CN107098398A - A kind of FeS2The preparation method of nano wire - Google Patents
A kind of FeS2The preparation method of nano wire Download PDFInfo
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- CN107098398A CN107098398A CN201710288577.0A CN201710288577A CN107098398A CN 107098398 A CN107098398 A CN 107098398A CN 201710288577 A CN201710288577 A CN 201710288577A CN 107098398 A CN107098398 A CN 107098398A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention discloses a kind of FeS2The preparation method of nano wire, including：1) take containing Fe3+、OH‑Solution, after hydro-thermal reaction, isolated FeOOH；2) step 1) obtained FeOOH heating responses, cooling obtains Fe2O3Nano wire；3) step 2) obtained Fe2O3Nano wire is mixed with sulphur sample, and vulcanization reaction obtains FeS2Nano wire；The FeS2Nano wire purity is high, and photoelectric properties are good, and pattern is uniform.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to FeS2The preparation method of nano wire.
Background technology
FeS2As a kind of semi-conducting material for having and being adapted to energy gap and high light absorption coefficient, in photovoltaic applications side
Face is attracted wide attention.FeS2Input practical application receives the too low influence of its photoelectric transformation efficiency.And FeS2It will produce
Nano wire, works as FeS2When nano wire is by photon irradiation more than bandwidth, photon-hole is to that will produce, if being adapted to
Surface defect state capture electronics or hole, the compound of electron-hole pair will be prevented from, and the oxidation-reduction process on surface is obtained
To carry out, reduction is combined caused by passing through multinomial multi phase interface, so as to improve the transformation efficiency of solar cell.
At present, FeS is prepared2Nano wire reacts direct frequently with method is directly prepared by physics or chemical method Fe and S
Synthesis obtains FeS2Nano wire, obtains FeS2The excessive phase of presence of nano wire, causes its photoelectric properties to decline.
The content of the invention
In view of this, this application provides a kind of FeS2The preparation method of nano wire, the FeS2Nano wire purity is high, light
Good electrical property, pattern is uniform.
To solve above technical problem, the technical scheme that the present invention is provided is to provide a kind of FeS2The preparation side of nano wire
Method, including：
1) take containing Fe3+、OH-Solution, after hydro-thermal reaction, isolated FeOOH；
2) step 1) obtained FeOOH heating responses, cooling obtains Fe2O3Nano wire；
3) step 2) obtained Fe2O3Nano wire is mixed with sulphur sample, and vulcanization reaction obtains FeS2Nano wire.
It is preferred that, the step 1) also obtain described containing Fe including taking molysite and highly basic to be dissolved in water3+、OH-Solution.
It is preferred that, the molysite is FeCl3And/or Fe (NO3)3。
It is preferred that, the highly basic is NaOH and/or KOH.
It is preferred that, the step 1) described in hydro-thermal reaction solvent be H2O。
It is preferred that, the step 1) described in hydro-thermal reaction pressure be 0.5~1.5MPa.
It is preferred that, the step 1) described in hydrothermal temperature be 100~200 DEG C.
It is preferred that, the step 1) described in hydro-thermal reaction carried out in autoclave.
It is preferred that, the step 1) described in hydrothermal temperature be 160 DEG C.
It is preferred that, the step 1) described in the hydro-thermal reaction time be 2h.
It is preferred that, it is described to contain Fe3+、OH-Solution in Fe3+With OH-Mol ratio is 1:(1~12).
It is preferred that, the step 1) in Fe3+With OH-Mol ratio is 1:8.
It is preferred that, the step 1) in separation process using centrifuge.
It is preferred that, the step 1) it is specially to take containing Fe3+、OH-Solution, stirring, it is isolated after hydro-thermal reaction
FeOOH。
It is preferred that, the mixing time is 30min.
It is preferred that, the step 2) described in heating response temperature be 200~400 DEG C.
It is preferred that, the step 2) described in the heating response time be 3h.
It is preferred that, the step 2) be specially：It is passed through H2With Ar mixed gas, by the step 1) obtained FeOOH adds
Thermal response, cooling obtains Fe2O3Nano wire.
