CN105314686A - FeS nanosheet preparing method - Google Patents
FeS nanosheet preparing method Download PDFInfo
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- CN105314686A CN105314686A CN201510619025.4A CN201510619025A CN105314686A CN 105314686 A CN105314686 A CN 105314686A CN 201510619025 A CN201510619025 A CN 201510619025A CN 105314686 A CN105314686 A CN 105314686A
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Abstract
The invention discloses a FeS nanosheet preparing method. The method comprises the steps of 1, dissolving an iron-containing precursor, a sulfur-containing precursor and a surface active agent in water to obtain a solution, wherein the surface active agent is hexadecyl trimethyl ammonium bromide; 2, transferring the solution obtained in the step 1 into a reaction still to be heated, conducting centrifugation after complete reaction, washing a sample with water and ethyl alcohol, and then obtaining a FeS nanosheet. According to the method, the technology is simple, production cost is low, and the prepared FeS nanosheets have a uniform shape and a thickness of about 3 nm and are suitable for directly preparing a lithium battery electrode material; during preparation, water serves as the solvent, preparation is safe, cost is low, and application and popularization are facilitated.
Description
Technical field
The present invention relates to technical field of nano material, especially a kind of preparation method of FeS nanometer sheet.
Background technology
FeS has another name called pyrrhotite, has and molybdenumdisulphide and the similar flaky texture of Graphene.It is diamagnetism semiconductor material, has been widely used for as solid lubricant, electrode material of lithium battery etc.
Utilizing solution method to prepare ultra-thin semiconductor nano sheet is one of most important study frontier in Materials science, both at home and abroad to this has been large quantifier elimination.But the method adopted at present is mostly oil phase method, so often need to use much poisonous organic solvent.
And hydrothermal method, as a kind of take water as the method for reaction medium, be applied to the multiple inorganic semiconductor nanometer material of synthesis, there is security advantages of higher, but up to the present, still there is no document about the report utilizing the ultra-thin FeS nanometer sheet of water heat transfer.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, provides technique simple, easy to prepare, safety, the preparation method of a kind of FeS nanometer sheet easy to utilize.
The present invention solves the problems of the technologies described above adopted technical scheme:
A preparation method for FeS nanometer sheet, comprises the following steps:
Step one, by iron content presoma, sulfur-bearing presoma and tensio-active agent obtained solution soluble in water, tensio-active agent is cetyl trimethylammonium bromide;
Step 2, solution obtained in step one transferred in reactor and heat, after reacting completely, centrifugal, with water and ethanol wash sample, obtained FeS nanometer sheet.
The technical measures optimized also comprise:
In above-mentioned step one, iron content presoma is iron protochloride, ferrous acetate or ferrous sulfate.
In above-mentioned step one, sulfur-bearing presoma is thiocarbamide, thioacetamide, sodium sulphite, halfcystine or reduced glutathione.
In above-mentioned step one, the mol ratio of iron content presoma and sulfur-bearing presoma is 1:1 to 1:12.
In above-mentioned step one, the mol ratio of iron content presoma and tensio-active agent is 1:0.1 to 1:2.
In above-mentioned step 2, temperature of reaction is 120 DEG C to 240 DEG C.
In above-mentioned step 2, the reaction times is 1h to 18h.
The preparation method of a kind of FeS nanometer sheet of the present invention, technique is simple, and production cost is low, and obtained FeS nanometer sheet pattern is homogeneous, and thickness is about 3nm, is suitable for directly preparing electrode material of lithium battery; In preparation process, using water as solvent, preparation safety, with low cost, be conducive to applying.
Accompanying drawing explanation
Fig. 1 is the electron-microscope scanning of FeS nanometer sheet of the present invention;
Fig. 2 is the energy spectrogram of FeS nanometer sheet of the present invention;
Fig. 3 is the X-ray diffractogram of FeS nanometer sheet of the present invention;
Fig. 4 is the atomic force microscope figure of FeS nanometer sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
A preparation method for FeS nanometer sheet, comprises the following steps:
Step one, by iron content presoma, sulfur-bearing presoma and tensio-active agent obtained solution soluble in water, tensio-active agent is cetyl trimethylammonium bromide;
Step 2, solution obtained in step one transferred in reactor and heat, after reacting completely, centrifugal, with water and ethanol wash sample, obtained FeS nanometer sheet.
