CN102807194B - Method for preparing lead tin selenide nanoflowers - Google Patents
Method for preparing lead tin selenide nanoflowers Download PDFInfo
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- CN102807194B CN102807194B CN201210271631.8A CN201210271631A CN102807194B CN 102807194 B CN102807194 B CN 102807194B CN 201210271631 A CN201210271631 A CN 201210271631A CN 102807194 B CN102807194 B CN 102807194B
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- acetate
- nanoflowers
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- 239000002057 nanoflower Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title abstract description 11
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 title abstract 5
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 8
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 24
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 claims description 22
- JEHCHYAKAXDFKV-UHFFFAOYSA-J lead tetraacetate Chemical compound CC(=O)O[Pb](OC(C)=O)(OC(C)=O)OC(C)=O JEHCHYAKAXDFKV-UHFFFAOYSA-J 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 8
- -1 octadecylene Chemical group 0.000 claims description 7
- 239000000243 solution Substances 0.000 abstract description 22
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 229940046892 lead acetate Drugs 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 241000500881 Lepisma Species 0.000 description 5
- 229910000679 solder Inorganic materials 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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Abstract
The invention relates to a method for preparing lead tin selenide nanoflowers in the technical field of a photoelectric material, which comprises the following steps of: step 1: mixing lead acetate and tin acetate, and then adding oleylamine and octadecene, and heating to obtain a solution A; step 2: adding tri-n-octylphosphine into selenium powder and then heating to obtain a solution B; and step 3: adding the solution B into the solution A, heating and purifying to obtain the lead tin selenide nanoflowers. The method provided by the invention is capable of synthesizing the lead tin selenide nanoflowers with adjustable spaces; and moreover, the method provided by the invention is a thermal injection synthesizing method, which is environmental-friendly, free from pollution and simple in requirements on devices, so that the lead tin selenide nanoflowers are suitable for industrial mass production.
Description
Technical field
The invention belongs to photoelectric material technical field, specifically a kind of preparation method of lead selenide tin nanoflower.
Background technology
Selenizing slicker solder (PbSnSe), owing to having larger exciton Bohr radius, more satisfactory band gap and the plurality of advantages such as more rich reserves on earth, is considered to the potential material of photoelectron device.By controlling element ratio that is plumbous and tin when synthesizing selenizing slicker solder, can realize being regulated band gap by the change of composition well, and continuously adjustable band gap one of most important character of photoelectric device just.Regulating the mode of band-gap energy not merely to have constituent adjustment a kind of, is also a kind of effective means to the control of the microscopic appearance of product.
Through finding the literature search of prior art, Harman T.C. etc. are at " Applied Physics letters " (Applied Physics bulletin) the 14th volume o. 11th in 1969 the 333 to 334 page of article " Temperature and compositional dependence of laser emission in PbSnSe " (temperature and composition are on the impact of the lasing behavior of selenizing slicker solder) delivered.Afterwards, researchist has synthesized the selenizing slicker solder of the pattern such as film like, band shape, but these products can only show a kind of pattern of macroscopic view substantially, lacks microscale, the especially structural characterization of nanometer scale.Therefore, proposing one can prepare in a large number, with low cost, has the selenizing slicker solder preparation method of certain nanostructure, significant for this area.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of lead selenide tin nanoflower is provided.Method of the present invention is pollution-free, and reaction conditions is gentle simple, and its physical properties can change with mixing the change of tin ratio.
The present invention is achieved by the following technical solutions, comprises the following steps:
Step one, gets plumbic acetate and tin acetate, mixing, then adds oleyl amine and octadecylene, and heating, obtains solution A;
Step 2, gets selenium powder, adds tri-n-octyl phosphine, post-heating, obtain solution B;
Step 3, joins solution B in solution A, and heating, purifying, obtains lead selenide tin nanoflower.
Preferably, in step one, described plumbic acetate: tin acetate=(0.125 ~ 2): 1; Described ratio is mol ratio.
Preferably, in step one, the total mole number of described oleyl amine and octadecylene add-on is 60 ~ 100 times of plumbic acetate and tin acetate total mole number.
Preferably, in step one, described in be heated to be: be heated to 280 ~ 320 DEG C, be incubated 1 ~ 3 hour afterwards.
Preferably, in step 2, described in be heated to be: be heated to 80 ~ 100 DEG C, be incubated 1 ~ 3 hour afterwards.
Preferably, described selenium powder: plumbic acetate and tin acetate summation=1:1; Described ratio is mol ratio.
Preferably, in step 3, the diameter of described lead selenide tin nanoflower is 40 ~ 60nm.
Compared with prior art, the present invention has following beneficial effect: method of the present invention can synthesize the adjustable lead selenide tin nanoflower of band gap, and method of the present invention is heat injection synthetic method, green non-pollution, equipment requirements is simple, is applicable to industrialization scale operation.
Accompanying drawing explanation
Fig. 1 is the TEM collection of illustrative plates of lead selenide tin nanoflower prepared by embodiment 1;
Fig. 2 is the TEM collection of illustrative plates of lead selenide tin nanoflower prepared by embodiment 2;
Fig. 3 is the TEM collection of illustrative plates of lead selenide tin nanoflower prepared by embodiment 3;
Embodiment
Following instance will the invention will be further described by reference to the accompanying drawings.The present embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.