It is preferred that, the H2In Ar mixed gas, Ar contents are that 93vol% and H2 contents are 7vol%.
It is preferred that, the step 3) described in sulphur sample be sulphur powder.
It is preferred that, the sulphur powder is sublimed sulfur.
It is preferred that, the step 3) described in vulcanization reaction temperature be less than or equal to 400 DEG C.
It is preferred that, the step 3) described in vulcanization reaction temperature be 200~400 DEG C.
It is preferred that, the step 3) described in the vulcanization reaction time be 0.5~2h.
It is preferred that, the step 3) described in vulcanization reaction carried out in vacuum tube tube furnace.
It is preferred that, S contents and the Fe in the sulphur sample2O3The mol ratio of nano wire be more than 11:2.
Compared with prior art, its detailed description is as follows by the application：The FeOOH that the application is synthesized by hydro-thermal reaction heats anti-
The Fe that should be obtained2O3Nano wire；Be conducive to growing defect under hydrothermal reaction condition less, go to be orientated, the high crystalline substance of crystallinity
Body；Pass through reaction temperature and the reaction time of the reaction pressure, reaction temperature and reaction time of hydro-thermal reaction, and heating response
Regulation can be achieved to Fe2O3The control of nano wire stoichiometric(al) and structural form；Therefore, the Fe obtained2O3Nano wire pattern is equal
Even, dispersiveness is preferably.Again by the Fe of regular appearance2O3Nano wire vulcanizing treatment, with sulphur sample mixing vulcanization reaction, obtains pattern rule
The FeS of whole even structure2Nano wire, it is to avoid excessive phase Fe1-xS appearance phase is purer, FeS2Make after nanometer line absorption photon
Electronics produces the electronics that can be moved freely in conduction band, can freely moved while being left in valence band from valence to conduction band
Dynamic hole, the generation in electronics-hole pair improves semiconductor carriers concentration, so as to produce photoconductive signal, photo electric
Can be excellent.
The reaction of the application preparation method is gentle, simple to operation, is applicable to scale industrial production.
Embodiment
In order that those skilled in the art more fully understands the technical scheme of the application, below will be to the embodiment of the present invention
In technical scheme carry out clear, complete description, it is clear that described embodiment is only a part of embodiment of the invention,
Rather than whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art are not making creative work
Under the premise of the every other embodiment that is obtained, belong to the scope of protection of the invention.
Embodiment 1
A kind of FeS2The preparation method of nano wire, it is characterised in that including：
1) take containing Fe3+、OH-Solution, stir 30min, be transferred to hydro-thermal reaction in autoclave, be centrifugally separating to obtain
FeOOH；The hydro-thermal reaction solvent is H2O；The hydrothermal temperature be 160 DEG C, the hydro-thermal reaction pressure be 0.5~
1.5MPa, the hydro-thermal reaction time is 2h；It is described to contain Fe3+、OH-Solution in Fe3+With OH-Mol ratio is 1:8；
2) step 2) be specially：It is passed through H2With Ar mixed gas, by the step 1) obtained FeOOH heating is anti-
Should, 15~30 DEG C are cooled down, Fe is obtained2O3Nano wire；The H2In Ar mixed gas, Ar contents are that 93vol% and H2 contents are
7vol%；The heating response temperature is 300 DEG C, and the heating response time is 3h；
3) step 2) step 3) be specially by the step 2) obtained Fe2O3Nano wire is mixed with sulphur sample, sulphur
Change reaction, obtain FeS2Nano wire；Content and the Fe in the sulphur sample2O3The mol ratio of nano wire be more than 11:2；The sulphur
Sample is sulphur powder, and the sulphur powder is sublimed sulfur；S contents and the Fe in the sulphur sample2O3The mol ratio of nano wire be more than 11:2；
The vulcanization reaction temperature is 200 DEG C, and the vulcanization reaction time is 1h；The vulcanization reaction enters in vacuum tube tube furnace
OK；
Wherein, the step 1) also obtain described containing Fe including taking molysite and highly basic to be dissolved in water3+、OH-Solution, the iron
Salt is FeCl3And/or Fe (NO3)3, the highly basic is NaOH and/or KOH.