Wherein, in step one, iron content presoma is iron protochloride, ferrous acetate or ferrous sulfate; Sulfur-bearing presoma is thiocarbamide, thioacetamide, sodium sulphite, halfcystine or reduced glutathione.The mol ratio of iron content presoma and sulfur-bearing presoma is 1:1 to 1:12; The mol ratio of iron content presoma and tensio-active agent is 1:0.1 to 1:2.
In step 2, temperature of reaction is 120 DEG C to 240 DEG C; Reaction times is 1h to 18h.
Utilize the FeS nanometer sheet that present method is obtained, there is the thickness of ultra-thin (below 10nm).
Obtained material obtains energy spectrogram as shown in Figure 2 by analysis, from confirming that the material obtained is FeS spectrogram; By scanning electron microscope scanning acquisition appearance structure figure as shown in Figure 1, clearly can see that from this figure obtained FeS presents sheet structure, sample is by X-ray diffraction analysis, and the sample obtained is FeS, as shown in Figure 3; Obtain figure as shown in Figure 4 by atomic force microscope, can see that from this figure obtained FeS thickness is about 3nm.
Embodiment one
Step one, by 1mmol ferrous acetate, 1mmol thioacetamide, 0.1mmol cetyl trimethylammonium bromide (CTAB) is dissolved in obtained solution in 80ml water;
Step 2, the solution of preparation in step one is transferred to reactor heating, controlling temperature of reaction is 120 DEG C, after reaction 1h, centrifugal, wash sample, obtained FeS nanometer sheet with water and alcohol.
Embodiment two
Step one, by 1mmol iron protochloride, 10mmol halfcystine, 0.5mmol cetyl trimethylammonium bromide (CTAB) is dissolved in obtained solution in 80ml water;
Step 2, the solution of preparation in step one is transferred to reactor heating, controlling temperature of reaction is 160 DEG C, after reaction 6h, centrifugal, wash sample, obtained FeS nanometer sheet with water and alcohol.
Embodiment three
Step 2, by 1mmol ferrous sulfate, 5mmol thiocarbamide, 1mmol cetyl trimethylammonium bromide (CTAB) is dissolved in obtained solution in 80ml water;
Step 3, the solution of preparation in step one is transferred to reactor heating, controlling temperature of reaction is 180 DEG C, after reaction 10h, centrifugal, wash sample, obtained FeS nanometer sheet with water and alcohol.
Embodiment four
Step one, by 1mmol iron protochloride, 5mmol reduced glutathione, 1.5mmol cetyl trimethylammonium bromide (CTAB) is dissolved in obtained solution in 80ml water;
Step 2, the solution of preparation in step one is transferred to reactor heating, controlling temperature of reaction is 200 DEG C, after reaction 15h, centrifugal, wash sample, obtained FeS nanometer sheet with water and alcohol.
Embodiment five
Step one, by 1mmol ferrous acetate, 12mmol halfcystine and 2mmol cetyl trimethylammonium bromide (CTAB) are dissolved in obtained solution in 80ml water;
Step 2, the solution of preparation in step one is transferred to reactor heating, controlling temperature of reaction is 240 DEG C, after reaction 18h, centrifugal, wash sample, obtained FeS nanometer sheet with water and alcohol.
Most preferred embodiment of the present invention is illustrated, and the various change made by those of ordinary skill in the art or remodeling all can not depart from the scope of the present invention.
Claims (7)
1. a preparation method for FeS nanometer sheet, is characterized in that: comprise the following steps:
Step one, by iron content presoma, sulfur-bearing presoma and tensio-active agent obtained solution soluble in water, described tensio-active agent is cetyl trimethylammonium bromide;
Step 2, solution obtained in step one transferred in reactor and heat, after reacting completely, centrifugal, with water and ethanol wash sample, obtained FeS nanometer sheet.