Embodiment 1
The present embodiment relates to a kind of preparation method of lead selenide tin nanoflower, and concrete steps are as follows:
Step one, gets 0.25mmol plumbic acetate and 2mmol tin acetate, mixing, then adds 67.5mmol oleyl amine and 67.5mmol octadecylene, is heated to 280 ° of C, keeps 3 hours, obtain solution A;
Step 2, gets 2.25mmol selenium powder, adds 1.25mmol tri-n-octyl phosphine, is heated to 80 ° of C afterwards, keeps 3 hours, obtains solution B;
Step 3, joins solution B in solution A, is heated to 280 ° of C afterwards, keeps 5 minutes; The product obtained is dissolved in ethanol, under 8000rpm centrifugal 10 minutes, gets lower sediment, add chloroform, under 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol, under 8000rpm after centrifugal 10 minutes; Get lower sediment, after solvent evaporated, obtain lead selenide tin nanoflower.
Prepare the transmission electron microscope photo of product as shown in Figure 1, the diameter of lead selenide tin nanoflower is 40 ~ 60nm.
Embodiment 2
The present embodiment relates to a kind of preparation method of lead selenide tin nanoflower, and concrete steps are as follows:
Step one, gets 1mmol plumbic acetate and 1mmol tin acetate, mixing, then adds 80mmol oleyl amine and 80mmol octadecylene, is heated to 300 ° of C, keeps 2 hours, obtain solution A;
Step 2, gets 2mmol selenium powder, adds 1.25mmol tri-n-octyl phosphine, is heated to 90 ° of C afterwards, keeps 2 hours, obtains solution B;
Step 3, joins solution B in solution A, is heated to 280 ° of C afterwards, keeps 5 minutes; The product obtained is dissolved in ethanol, under 8000rpm centrifugal 10 minutes, gets lower sediment, add chloroform, under 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol, under 8000rpm after centrifugal 10 minutes; Get lower sediment, after solvent evaporated, obtain lead selenide tin nanoflower.
Prepare the transmission electron microscope photo of product as shown in Figure 2, the diameter of lead selenide tin nanoflower is 40 ~ 60nm.
Embodiment 3
The present embodiment relates to a kind of preparation method of lead selenide tin nanoflower, and concrete steps are as follows:
Step one, gets 1.33mmol plumbic acetate and 0.67mmol tin acetate, mixing, then adds 100mmol oleyl amine and 100mmol octadecylene, is heated to 320 ° of C, keeps 1 hour, obtain solution A;
Step 2, gets 2mmol selenium powder, adds 1.25mmol tri-n-octyl phosphine, is heated to 100 ° of C afterwards, keeps 1 hour, obtains solution B;
Step 3, joins solution B in solution A, is heated to 280 ° of C afterwards, keeps 5 minutes; The product obtained is dissolved in ethanol, under 8000rpm centrifugal 10 minutes, gets lower sediment, add chloroform, under 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol, under 8000rpm after centrifugal 10 minutes; Get lower sediment, after solvent evaporated, obtain lead selenide tin nanoflower.
Prepare the transmission electron microscope photo of product as shown in Figure 3, the diameter of lead selenide tin nanoflower is 40 ~ 60nm.
In sum, method of the present invention can synthesize the adjustable lead selenide tin nanoflower of band gap, and method of the present invention is heat injection synthetic method, and green non-pollution, equipment requirements is simple, is applicable to industrialization scale operation.
Claims (1)
1. a preparation method for lead selenide tin nanoflower, is characterized in that, comprises the steps:
Step one, gets plumbic acetate and tin acetate, mixing, then adds oleyl amine and octadecylene, and heating, obtains solution A;
Step 2, gets selenium powder, adds tri-n-octyl phosphine, post-heating, obtain solution B;
Step 3, joins solution B in solution A, heating, and purifying, obtains lead selenide tin nanoflower; The diameter of described lead selenide tin nanoflower is 40 ~ 60nm;
In step one, described plumbic acetate: tin acetate=(0.125 ~ 2): 1; Described ratio is mol ratio;
In step one, the total mole number of described oleyl amine and octadecylene add-on is 60 ~ 100 times of plumbic acetate and tin acetate total mole number;
In step one, described in be heated to be: be heated to 280 ~ 320 DEG C, be incubated 1 ~ 3 hour afterwards;
In step 2, described in be heated to be: be heated to 80 ~ 100 DEG C, be incubated 1 ~ 3 hour afterwards;
Described selenium powder: plumbic acetate and tin acetate summation=1:1; Described ratio is mol ratio.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210271631.8A CN102807194B (en) | 2012-08-01 | 2012-08-01 | Method for preparing lead tin selenide nanoflowers |
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| CN201210271631.8A CN102807194B (en) | 2012-08-01 | 2012-08-01 | Method for preparing lead tin selenide nanoflowers |
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| CN102807194B true CN102807194B (en) | 2015-05-20 |
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| RU2552588C1 (en) * | 2013-11-14 | 2015-06-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | METHOD FOR MAKING PbSnSe SUBSTITUTION SOLID SOLUTION FILMS BY ION EXCHANGE PROCESS |
| CN107792839B (en) * | 2017-10-18 | 2021-01-29 | 苏州大学 | Lead selenide nanorod, preparation method and application in field effect transistor |
| CN109880624B (en) * | 2019-04-18 | 2020-07-10 | 武汉理工大学 | Preparation method of subminiature PbSe quantum dot |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070183A (en) * | 2007-05-24 | 2007-11-14 | 上海大学 | Electronic-beam radiation synthesizing method for nano lead-selenide |
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| US20110033368A1 (en) * | 2007-10-05 | 2011-02-10 | Agency For Science, Technology And Research | Methods of forming a nanocrystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101070183A (en) * | 2007-05-24 | 2007-11-14 | 上海大学 | Electronic-beam radiation synthesizing method for nano lead-selenide |
Non-Patent Citations (1)
| Title |
|---|
| William W. Yu et al,.Preparation and Characterization of Monodisperse PbSe Semiconductor Nanocrystals in a Noncoordinating Solvent.《Chem. Mater.》.2004,第16卷(第17期),3318-3322. * |
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