provide differential responses at a temperature of lead telluride nanometer rods in hexane solution it is ultraviolet-
Visible absorption spectra figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical solution of the present invention is further elaborated.
Embodiment 1：
The present embodiment synthesizes lead telluride nanometer rods under conditions of being 100 DEG C in temperature, comprises the following steps that：
1）The preparation of lead presoma：Under nitrogen protection, by 89 mg（0.4 mmol）Lead oxide, 170 mg（1 mmol）Trans-
2- decylenic acids and 8 g octadecylenes are added in 50 mL three-necked flasks, are stirred 1 hour under conditions of being 120 DEG C in temperature, until
Solution becomes clear shape, then vacuumize process 1 hour under conditions of temperature is 110 DEG C, removes the water in three-necked flask
And oxygen, lead presoma is obtained, it is stand-by；
2）The preparation of tellurium presoma：In nitrogen glove box, by 153 mg（1.2 mmol）Tellurium simple substance is added to equipped with 1.2 ml
Three（Diethylin）In the vial of phosphine, it is stirred at room temperature, until tellurium simple substance is dissolved completely in solution, obtains tellurium forerunner
Body, it is stand-by；
3）Synthetic reaction under default lead tellurium presoma ratio, temperature conditionss：By 60 μ L tellurium presomas（Molar concentration is 1
mol/L）It is dissolved in 1.14 ml tri-（Diethylin）In phosphine and 1.2 ml octadecylenes, it is rapidly injected after well mixed with syringe
To being pre-adjusted into 100 DEG C of lead presoma, react 80 minutes；
4）Post processing：After being down to room temperature using water-bath, 5mL n-hexanes are injected into three-necked flask, reaction solution is transferred to gloves
In case, isopropanol precipitating is added, then through centrifuge（8000rpm）Centrifugation discards upper liquid after 5 minutes, then with n-hexane dissolution,
Centrifuged 5 minutes after adding isopropanol, discard upper liquid, the solid vacuum that centrifugation obtains is drained, obtains size uniformity lead telluride
Nanometer rods, it is placed in glove box and preserves.
Referring to accompanying drawing 1, it is the lead selenide nanometer rods that the present embodiment uses 100 DEG C of temperature conditionss synthetic reactions to obtain
Transmission electron microscope picture, as shown in Figure 1, the Size Distribution of the nanometer rods are homogeneous（Diameter is about 2.8nm, and length is about 39nm, aspect ratio
About 14）.
Referring to accompanying drawing 2, it is the photo of the hexane solution of lead telluride nanometer rods manufactured in the present embodiment, and solution colour is
Purple, the state of clear is presented, it was demonstrated that lead telluride nanometer rods have good dissolubility in hexane solution.
Embodiment 2：
The present embodiment synthesizes lead telluride nanometer rods under conditions of being 120 DEG C in temperature, comprises the following steps that：
1）The preparation of lead presoma：Under nitrogen protection, by 89 mg（0.4 mmol）Lead oxide, 170 mg（1 mmol）Trans-
2- decylenic acids and 8 g octadecylenes are added in 50 mL three-necked flasks, are stirred 1 hour at 120 DEG C, until solution becomes to clarify
Transparence, then vacuumized at 110 DEG C 1 hour, remove water and oxygen in three-necked flask, obtain lead presoma, it is stand-by；
2）The preparation of tellurium presoma：In nitrogen glove box, by 153 mg（1.2 mmol）Tellurium simple substance is added to equipped with 1.2 ml
Three（Diethylin）In the vial of phosphine, dissolving is stirred at room temperature, until tellurium simple substance is dissolved completely in solution, before obtaining tellurium
Body is driven, it is stand-by；
3）Default lead tellurium presoma ratio, at a temperature of reaction：By the three of 60 μ L telluriums（Diethylin）Phosphine solution（Molar concentration
For 1 mol/L）It is dissolved in 1.14 ml tri-（Diethylin）It is quick with syringe after being well mixed in phosphine and 1.2 ml octadecylenes
It is injected into and is pre-adjusted into 120 DEG C of above-mentioned lead presoma, reacts 80 minutes；
4）Post processing：After being down to room temperature using water-bath, 5mL n-hexanes are injected into three-necked flask, reaction solution is transferred to gloves
In case, isopropanol precipitating is added, then through centrifuge（8000rpm）Centrifugation discards upper liquid after 5 minutes, then with n-hexane dissolution,
Centrifuged 5 minutes after adding isopropanol, discard upper liquid, the solid vacuum that centrifugation obtains is drained, obtains size uniformity lead telluride
Nanometer rods, it is placed in glove box and preserves.
