CN102765704A - Preparation method of tin-doped lead selenide nanoparticle - Google Patents
Preparation method of tin-doped lead selenide nanoparticle Download PDFInfo
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- CN102765704A CN102765704A CN2012102703407A CN201210270340A CN102765704A CN 102765704 A CN102765704 A CN 102765704A CN 2012102703407 A CN2012102703407 A CN 2012102703407A CN 201210270340 A CN201210270340 A CN 201210270340A CN 102765704 A CN102765704 A CN 102765704A
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- tin
- lead selenide
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- tin dope
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- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 40
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 39
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 23
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 12
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005642 Oleic acid Substances 0.000 claims abstract description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-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
- 239000002245 particle Substances 0.000 claims description 16
- -1 octadecylene Chemical group 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 229910000464 lead oxide Inorganic materials 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 abstract 1
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 2
- 229910002665 PbTe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KBPGBEFNGHFRQN-UHFFFAOYSA-N bis(selanylidene)tin Chemical compound [Se]=[Sn]=[Se] KBPGBEFNGHFRQN-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of a tin-doped lead selenide nanoparticle, belonging to the technical field of a photoelectric material. The preparation method comprises the following steps: step 1, lead oxide and tin oxide are taken out and mixed, and oleic acid and octadecene are added in the mixture to obtain solution A; step 2, selenium powder is taken and added with tri-n-octyl phosphine, and the mixture is heated to obtain solution B; and step 3, the solution B is injected into the solution A, and the mixed solution is heated and purified to obtain the tin-doped lead selenide nanoparticle. The method provided by the invention is free from pollution; the reaction conditions are mild and simple; and the requirements to the device are simple, so that the method is fit for industrial large-scale production. As for the prepared tin-doped lead selenide nanoparticle, the band-gap energy can vary according to the tin doping ratio basically in linear relation; and when the tin content is raised from 0 to 42%, the band-gap energy can be reduced from 1.61eV to 0.79eV.
Description
Technical field
The invention belongs to the photovaltaic material technical field, be specifically related to a kind of tin dope lead selenide nanometer particle process method.
Background technology
In recent years, because the band gap of its relative narrower and bigger exciton Bohr radius, IV-VI family semi-conductor is considered to the potential equivalent material of solar cell film light-absorption layer.Wherein, the correlative study of Tin diselenide (SnSe), lead selenide (PbSe), lead telluride binary compounds such as (PbTe) is reported widely.Yet photoelectric device is exactly continuously adjustable band gap in one of most important character of application facet, and this but is that binary compounds such as lead selenide are difficult to realize.If lead selenide is carried out tin dope, just can regulate band-gap energy through the variation of composition well.
Literature search through to prior art is found; Harman T.C. etc. are at " Applied Physics letters " (Applied Physics wall bulletin) 1969 the 14th volumes the 333rd～334 page of article of delivering of o. 11th " Temperature and compositional dependence of laser emission in PbSnSe " (temperature and composition are to the influence of the Laser emission characteristic of tin dope lead selenide); And then; The method of multiple tin dope lead selenide preparation such as magnetron sputtering, hot vapor deposition is developed successively, but these method reaction conditionss are harsh.Therefore, with low cost a kind of can the preparation in a large number, eco-friendly tin dope lead selenide nanoparticle preparation method, significant for this area.
Summary of the invention
The objective of the invention is to deficiency, a kind of tin dope lead selenide nanometer particle process method is provided to prior art.Method of the present invention is pollution-free, and reaction conditions is gentle simple, and its band-gap energy can change with mixing the tin ratio: when tin content when 0 rises to 42%, band-gap energy drops to 0.79eV from 1.61eV, and presents linear relationship basically.
The present invention realizes that through following technical scheme the tin dope lead selenide nanometer particle process method that the present invention relates to may further comprise the steps:
Step 1 is got plumbous oxide, and White tin oxide mixes, and adds oleic acid and octadecylene, and heating gets solution A;
Step 2 is got selenium powder, adds tri-n-octyl phosphine, and heating gets solution B;
Step 3 is injected into solution B in the solution A, heating, and purifying obtains tin dope lead selenide nanoparticle.
Preferably, said plumbous oxide: White tin oxide=(0.125～2): 1; Said selenium powder: the summation=1:1 of plumbous oxide and White tin oxide; Said ratio is a mol ratio.
Preferably, in the step 1, the oleic acid of said adding and the total mole number of octadecylene are plumbous oxide and White tin oxide total mole number 5～50 times.
