CN104445440A - Preparation method of Fe1-XS nanomaterial with controllable size and shape - Google Patents
Preparation method of Fe1-XS nanomaterial with controllable size and shape Download PDFInfo
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- CN104445440A CN104445440A CN201410627218.XA CN201410627218A CN104445440A CN 104445440 A CN104445440 A CN 104445440A CN 201410627218 A CN201410627218 A CN 201410627218A CN 104445440 A CN104445440 A CN 104445440A
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Abstract
The invention relates to a preparation method of a Fe1-XS nanomaterial with controllable size and shape. The preparation method comprises the following steps: (1) mixing oleic acid and oleylamine, so as to obtain a mixed solution; stirring the mixed solution at the room temperature, feeding argon which is an inert gas for 10-15 minutes, and carrying out heating and heat insulation in the presence of argon; after the heat insulation is ended, under the protection of the inert gas argon, further heating the mixed solution and rapidly injecting pentacarbonyl iron; then insulating the heat, further heating, rapidly injecting N-dodecyl mercaptan, maintaining the temperature at 240-320 DEG C for 45-90 minutes, and naturally cooling to the room temperature, so as to obtain a cooled solution; (2) adding absolute ethanol into the cooled solution, carrying out ultrasonic centrifuging to obtain black precipitate and a reaction mother solution, wherein the black precipitate is washed and centrifuged with mixed liquid of absolute ethanol and normal hexane; carrying out vacuum drying to constant weight, so as to obtain black powdery Fe1-XS. The preparation method is simple, easy to operate and low in cost and hardly causes environmental pollution, and the product is high in purity and has no other impurities.
Description
Technical field
The present invention relates to the preparing technical field of nano material, particularly relate to the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material.
Background technology
Metallic sulfide is considered to a kind of pollutent or objectionable impurities usually, but along with the development of science and technology, and metallic sulfide is widely used in energy storage, Conversion of energy and luminaire due to character such as its special optics, electricity.
Recently, various metallic sulfide matrix material due to features such as its theoretical capacity is high, good cycle, environmental friendliness, safety, cheapnesss, and is used as the rechargeable lithium ion batteries (electrode materials of (LIBs).In numerous metallic sulfide, iron sulfide is because its cost is low, and nature storage capacity becomes greatly energy storage applications and to leaven dough the lithium electric material be popular.Such as, FeS, FeS
2nano material can improve reversible capacity and the rated capacity of battery as the anode material of lithium ion battery.Therefore, find a kind of cost lower, method is simple, the synthesis Fe that environmental pollution is less
1-Xthe method of S nano material has realistic meaning.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of method is simple, cost is low, environmental pollution is little, size, morphology controllable Fe
1-Xthe preparation method of S nano material.
For solving the problem, the Fe of a kind of size of the present invention, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 0.3 ~ 3mL oleic acid and the mixing of 3 ~ 15mL oleyl amine, obtain mixing solutions; This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10 ~ 15min, is heated to 120 ~ 140 DEG C subsequently, and is incubated 15 ~ 60min at such a temperature under the protection of rare gas element argon gas with the speed of 5 ~ 20 DEG C/min; After insulation terminates, 0.3 ~ 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min by described mixing solutions under the protection of rare gas element argon gas, then be incubated at such a temperature and 20 ~ 60min follow-up continuing be warmed up to 240 ~ 320 DEG C, inject 1 ~ 6mmol n-dodecyl mereaptan fast again, finally at 240 ~ 320 DEG C of insulation 45 ~ 90min, through naturally cooling to room temperature, obtain cooling solution;
(2) add 10 ~ 20mL dehydrated alcohol in described cooling solution, through ultrasonic centrifugal after obtain black precipitate and reaction mother liquor; Described the black precipitate dehydrated alcohol of 4 ~ 10mL and the mixed solution of normal hexane wash centrifugal 3 ~ 6 times, through vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Described step is replaced (1) to prepare cooling solution by following preparation method: after 0.5 ~ 3mL oleic acid and the mixing of 3 ~ 15mL octadecylene, to obtain mixed solution; This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10 ~ 15min, is heated to 120 ~ 140 DEG C subsequently, and is incubated 15 ~ 60min at such a temperature under the protection of rare gas element argon gas with the speed of 5 ~ 20 DEG C/min; After insulation terminates; 0.3 ~ 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 20 ~ 60min follow-up continuing be warmed up to 250 ~ 310 DEG C; inject 0.5 ~ 6mmol n-dodecyl mereaptan fast again; finally at 250 ~ 310 DEG C of insulation 45 ~ 90min; through naturally cooling to room temperature, obtain cooling solution.
Described step (1) in the flow velocity of rare gas element argon gas be 20 ~ 80mL/min.
In the mixed solution of described step (2) dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane is 2 ~ 8.