Embodiment 2
The present embodiment is in addition to following characteristics, and other are same as Example 1：The hydrothermal temperature is 100 DEG C.
Embodiment 3
The present embodiment is in addition to following characteristics, and other are same as Example 1：The hydrothermal temperature is 200 DEG C.
Embodiment 4
The present embodiment is in addition to following characteristics, and other are same as Example 1：The heating response temperature is 200 DEG C.
Embodiment 5
The present embodiment is in addition to following characteristics, and other are same as Example 1：The heating response temperature is 400 DEG C.
Embodiment 6
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction temperature is 300 DEG C.
Embodiment 7
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction temperature is 350 DEG C.
Embodiment 8
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction temperature is 400 DEG C.
Embodiment 9
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction time is 0.5h.
Embodiment 10
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction time is 1.5h.
Embodiment 11
The present embodiment is in addition to following characteristics, and other are same as Example 1：The vulcanization reaction time is 2h.
Embodiment 12
The present embodiment is in addition to following characteristics, and other are same as Example 1：It is described to contain Fe3+、OH-Solution in Fe3+With
OH-Mol ratio is 1:1.
Embodiment 13
The present embodiment is in addition to following characteristics, and other are same as Example 1：It is described to contain Fe3+、OH-Solution in Fe3+With
OH-Mol ratio is 1:12.
Embodiment 14
Preparation process reaction temperature is to FeS2The influence of nano wire purity
1st, laboratory sample：FeS described in embodiment 1~82Nano wire sample；
2nd, experimental method：Thickness, width, length are measured, and according to RIR thing phase method calculated purities；
2nd, experimental result：It is shown in Table 1.
The reaction temperature of table 1 is to FeS2The influence result of nano wire purity
Embodiment 15
The preparation process vulcanization reaction time is to FeS2The influence of nano wire purity
1st, laboratory sample：FeS described in embodiment 1,9~112Nano wire sample；
2nd, experimental method：Thickness, width, length are measured, and according to RIR thing phase method calculated purities；
3rd, experimental result：It is shown in Table 2.
The vulcanization reaction time of table 2 is to FeS2The influence result of nano wire purity
| Battery sample | The vulcanization reaction time (DEG C) | Purity (%) | Width (nm) | Length (nm) |
| Embodiment 1 | 1 | 95 | 50 | 500 |
| Embodiment 9 | 0.5 | 50 | 50 | 500 |
| Embodiment 10 | 1.5 | 95 | 50 | 500 |
| Embodiment 11 | 2 | 95 | 50 | 500 |
Embodiment 16
Containing Fe3+、OH-Solution in Fe3+With OH-Mol ratio is to FeS2The influence of nano wire purity
1st, laboratory sample：FeS described in embodiment 1,12~132Nano wire sample；
2nd, experimental method：Thickness, width, length are measured, and according to RIR thing phase method calculated purities；
2nd, experimental result：It is shown in Table 3.
Table 3 contains Fe3+、OH-Solution in Fe3+With OH-Mol ratio is to FeS2The influence of nano wire purity
| Battery sample | Fe3+With OH-Mol ratio | Purity (%) | Width (nm) | Length (nm) |
| Embodiment 1 | 1：8 | 95 | 50 | 500 |
| Embodiment 12 | 1：12 | 90 | 20 | 700 |
| Embodiment 13 | 1：1 | 72 | 150 | 300 |
The sample purity of embodiment 1 as can be seen from the above data is higher, i.e. FeS2Nano wire Fe3+With OH-Mol ratio is
1:When 8, its purity is higher, is preferred scheme.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of FeS2The preparation method of nano wire, it is characterised in that including：
1) take containing Fe3+、OH-Solution, after hydro-thermal reaction, isolated FeOOH；
2) step 1) obtained FeOOH heating responses, cooling obtains Fe2O3Nano wire；
3) step 2) obtained Fe2O3Nano wire is mixed with sulphur sample, and vulcanization reaction obtains FeS2Nano wire.