Preferably, in the step 1, said being heated to be: be heated to 230～250 ℃, and be incubated 1～3 hour.
Preferably, in the step 2, said being heated to be: be heated to 50～70 ℃, and be incubated 0.5～2 hour.
Preferably, in the step 3, said being heated to be: be heated to 260～280 ℃, and be incubated 2～10 minutes.
Preferably, the particle diameter of said tin dope lead selenide nanoparticle is 5～30nm.
Compared with prior art; The present invention has following beneficial effect: the synthetic first adjustable tin dope lead selenide nanoparticle of band gap of method of the present invention, and method of the present invention adopts heat injection compound method, green non-pollution; Requirement to equipment is simple, is fit to large-scale industrialization production.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the tin dope lead selenide nanoparticle of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of the tin dope lead selenide nanoparticle of embodiment 2 preparations;
Fig. 3 is the X ray diffracting spectrum of the tin dope lead selenide nanoparticle of embodiment 3 preparations;
Embodiment
Following instance will combine accompanying drawing that the present invention is described further.Present embodiment provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
Present embodiment provides a kind of tin dope lead selenide nanometer particle process method, and step is following:
Step 1 is got 0.25mmol plumbous oxide, 2mmol White tin oxide; Add reaction tubes afterwards, add 2.5mmol oleic acid, 2.5mmol octadecylene again, be heated to 230 ° of C, kept 3 hours; Get solution A;
Step 2 is got another reaction tubes, adds 2mmol selenium powder, 1.25mmol tri-n-octyl phosphine, is heated to 50 ° of C, keeps 2 hours; Get solution B;
Step 3 is injected into solution B in the solution A, is warming up to 260 ° of C and is incubated 2 minutes; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol; Under the 8000rpm centrifugal 10 minutes, take off layer deposition, add chloroform; Under the 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol; Take off layer deposition under the 8000rpm after centrifugal 10 minutes, solvent evaporated obtains tin dope lead selenide nanoparticle.
Implementation result, the tin dope lead selenide diameter of nano particles of present embodiment preparation is 5nm, its X-ray diffractogram is as shown in Figure 1.
Embodiment 2
Present embodiment provides a kind of tin dope lead selenide nanometer particle process method, and step is following:
Step 1 is got 1mmol plumbous oxide, 1mmol White tin oxide; Add reaction tubes afterwards, add 12.5mmol oleic acid, 12.5mmol octadecylene again, be heated to 240 ° of C, kept 1 hour; Get solution A;
Step 2 is got another reaction tubes, adds 2mmol selenium powder, 1.25mmol tri-n-octyl phosphine, is heated to 60 ° of C, keeps 1 hour; Get solution B;
Step 3 is injected into solution B in the solution A, is warming up to 280 ° of C and is incubated 5 minutes; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol; Under the 8000rpm centrifugal 10 minutes, take off layer deposition, add chloroform; Under the 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol; Take off layer deposition under the 8000rpm after centrifugal 10 minutes, solvent evaporated obtains tin dope lead selenide nanoparticle.
Implementation result, the tin dope lead selenide diameter of nano particles of present embodiment preparation is 25nm, its X-ray diffractogram is as shown in Figure 2.
Embodiment 3
Present embodiment provides a kind of tin dope lead selenide nanometer particle process method, and step is following:
Step 1 is got 1.34mmol plumbous oxide, 0.67mmol White tin oxide; Add reaction tubes afterwards, add 25mmol oleic acid, 25mmol octadecylene again, be heated to 250 ° of C, kept 2 hours; Get solution A;
Step 2 is got another reaction tubes, adds 2mmol selenium powder, 1.25mmol tri-n-octyl phosphine, is heated to 70 ° of C, keeps half a hour; Get solution B;
Step 3 is injected into solution B in the solution A, is warming up to 270 ° of C and is incubated 10 minutes; Afterwards, products therefrom is carried out purifying, be specially: product is dissolved in ethanol; Under the 8000rpm centrifugal 10 minutes, take off layer deposition, add chloroform; Under the 7000rpm centrifugal 5 minutes, get supernatant liquid, add ethanol; Take off layer deposition under the 8000rpm after centrifugal 10 minutes, solvent evaporated obtains tin dope lead selenide nanoparticle.
Implementation result, the tin dope lead selenide diameter of nano particles of present embodiment preparation is 30nm, its X-ray diffractogram is as shown in Figure 3.