Described step (2) in ultrasonic centrifugal condition refer to that ultrasonic frequency is 40kHz ~ 60kHz, ultrasonic time is 20 ~ 120 seconds.
Described step (2) in centrifugal condition refer to that centrifugation rate is 4500 ~ 9000rpm, the time is 120 ~ 200 seconds.
Described step (2) in vacuum drying condition refer to that temperature is 30 ~ 60 DEG C, vacuum tightness is-0.07 ~-0.09MPa.
The present invention compared with prior art has the following advantages:
1, the present invention adopts the hot injection of two steps, pentacarbonyl iron and n-dodecyl mereaptan are joined in the solution containing octadecylene (or oleyl amine) and oleic acid, reacting at a certain temperature, by controlling the mol ratio of reaction solvent kind and sulphur and iron, having synthesized the Fe of size, morphology controllable
1-Xs nano material, not only simplifies preparation technology, and reduces operation easier and cost.Can see from Fig. 1 a, when sulphur and the molar ratio of iron are less, product becomes rice krispies flower-shaped, the product slabbing crystal when the molar ratio of sulphur and iron is larger, namely along with the increase gradually of sulphur iron molar ratio, product pattern gradually become tabular crystal (see Fig. 1 b) from rice krispies is flower-shaped gradually.Can see from Fig. 2 a, when the molar ratio of sulphur and iron is less, the particle of product is comparatively large, becomes rice krispies flower-shaped; 2b can see, when the molar ratio of sulphur and iron is larger, the particle of product is less, globulate particle.
2, x-ray diffraction experiment is carried out to the iron sulphide of gained of the present invention, 2 θ=(29.848,33.789,43.733,53.071,71.140 and 88.664 can be found
.) obvious diffraction peak appearred in place, these diffraction peaks correspond respectively to Fe
1-X(200), (205), (2,0,10), (220), (1,1 of S, 20) and (2,2,2) crystal face analyze from peak width at half height, the size of Fig. 4 product is large compared with Fig. 3, and degree of crystallinity is higher, and this conforms to the SEM figure of Fig. 1.(see Fig. 3, Fig. 4).
3, because the present invention adopts high-temperature solvent method, can react under violent stirring and under higher temperature again, reaction nucleation is fast, system is heated evenly, therefore, presoma not only can be made fully to react but also the time of reaction can be reduced, thus make the purity of product high and generate without other impurity, also greatly reduce the pollution to environment simultaneously.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is transmission electron microscope photo (SEM) figure of the iron sulphide nano material of different-shape of the present invention, and wherein a figure is that rice krispies is flower-shaped, and b figure is that (raw material is pentacarbonyl iron, n-dodecyl mereaptan and octadecylene to nano-sheet; Dispersion solvent is normal hexane).
Fig. 2 is transmission electron microscope photo (SEM) figure of iron sulphide nano material of different size of the present invention, pattern, wherein the Product size of a figure is greatly about about 150nm, product is the flower-shaped particle of rice krispies, the Product size of b figure is greatly about about 50nm, and the particle of product is spherical in shape, and (raw material is pentacarbonyl iron, n-dodecyl mereaptan and oleyl amine; Dispersion solvent is normal hexane).
Fig. 3 is Fe of the present invention
1-Xthe X ray diffracting spectrum (raw material is pentacarbonyl iron, n-dodecyl mereaptan and octadecylene) of S nano material.
Fig. 4 is Fe of the present invention
1-Xthe X ray diffracting spectrum (raw material is pentacarbonyl iron, n-dodecyl mereaptan and octadecylene) of S nano material.
Embodiment
embodiment 1the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 0.3mL oleic acid and the mixing of 3mL oleyl amine, obtain mixing solutions.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10min with the flow velocity of 20mL/min, is heated to 120 DEG C subsequently, and is incubated 60min at such a temperature under the protection of rare gas element argon gas with the speed of 5 DEG C/min.
After insulation terminates; 0.3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 DEG C with the speed of 5 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 20min follow-up continuing be warmed up to 240 DEG C; inject 1mmol n-dodecyl mereaptan fast again; finally at 240 DEG C of insulation 45min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 10mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 120 seconds of 40kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 4mL and the mixed solution of normal hexane with centrifugal 3 times of the centrifugation rate of 4500rpm washing, each 200 seconds, temperature be 30 DEG C, vacuum tightness be the condition of-0.07MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 2.
embodiment 2the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 3mL oleic acid and the mixing of 15mL oleyl amine, obtain mixing solutions.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 15min with the flow velocity of 80mL/min, is heated to 140 DEG C subsequently, and is incubated 15min at such a temperature under the protection of rare gas element argon gas with the speed of 20 DEG C/min.