2. preparation method according to claim 1, it is characterised in that the step 1) also include taking molysite and highly basic to be dissolved in
Water obtains described containing Fe3+、OH-Solution.
3. preparation method according to claim 1, it is characterised in that the step 1) described in hydrothermal temperature be
100~200 DEG C.
4. preparation method according to claim 1, it is characterised in that described to contain Fe3+、OH-Solution in Fe3+With OH-Rub
You are than being 1:(1~12).
5. preparation method according to claim 1, it is characterised in that the step 2) described in heating response temperature be
200~400 DEG C.
6. preparation method according to claim 1, it is characterised in that the step 2) be specially：It is passed through H2With Ar gaseous mixtures
Body, by the step 1) obtained FeOOH heating responses, cooling obtains Fe2O3Nano wire.
7. preparation method according to claim 1, it is characterised in that the step 3) described in sulphur sample be sulphur powder.
8. preparation method according to claim 7, it is characterised in that the step 3) described in vulcanization reaction temperature be less than
Equal to 400 DEG C.
9. preparation method according to claim 7, it is characterised in that the step 3) described in the vulcanization reaction time be
0.5~2h.
10. preparation method according to claim 7, it is characterised in that the step 3) described in S contents and institute in sulphur sample
State Fe2O3The mol ratio of nano wire is more than 11:2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675357A (en) * | 2018-06-28 | 2018-10-19 | 福州大学 | A kind of preparation method and applications of inorganic hole transporter ferrous disulfide |
| CN110064408A (en) * | 2019-06-04 | 2019-07-30 | 东华理工大学 | A kind of preparation method for the alpha-crystal form FeOOH catalyst having loaded iron sulfide |
| CN116161708A (en) * | 2022-12-16 | 2023-05-26 | 浙江工业大学 | Preparation method for synthesizing pyrite by hydrothermal method |
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| CN102134103A (en) * | 2011-02-18 | 2011-07-27 | 中山火炬职业技术学院 | Method for preparing hydroxyl iron oxide nanowire |
| CN103872186A (en) * | 2014-03-19 | 2014-06-18 | 浙江大学 | FeS2 thin film and preparation method thereof |
| CN104475116A (en) * | 2014-11-24 | 2015-04-01 | 中国人民解放军军械工程学院 | Preparation method of stannic oxide nanowire-decorated ferric oxide nanorod array |
| CN104638067A (en) * | 2015-02-09 | 2015-05-20 | 浙江大学 | Preparation method of FeS2 nanotube film |
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2017
- 2017-04-27 CN CN201710288577.0A patent/CN107098398A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102134103A (en) * | 2011-02-18 | 2011-07-27 | 中山火炬职业技术学院 | Method for preparing hydroxyl iron oxide nanowire |
| CN103872186A (en) * | 2014-03-19 | 2014-06-18 | 浙江大学 | FeS2 thin film and preparation method thereof |
| CN104475116A (en) * | 2014-11-24 | 2015-04-01 | 中国人民解放军军械工程学院 | Preparation method of stannic oxide nanowire-decorated ferric oxide nanorod array |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675357A (en) * | 2018-06-28 | 2018-10-19 | 福州大学 | A kind of preparation method and applications of inorganic hole transporter ferrous disulfide |
| CN110064408A (en) * | 2019-06-04 | 2019-07-30 | 东华理工大学 | A kind of preparation method for the alpha-crystal form FeOOH catalyst having loaded iron sulfide |
| CN110064408B (en) * | 2019-06-04 | 2021-11-02 | 东华理工大学 | Preparation method of iron sulfide-loaded alpha crystal form iron oxyhydroxide catalyst |
| CN116161708A (en) * | 2022-12-16 | 2023-05-26 | 浙江工业大学 | Preparation method for synthesizing pyrite by hydrothermal method |
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Application publication date: 20170829 |