Simultaneously, verify that find that tin content rises at 42% o'clock from 0, band-gap energy drops to 0.79eV from 1.61eV, and presents linear relationship basically through tin dope lead selenide nanoparticle to embodiment 1-3 preparation.
In sum, the synthetic first adjustable tin dope lead selenide nanoparticle of band gap of method of the present invention, method of the present invention adopts heat injection compound method, and green non-pollution is simple to the requirement of equipment, is fit to large-scale industrialization production.
Claims (7)
1. a tin dope lead selenide nanometer particle process method is characterized in that, comprises the steps:
Step 1 is got plumbous oxide, and White tin oxide mixes, and adds oleic acid and octadecylene, and heating gets solution A;
Step 2 is got selenium powder, adds tri-n-octyl phosphine, and heating gets solution B;
Step 3 is injected into solution B in the solution A, heating, and purifying obtains tin dope lead selenide nanoparticle.
2. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that said plumbous oxide: White tin oxide=(0.125～2): 1; Said selenium powder: the summation=1:1 of plumbous oxide and White tin oxide; Said ratio is a mol ratio.
3. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that, in the step 1, the oleic acid of said adding and the total mole number of octadecylene are plumbous oxide and White tin oxide total mole number 5～50 times.
4. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that, in the step 1, and said being heated to be: be heated to 230～250 ℃, and be incubated 1～3 hour.
5. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that, in the step 2, and said being heated to be: be heated to 50～70 ℃, and be incubated 0.5～2 hour.
6. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that, in the step 3, and said being heated to be: be heated to 260～280 ℃, and be incubated 2～10 minutes.
7. tin dope lead selenide nanometer particle process method according to claim 1 is characterized in that the particle diameter of said tin dope lead selenide nanoparticle is 5～30nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792839A (en) * | 2017-10-18 | 2018-03-13 | 苏州大学 | A kind of application in lead selenide nanometer rods, preparation method and scene effect transistor |
| CN109880624A (en) * | 2019-04-18 | 2019-06-14 | 武汉理工大学 | Preparation method of ultra-small PbSe quantum dots |
| CN114620693A (en) * | 2022-03-04 | 2022-06-14 | 浙大城市学院 | Controllable growth of lead selenide nanorods based on a hydrophobic synthesis system |
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| CN101235546A (en) * | 2007-11-07 | 2008-08-06 | 华东理工大学 | A micro-reaction device and method for synthesizing cadmium selenide nanocrystals using temperature gradient |
| CN101830446A (en) * | 2010-04-30 | 2010-09-15 | 西安交通大学 | Preparation method of PbTe colloid nanocrystalline self-assembly film |
| US20110033368A1 (en) * | 2007-10-05 | 2011-02-10 | Agency For Science, Technology And Research | Methods of forming a nanocrystal |
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Patent Citations (3)
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| US20110033368A1 (en) * | 2007-10-05 | 2011-02-10 | Agency For Science, Technology And Research | Methods of forming a nanocrystal |
| CN101235546A (en) * | 2007-11-07 | 2008-08-06 | 华东理工大学 | A micro-reaction device and method for synthesizing cadmium selenide nanocrystals using temperature gradient |
| CN101830446A (en) * | 2010-04-30 | 2010-09-15 | 西安交通大学 | Preparation method of PbTe colloid nanocrystalline self-assembly film |
Non-Patent Citations (1)
| Title |
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| WILLIAM W. YU ET AL: "Preparation and Characterization of Monodisperse PbSe Semiconductor Nanocrystals in a Noncoordinating Solvent", 《CHEM. MATER.》, vol. 16, no. 17, 17 July 2004 (2004-07-17), pages 3318 - 3322, XP008092382, DOI: doi:10.1021/cm049476y * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792839A (en) * | 2017-10-18 | 2018-03-13 | 苏州大学 | A kind of application in lead selenide nanometer rods, preparation method and scene effect transistor |
| CN109880624A (en) * | 2019-04-18 | 2019-06-14 | 武汉理工大学 | Preparation method of ultra-small PbSe quantum dots |
| CN109880624B (en) * | 2019-04-18 | 2020-07-10 | 武汉理工大学 | Preparation method of ultra-small PbSe quantum dots |
| CN114620693A (en) * | 2022-03-04 | 2022-06-14 | 浙大城市学院 | Controllable growth of lead selenide nanorods based on a hydrophobic synthesis system |
| CN114620693B (en) * | 2022-03-04 | 2023-08-22 | 浙大城市学院 | Controllable Growth Method of Lead Selenide Nanorods Based on Hydrophobic Synthesis System |
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Application publication date: 20121107 |