CN104445440B - A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material - Google Patents
A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material Download PDFInfo
- Publication number
- CN104445440B CN104445440B CN201410627218.XA CN201410627218A CN104445440B CN 104445440 B CN104445440 B CN 104445440B CN 201410627218 A CN201410627218 A CN 201410627218A CN 104445440 B CN104445440 B CN 104445440B
- Authority
- CN
- China
- Prior art keywords
- inert gas
- nano material
- preparation
- argon gas
- ethyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to the Fe of a kind of size, morphology controllable1‑XThe preparation method of S nano material, the method comprises the following steps: after (1) oleic acid and oleyl amine being mixed, obtain mixed solution；This mixed solution is stirred at room temperature and is passed through inert gas argon gas 10 ~ 15min, heats subsequently, is incubated under the protection of inert gas argon gas；After insulation terminates, described mixed solution continued under the protection of inert gas argon gas heating and is rapidly injected iron pentacarbonyl, being then incubated, continue to heat up; it is rapidly injected n-dodecyl mereaptan again; finally it is incubated 45 ~ 90min at 240 ~ 320 DEG C, through naturally cooling to room temperature, obtains cooling down solution；The most described cooling solution adds absolute ethyl alcohol, after ultrasonic being centrifuged, obtains black precipitate and reaction mother liquor；The mixed liquor washing of described black precipitate absolute ethyl alcohol and n-hexane is centrifugal, vacuum dried to constant weight, i.e. obtains black powder Fe1‑XS.The inventive method is simple, easily operation, low cost, environmental pollution is little, product purity is high without other impurity.
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 controllable1-XS nanometer
The preparation method of material.
Background technology
Metal sulfide is typically considered a kind of pollutant or harmful substance, however as the development of science and technology,
Metal sulfide sets in energy storage, energy conversion and luminescence owing to the character such as its special optics, electricity are widely used
In Bei.
Recently, various metal sulfide composites due to its theoretical capacity height, good cycle, environmental friendliness, safety,
The feature such as cheap, and it is used as the rechargeable lithium ion batteries (electrode material of (LIBs).In numerous metal sulfides, iron sulphur
Compound is because its low cost, and nature storage capacity becomes greatly the lithium electric material that energy storage applications fermentation is popular.Such as,
FeS、FeS2 Nano material can improve reversible capacity and the rated capacity of battery as the anode material of lithium ion battery.Cause
This, find a kind of cost relatively low, and method is simple, the synthesis Fe that environmental pollution is less1-XThe method of S nano material has reality
Meaning.
Summary of the invention
The technical problem to be solved is to provide that a kind of method is simple, low cost, environmental pollution are little, size,
The Fe of morphology controllable1-XThe preparation method of S nano material.
For solving the problems referred to above, a kind of size of the present invention, the Fe of morphology controllable1-XThe preparation side of S nano material
Method, comprises the following steps:
(1), after 0.3 ~ 3mL oleic acid and 3 ~ 15mL oleyl amine being mixed, obtain mixed solution；This mixed solution is stirred at room temperature
And it is passed through inert gas argon gas 10 ~ 15min, it is heated to the speed of 5 ~ 20 DEG C/min under the protection of inert gas argon gas subsequently
120 ~ 140 DEG C, and it is incubated 15 ~ 60min at such a temperature；After insulation terminates, by described mixed solution at inert gas argon gas
It is rapidly injected 0.3 ~ 3mmol iron pentacarbonyl when continuing to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min under protection, then exists
It is incubated at a temperature of Gai and 20 ~ 60min follow-up continuing is warmed up to 240 ~ 320 DEG C, then be rapidly injected 1 ~ 6mmol n-dodecyl mereaptan, finally exist
240 ~ 320 DEG C of insulation 45 ~ 90min, through naturally cooling to room temperature, obtain cooling down solution；
The most described cooling solution adds 10 ~ 20mL absolute ethyl alcohol, after ultrasonic being centrifuged, obtains black precipitate and reaction
Mother liquor；Described the black precipitate absolute ethyl alcohol of 4 ~ 10mL and the mixed liquor washing of n-hexane are centrifuged 3 ~ 6 times, vacuum dried
To constant weight, i.e. obtain black powder Fe1-XS。
Described step is replaced (1) to prepare cooling solution by following preparation method: by 0.5 ~ 3mL oleic acid and 3 ~ 15mL octadecylene
After mixing, obtain mixed liquor；This mixed solution is stirred at room temperature and is passed through inert gas argon gas 10 ~ 15min, subsequently in inertia
It is heated to 120 ~ 140 DEG C with the speed of 5 ~ 20 DEG C/min under the protection of gases argon, and is incubated 15 ~ 60min at such a temperature；Protect
After temperature terminates, continue to be heated to 160 ~ 240 with the speed of 5 ~ 20 DEG C/min under the protection of inert gas argon gas by mixed solution
DEG C time be rapidly injected 0.3 ~ 3mmol iron pentacarbonyl, be incubated that 20 ~ 60min is follow-up continuous is warmed up to 250 ~ 310 the most at such a temperature
DEG C, then it is rapidly injected 0.5 ~ 6mmol n-dodecyl mereaptan, finally it is incubated 45 ~ 90min at 250 ~ 310 DEG C, through naturally cooling to room
Temperature, obtains cooling down solution.