After insulation terminates; 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 240 DEG C with the speed of 20 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 60min follow-up continuing be warmed up to 320 DEG C; inject 6mmol n-dodecyl mereaptan fast again; finally at 320 DEG C of insulation 90min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 20mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 20 seconds of 60kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 10mL and the mixed solution of normal hexane with centrifugal 6 times of the centrifugation rate of 9000rpm washing, each 120 seconds, temperature be 60 DEG C, vacuum tightness be the condition of-0.09MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 8.
embodiment 3the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 1.5mL oleic acid and the mixing of 9mL oleyl amine, obtain mixing solutions.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 12min with the flow velocity of 50mL/min, is heated to 130 DEG C subsequently, and is incubated 35min at such a temperature under the protection of rare gas element argon gas with the speed of 12 DEG C/min.
After insulation terminates; 1.5mmol pentacarbonyl iron is injected fast when being continued to be heated to 200 DEG C with the speed of 12 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 40min follow-up continuing be warmed up to 280 DEG C; inject 3mmol n-dodecyl mereaptan fast again; finally at 280 DEG C of insulation 65min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 15mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 70 seconds of 50kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 7mL and the mixed solution of normal hexane with centrifugal 4 times of the centrifugation rate of 6500rpm washing, each 160 seconds, temperature be 45 DEG C, vacuum tightness be the condition of-0.08MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 5.
embodiment 4the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 0.5mL oleic acid and the mixing of 3mL octadecylene, obtain mixed solution.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10min with the flow velocity of 20mL/min, is heated to 120 DEG C subsequently, and is incubated 15min at such a temperature under the protection of rare gas element argon gas with the speed of 5 DEG C/min.
After insulation terminates; 0.3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 DEG C with the speed of 5 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 20min follow-up continuing be warmed up to 250 DEG C; inject 0.5mmol n-dodecyl mereaptan fast again; finally at 250 DEG C of insulation 45min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 10mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 120 seconds of 40kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 4mL and the mixed solution of normal hexane with centrifugal 3 times of the centrifugation rate of 4500rpm washing, each 200 seconds, temperature be 30 DEG C, vacuum tightness be the condition of-0.07MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 2.
embodiment 5the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 3mL oleic acid and the mixing of 15mL octadecylene, obtain mixed solution.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 15min with the flow velocity of 80mL/min, is heated to 140 DEG C subsequently, and is incubated 60min at such a temperature under the protection of rare gas element argon gas with the speed of 20 DEG C/min.
After insulation terminates; 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 240 DEG C with the speed of 20 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 60min follow-up continuing be warmed up to 310 DEG C; inject 6mmol n-dodecyl mereaptan fast again; finally at 310 DEG C of insulation 90min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 20mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 20 seconds of 60kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 10mL and the mixed solution of normal hexane with centrifugal 6 times of the centrifugation rate of 9000rpm washing, each 120 seconds, temperature be 60 DEG C, vacuum tightness be the condition of-0.09MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 2.
embodiment 6the Fe of a kind of size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 1.5mL oleic acid and the mixing of 9mL octadecylene, obtain mixed solution.
This mixing solutions at room temperature stirs and passes into rare gas element argon gas 12min with the flow velocity of 50mL/min, is heated to 130 DEG C subsequently, and is incubated 35min at such a temperature under the protection of rare gas element argon gas with the speed of 12 DEG C/min.
After insulation terminates; 1.5mmol pentacarbonyl iron is injected fast when being continued to be heated to 200 DEG C with the speed of 12 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 40min follow-up continuing be warmed up to 280 DEG C; inject 3mmol n-dodecyl mereaptan fast again; finally at 280 DEG C of insulation 65min; through naturally cooling to room temperature, obtain cooling solution.
(2) adding 15mL dehydrated alcohol in cooling solution, is obtain black precipitate and reaction mother liquor after ultrasonic centrifugal 75 seconds of 50kHz through ultrasonic frequency; The dehydrated alcohol of black precipitate 7mL and the mixed solution of normal hexane with centrifugal 5 times of the centrifugation rate of 6500rpm washing, each 160 seconds, temperature be 45 DEG C, vacuum tightness be the condition of-0.08MPa under vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio (mL/mL) of dehydrated alcohol and normal hexane is 5.
Claims (7)
1. the Fe of a size, morphology controllable
1-Xthe preparation method of S nano material, comprises the following steps:
(1), by after 0.3 ~ 3mL oleic acid and the mixing of 3 ~ 15mL oleyl amine, obtain mixing solutions; This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10 ~ 15min, is heated to 120 ~ 140 DEG C subsequently, and is incubated 15 ~ 60min at such a temperature under the protection of rare gas element argon gas with the speed of 5 ~ 20 DEG C/min; After insulation terminates, 0.3 ~ 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min by described mixing solutions under the protection of rare gas element argon gas, then be incubated at such a temperature and 20 ~ 60min follow-up continuing be warmed up to 240 ~ 320 DEG C, inject 1 ~ 6mmol n-dodecyl mereaptan fast again, finally at 240 ~ 320 DEG C of insulation 45 ~ 90min, through naturally cooling to room temperature, obtain cooling solution;
(2) add 10 ~ 20mL dehydrated alcohol in described cooling solution, through ultrasonic centrifugal after obtain black precipitate and reaction mother liquor; Described the black precipitate dehydrated alcohol of 4 ~ 10mL and the mixed solution of normal hexane wash centrifugal 3 ~ 6 times, through vacuum-drying to constant weight, namely obtain black powder Fe
1-Xs.