2. the preparation method of a kind of FeS nanometer sheet according to claim 1, is characterized in that: in described step one, and iron content presoma is iron protochloride, ferrous acetate or ferrous sulfate.
3. the preparation method of a kind of FeS nanometer sheet according to claim 2, is characterized in that: in described step one, and sulfur-bearing presoma is thiocarbamide, thioacetamide, sodium sulphite, halfcystine or reduced glutathione.
4. the preparation method of a kind of FeS nanometer sheet according to claim 3, is characterized in that: in described step one, and the mol ratio of iron content presoma and sulfur-bearing presoma is 1:1 to 1:12.
5. the preparation method of a kind of FeS nanometer sheet according to claim 4, is characterized in that: in described step one, and the mol ratio of iron content presoma and tensio-active agent is 1:0.1 to 1:2.
6. the preparation method of a kind of FeS nanometer sheet according to claim 5, is characterized in that: in described step 2, and temperature of reaction is 120 DEG C to 240 DEG C.
7. the preparation method of a kind of FeS nanometer sheet according to claim 6, is characterized in that: in described step 2, and the reaction times is 1h to 18h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106205857A (en) * | 2016-06-24 | 2016-12-07 | 中国科学院地球化学研究所 | A kind of preparation method of magnetic iron ore electrode |
| CN106986392A (en) * | 2017-04-13 | 2017-07-28 | 环境保护部南京环境科学研究所 | The synthetic method and synthesizer of a kind of troilite |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN108083237A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院金属研究所 | A kind of method for preparing iron selenium superconductor |
| CN110124695A (en) * | 2019-06-12 | 2019-08-16 | 南昌航空大学 | The catalyst of organic pollutant, preparation method and application in a kind of degradation dyeing waste water |
| CN110526300A (en) * | 2019-06-28 | 2019-12-03 | 中冶华天工程技术有限公司 | The one heavy metal species processing preparation method of magnetic Nano Fe-S material |
| CN115254196A (en) * | 2022-07-25 | 2022-11-01 | 武汉理工大学 | Preparation method of glutathione-modified ferrous sulfide nano particles and application of glutathione-modified ferrous sulfide nano particles in glucose detection |
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| CN103950989A (en) * | 2014-05-07 | 2014-07-30 | 安徽师范大学 | FeS nano-material and preparation method thereof |
| CN104466089A (en) * | 2014-12-12 | 2015-03-25 | 浙江大学 | FeS flaky array film and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106205857A (en) * | 2016-06-24 | 2016-12-07 | 中国科学院地球化学研究所 | A kind of preparation method of magnetic iron ore electrode |
| CN106205857B (en) * | 2016-06-24 | 2018-02-13 | 中国科学院地球化学研究所 | A kind of preparation method of magnetic iron ore electrode |
| CN108083237A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院金属研究所 | A kind of method for preparing iron selenium superconductor |
| CN108083237B (en) * | 2016-11-22 | 2020-12-18 | 中国科学院金属研究所 | Method for preparing iron selenium superconductor |
| CN106986392A (en) * | 2017-04-13 | 2017-07-28 | 环境保护部南京环境科学研究所 | The synthetic method and synthesizer of a kind of troilite |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN110124695A (en) * | 2019-06-12 | 2019-08-16 | 南昌航空大学 | The catalyst of organic pollutant, preparation method and application in a kind of degradation dyeing waste water |
| CN110124695B (en) * | 2019-06-12 | 2021-07-30 | 南昌航空大学 | Catalyst for degrading organic pollutants in printing and dyeing wastewater, preparation method and application |
| CN110526300A (en) * | 2019-06-28 | 2019-12-03 | 中冶华天工程技术有限公司 | The one heavy metal species processing preparation method of magnetic Nano Fe-S material |
| CN110526300B (en) * | 2019-06-28 | 2022-01-04 | 中冶华天工程技术有限公司 | Preparation method of magnetic nano Fe-S material for heavy metal treatment |
| CN115254196A (en) * | 2022-07-25 | 2022-11-01 | 武汉理工大学 | Preparation method of glutathione-modified ferrous sulfide nano particles and application of glutathione-modified ferrous sulfide nano particles in glucose detection |
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