The flow velocity of described step (1) middle inert gas argon gas is 20 ~ 80mL/min.
In the mixed liquor of described step (2) absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 2 ~ 8 with the volume ratio of n-hexane.
Described step (2) in ultrasonic centrifugal condition refer to that supersonic frequency is 40kHz ~ 60kHz, ultrasonic time is 20 ~ 120
Second.
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 temperature be 30 ~ 60 DEG C, vacuum be-0.07 ~-0.09MPa.
The present invention compared with prior art has the advantage that
1, the present invention uses the two hot injections of step, iron pentacarbonyl and n-dodecyl mereaptan is joined containing octadecylene (or oil
Amine) and the solution of oleic acid in, react at a certain temperature, by controlling the mol ratio of reaction dissolvent kind and sulphur and iron,
Synthesize the Fe of size, morphology controllable1-XS nano material, not only simplifies preparation technology, and reduces operation easier and become
This.It can be seen from figure 1a that product becomes rice krispies flower-shaped when sulphur is less with the molar ratio of iron, when sulphur and iron molar ratio relatively
Product slabbing crystal, i.e. being gradually increased along with sulphur iron molar ratio time big, product pattern gradually from rice krispies flower-shaped by
Fade to flat crystal (seeing Fig. 1 b).From Fig. 2 a it will be seen that the particle of product is relatively when the molar ratio of sulphur Yu iron is less
Greatly, become rice krispies flower-shaped；2b it will be seen that when sulphur is bigger with the molar ratio of iron the particle of product less, globulate particle.
2, the iron sulfide of gained of the present invention is carried out x-ray diffraction experiment, it appeared that 2 θ=(29.848,33.789,
43.733,53.071,71.140 and 88.664。) place occurs in that obvious diffraction maximum, these diffraction maximums correspond respectively to Fe1-XS
(200), (205), (2,0,10), (220), (1,1,20) and (2,2,2) crystal face knowable to half-peak breadth analysis, Fig. 4 product
Size is relatively big compared with Fig. 3, and degree of crystallinity is higher, and this is consistent with the SEM figure of Fig. 1.(seeing Fig. 3, Fig. 4).
3, use high-temperature solvent method due to the present invention, can react under strong agitation and under higher temperature again, react nucleation
Hurry up, system is heated evenly, and therefore, presoma not only can be made fully to react but also can reduce the time of reaction, so that produce
The purity of thing is high and generates without other impurity, also greatly reduces the pollution to environment simultaneously.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in further detail.
Fig. 1 is transmission electron microscope photo (SEM) figure of the iron sulfide nano material of different-shape of the present invention, and wherein a figure is quick-fried
Popped rice shape, b figure is that (raw material is iron pentacarbonyl, n-dodecyl mereaptan and octadecylene to nano-sheet；Dispersion solvent is n-hexane).
Fig. 2 is transmission electron microscope photo (SEM) figure of the iron sulfide nano material of different size of the present invention, pattern, wherein a figure
Product size about at about 150nm, product is the flower-shaped particle of rice krispies, and the Product size of b figure is about at about 50nm, product
Particle spherical in shape (raw material is iron pentacarbonyl, n-dodecyl mereaptan and oleyl amine；Dispersion solvent is n-hexane).
Fig. 3 is Fe of the present invention1-X(raw material is iron pentacarbonyl, n-dodecyl mereaptan and ten to the X ray diffracting spectrum of S nano material
Eight alkene).
Fig. 4 is Fe of the present invention1-X(raw material is iron pentacarbonyl, n-dodecyl mereaptan and ten to the X ray diffracting spectrum of S nano material
Eight alkene).
Detailed description of the invention
1 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 0.3mL oleic acid and 3mL oleyl amine being mixed, obtain mixed solution.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 10min with the flow velocity of 20mL/min, exists subsequently
It is heated to 120 DEG C with the speed of 5 DEG C/min under the protection of inert gas argon gas, and is incubated 60min at such a temperature.
After insulation terminates, continue to be heated to the speed of 5 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 0.3mmol iron pentacarbonyl when 160 DEG C, insulation 20min follow-up continuing is warmed up to 240 DEG C the most at such a temperature, sooner
Speed injects 1mmol n-dodecyl mereaptan, is finally incubated 45min at 240 DEG C, through naturally cooling to room temperature, obtains cooling down solution.