2. the Fe of a kind of size as claimed in claim 1, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: replace step described in claim 1 (1) to prepare cooling solution by following preparation method: after 0.5 ~ 3mL oleic acid and the mixing of 3 ~ 15mL octadecylene, obtain mixed solution; This mixing solutions at room temperature stirs and passes into rare gas element argon gas 10 ~ 15min, is heated to 120 ~ 140 DEG C subsequently, and is incubated 15 ~ 60min at such a temperature under the protection of rare gas element argon gas with the speed of 5 ~ 20 DEG C/min; After insulation terminates; 0.3 ~ 3mmol pentacarbonyl iron is injected fast when being continued to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min by mixing solutions under the protection of rare gas element argon gas; then be incubated at such a temperature and 20 ~ 60min follow-up continuing be warmed up to 250 ~ 310 DEG C; inject 0.5 ~ 6mmol n-dodecyl mereaptan fast again; finally at 250 ~ 310 DEG C of insulation 45 ~ 90min; through naturally cooling to room temperature, obtain cooling solution.
3. the Fe of a kind of size as claimed in claim 1 or 2, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: described step (1) in the flow velocity of rare gas element argon gas be 20 ~ 80mL/min.
4. the Fe of a kind of size as claimed in claim 1, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: in the mixed solution of described step (2) dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane is 2 ~ 8.
5. the Fe of a kind of size as claimed in claim 1, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: described step (2) in ultrasonic centrifugal condition refer to that ultrasonic frequency is 40kHz ~ 60kHz, ultrasonic time is 20 ~ 120 seconds.
6. the Fe of a kind of size as claimed in claim 1, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: described step (2) in centrifugal condition refer to that centrifugation rate is 4500 ~ 9000rpm, the time is 120 ~ 200 seconds.
7. the Fe of a kind of size as claimed in claim 1, morphology controllable
1-Xthe preparation method of S nano material, is characterized in that: described step (2) in vacuum drying condition refer to that temperature is 30 ~ 60 DEG C, vacuum tightness is-0.07 ~-0.09MPa.
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| CN105709781A (en) * | 2016-01-24 | 2016-06-29 | 太原理工大学 | Coal direct liquefaction catalyst and preparation method and application thereof |
| CN105945303A (en) * | 2016-05-17 | 2016-09-21 | 西北师范大学 | Preparing method of nano alpha-Fe metal powder |
| CN108940318A (en) * | 2018-06-29 | 2018-12-07 | 河北工业大学 | A kind of preparation method of nanometer nickel sulfide chip arrays |
| CN109226781A (en) * | 2018-10-30 | 2019-01-18 | 郑州大学 | A kind of method that organic phase prepares different shape Ru nano material |
| CN110627132A (en) * | 2019-09-26 | 2019-12-31 | 黑龙江工程学院 | Preparation method of small-size iron disulfide nano hollow sphere |
| CN110745869A (en) * | 2019-11-11 | 2020-02-04 | 青岛科技大学 | FeS nano-particles synthesized based on solvothermal method, preparation method and application |
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| CN105709781A (en) * | 2016-01-24 | 2016-06-29 | 太原理工大学 | Coal direct liquefaction catalyst and preparation method and application thereof |
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| CN108940318A (en) * | 2018-06-29 | 2018-12-07 | 河北工业大学 | A kind of preparation method of nanometer nickel sulfide chip arrays |
| CN108940318B (en) * | 2018-06-29 | 2021-04-30 | 河北工业大学 | Preparation method of nickel sulfide nanosheet array |
| CN109226781A (en) * | 2018-10-30 | 2019-01-18 | 郑州大学 | A kind of method that organic phase prepares different shape Ru nano material |
| CN110627132A (en) * | 2019-09-26 | 2019-12-31 | 黑龙江工程学院 | Preparation method of small-size iron disulfide nano hollow sphere |
| CN110627132B (en) * | 2019-09-26 | 2022-02-22 | 黑龙江工程学院 | Preparation method of small-size iron disulfide nano hollow sphere |
| CN110745869A (en) * | 2019-11-11 | 2020-02-04 | 青岛科技大学 | FeS nano-particles synthesized based on solvothermal method, preparation method and application |
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