Referring to accompanying drawing 3, it is the present embodiment with the transmission electron microscope picture of the lead selenide nanometer rods synthesized at a temperature of 120 DEG C, by
Fig. 3 understands that the Size Distribution of the nanometer rods is homogeneous（Diameter is about 3.8nm, and length is about 56nm, and aspect ratio is about 14.7）.
The lead selenide nanometer rods that the present embodiment provides have preferable dissolubility in n-hexane.
Embodiment 3：
The present embodiment synthesizes lead telluride nanometer rods under conditions of being 140 DEG C in temperature, comprises the following steps that：
1）The preparation of lead presoma：Under nitrogen protection, by 89 mg（0.4 mmol）Lead oxide, 170 mg（1 mmol）Trans-
2- decylenic acids and 8 g octadecylenes are added in 50 mL three-necked flasks, are stirred 1 hour at 120 DEG C, until solution becomes to clarify
Transparence, then vacuumized at 110 DEG C 1 hour, remove water and oxygen in three-necked flask, obtain lead presoma, it is stand-by；
2）The preparation of tellurium presoma：In nitrogen glove box, by 153 mg（1.2 mmol）Tellurium simple substance is added to equipped with 1.2 ml
Three（Diethylin）In the vial of phosphine, dissolving is stirred at room temperature, until tellurium simple substance is dissolved completely in solution, before obtaining tellurium
Body is driven, it is stand-by；
3）Default lead tellurium presoma ratio, at a temperature of reaction：By the three of 60 μ L telluriums（Diethylin）Phosphine solution（Molar concentration
For 1 mol/L）It is dissolved in 1.14 ml tri-（Diethylin）It is quick with syringe after being well mixed in phosphine and 1.2 ml octadecylenes
It is injected into and is pre-adjusted into 140 DEG C of above-mentioned lead presoma, reacts 80 minutes；
4）Post processing：After being down to room temperature using water-bath, 5mL n-hexanes are injected into three-necked flask, reaction solution is transferred to gloves
In case, isopropanol precipitating is added, then through centrifuge（8000rpm）Centrifugation discards upper liquid after 5 minutes, then with n-hexane dissolution,
Centrifuged 5 minutes after adding isopropanol, discard upper liquid, the solid vacuum that centrifugation obtains is drained, obtains size uniformity lead telluride
Nanometer rods, it is placed in glove box and preserves.
Referring to accompanying drawing 4, it is the present embodiment with the transmission electron microscope picture of the lead selenide nanometer rods synthesized at a temperature of 140 DEG C, by
Fig. 4 understands that the Size Distribution of the nanometer rods is homogeneous（Diameter is about 5.4nm, and length is about 30nm, and aspect ratio is about 5.5）.
The lead selenide nanometer rods that the present embodiment provides have preferable dissolubility in n-hexane.
Referring to accompanying drawing 5, it is the X-ray diffraction spectrogram of lead telluride nanometer rods prepared by the embodiment of the present invention, with lead telluride
Crystal diffraction peak position is mutually corresponding in crystal PDF card numberings 38-1435.Diffraction peak type is sharp, demonstrates again that lead telluride is received
Rice rod does not have obvious lattice defect.
Referring to accompanying drawing 6, it is purple of the corresponding lead telluride nanometer rods in hexane solution in the embodiment of the present invention 1~3
Outside-visible absorption spectra figure.The first of lead telluride nanometer rods excites peak position from 1182 nm red shifts to 1713 nm with nanometer
Rod diameter rises to 5.4 nm from 2.8 nm.Particularly it is noted that in visible region, lead telluride nanometer rods have obvious special
It is the 3rd excitation peak to levy absworption peak, absorbs peak position and increases from 487 nm red shifts to 549 nm with the length of nanometer rods from 30 nm
Grow to 56 nm.The anisotropy of this peculiar optical property of lead telluride nanometer rods electronic band with itself is relevant, this performance
Possess, be applied more broadly in photoelectricity, thermo-electric device and lay a good foundation for product provided by the invention.
Claims (8)
- A kind of 1. lead telluride nanometer rods, it is characterised in that：Its molecular formula is PbTe, a diameter of 2~5 nanometers, length is 10~ 60 nanometers, the characteristic absorption peak position in UV, visible light-near-infrared absorption spectrum is between 400~550 nm.
- 2. a kind of preparation method of lead telluride nanometer rods as claimed in claim 1, it is characterised in that comprise the following steps：1）The preparation of lead presoma：It is 1 by the mol ratio of lead oxide and trans unrighted acid under inert gas shielding:2 ~6, lead oxide, trans unrighted acid and solvent octadecylene are added in reaction vessel, they are 100~150 DEG C in temperature Stirring condition under, obtain clear shape solution；Vacuumized under conditions of being again 100~130 DEG C in temperature, except dereaction After water and oxygen in container, lead presoma is obtained；2）The preparation of tellurium presoma：By tellurium simple substance and three（Diethylin）Phosphine is configured to the mixed solution that concentration is 1 mole every liter, Tellurium simple substance is continued stirring until to be completely dissolved；3）Synthetic reaction：By step 2）Three (diethylin) phosphine mixed solutions of obtained tellurium are dissolved in three（Diethylin）Phosphine and The in the mixed solvent of octadecylene, after being well mixed, then by the mol ratio of lead oxide and tellurium simple substance it is 1:0.15~5, it is placed in temperature For 100~150 DEG C of step 1）In obtained lead presoma, reacted 10~90 minutes under stirring condition；4）Post processing：By step 3）After obtained reactant is down to room temperature, n-hexane is injected into reaction vessel, adds isopropyl Alcohol precipitates, until reaction solution becomes cloudy, upper liquid is discarded after centrifugal treating, solid vacuum is drained, a kind of lead telluride is obtained and receives Rice rod.
- A kind of 3. preparation method of lead telluride nanometer rods according to claim 2, it is characterised in that：Described inert gas For any one in nitrogen, helium, neon.
- A kind of 4. preparation method of lead telluride nanometer rods according to claim 2, it is characterised in that：The lead oxide with it is anti- The mol ratio of formula unrighted acid is 1:2.5.
- A kind of 5. preparation method of lead telluride nanometer rods according to claim 2, it is characterised in that：Described trans insatiable hunger It is any one in trans -2- hexenoic acids, trans -2- octenoic acids, trans -2- decylenic acids with aliphatic acid.
- A kind of 6. preparation method of lead telluride nanometer rods according to claim 2, it is characterised in that：Described octadecylene, N-hexane, isopropanol are through Non-aqueous processing.
- A kind of 7. preparation method of lead telluride nanometer rods according to claim 2, it is characterised in that：Repeat step 4）1~2 It is secondary, carry out purification processes.
- 8. a kind of application of lead telluride nanometer rods as claimed in claim 1, it is characterised in that be used as solar cell, light In the photoelectricity and thermo-electric device in electric explorer field.
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| CN110451464A (en) * | 2019-08-18 | 2019-11-15 | 王杰 | A kind of preparation method of lead telluride nanometer rods |
| CN113755174A (en) * | 2021-09-26 | 2021-12-07 | 杭州师范大学 | Lead telluride quantum dot and preparation method and application thereof |
| CN114620693A (en) * | 2022-03-04 | 2022-06-14 | 浙大城市学院 | Controllable growth method of lead selenide nanorod based on hydrophobic synthesis system |
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| CN110451464A (en) * | 2019-08-18 | 2019-11-15 | 王杰 | A kind of preparation method of lead telluride nanometer rods |
| CN113755174A (en) * | 2021-09-26 | 2021-12-07 | 杭州师范大学 | Lead telluride quantum dot and preparation method and application thereof |
| CN113755174B (en) * | 2021-09-26 | 2023-10-20 | 杭州师范大学 | Lead telluride quantum dot and preparation method and application thereof |
| CN114620693A (en) * | 2022-03-04 | 2022-06-14 | 浙大城市学院 | Controllable growth method of lead selenide nanorod based on hydrophobic synthesis system |
| CN114620693B (en) * | 2022-03-04 | 2023-08-22 | 浙大城市学院 | Controllable growth method of lead selenide nano rod based on hydrophobic synthesis system |
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| CN107892282B (en) | 2020-11-17 |
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