(2) cooling solution adds 10mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 120 seconds that supersonic frequency is 40kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 4mL and the mixed liquor of n-hexane are with the centrifugal speed of 4500rpm
Centrifugal 3 times of rate washing, each 200 seconds, temperature be 30 DEG C, vacuum for-0.07MPa under conditions of be dried under vacuum to constant weight,
I.e. obtain black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 2 with the volume ratio (mL/mL) of n-hexane.
2 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 3mL oleic acid and 15mL oleyl amine being mixed, obtain mixed solution.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 15min with the flow velocity of 80mL/min, exists subsequently
It is heated to 140 DEG C with the speed of 20 DEG C/min under the protection of inert gas argon gas, and is incubated 15min at such a temperature.
After insulation terminates, continue to be heated to the speed of 20 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 3mmol iron pentacarbonyl when 240 DEG C, insulation 60min follow-up continuing is warmed up to 320 DEG C the most at such a temperature, more quickly
Inject 6mmol n-dodecyl mereaptan, be finally incubated 90min at 320 DEG C, through naturally cooling to room temperature, obtain cooling down solution.
(2) cooling solution adds 20mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 20 seconds that supersonic frequency is 60kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 10mL and the mixed liquor of n-hexane being centrifuged with 9000rpm
Centrifugal 6 times of speed washing, each 120 seconds, temperature be 60 DEG C, vacuum for-0.09MPa under conditions of be dried under vacuum to perseverance
Weight, i.e. obtains black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 8 with the volume ratio (mL/mL) of n-hexane.
3 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 1.5mL oleic acid and 9mL oleyl amine being mixed, obtain mixed solution.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 12min with the flow velocity of 50mL/min, exists subsequently
It is heated to 130 DEG C with the speed of 12 DEG C/min under the protection of inert gas argon gas, and is incubated 35min at such a temperature.
After insulation terminates, continue to be heated to the speed of 12 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 1.5mmol iron pentacarbonyl when 200 DEG C, insulation 40min follow-up continuing is warmed up to 280 DEG C the most at such a temperature, sooner
Speed injects 3mmol n-dodecyl mereaptan, is finally incubated 65min at 280 DEG C, through naturally cooling to room temperature, obtains cooling down solution.
(2) cooling solution adds 15mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 70 seconds that supersonic frequency is 50kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 7mL and the mixed liquor of n-hexane are with the centrifugal speed of 6500rpm
Centrifugal 4 times of rate washing, each 160 seconds, temperature be 45 DEG C, vacuum for-0.08MPa under conditions of be dried under vacuum to constant weight,
I.e. obtain black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 5 with the volume ratio (mL/mL) of n-hexane.
4 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 0.5mL oleic acid and 3mL octadecylene being mixed, obtain mixed liquor.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 10min with the flow velocity of 20mL/min, exists subsequently
It is heated to 120 DEG C with the speed of 5 DEG C/min under the protection of inert gas argon gas, and is incubated 15min at such a temperature.
After insulation terminates, continue to be heated to the speed of 5 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 0.3mmol iron pentacarbonyl when 160 DEG C, insulation 20min follow-up continuing is warmed up to 250 DEG C the most at such a temperature, sooner
Speed injects 0.5mmol n-dodecyl mereaptan, is finally incubated 45min at 250 DEG C, through naturally cooling to room temperature, obtains cooling down solution.
(2) cooling solution adds 10mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 120 seconds that supersonic frequency is 40kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 4mL and the mixed liquor of n-hexane are with the centrifugal speed of 4500rpm
Centrifugal 3 times of rate washing, each 200 seconds, temperature be 30 DEG C, vacuum for-0.07MPa under conditions of be dried under vacuum to constant weight,
I.e. obtain black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 2 with the volume ratio (mL/mL) of n-hexane.
5 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 3mL oleic acid and 15mL octadecylene being mixed, obtain mixed liquor.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 15min with the flow velocity of 80mL/min, exists subsequently
It is heated to 140 DEG C with the speed of 20 DEG C/min under the protection of inert gas argon gas, and is incubated 60min at such a temperature.
After insulation terminates, continue to be heated to the speed of 20 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 3mmol iron pentacarbonyl when 240 DEG C, insulation 60min follow-up continuing is warmed up to 310 DEG C the most at such a temperature, more quickly
Inject 6mmol n-dodecyl mereaptan, be finally incubated 90min at 310 DEG C, through naturally cooling to room temperature, obtain cooling down solution.
(2) cooling solution adds 20mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 20 seconds that supersonic frequency is 60kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 10mL and the mixed liquor of n-hexane being centrifuged with 9000rpm
Centrifugal 6 times of speed washing, each 120 seconds, temperature be 60 DEG C, vacuum for-0.09MPa under conditions of be dried under vacuum to perseverance
Weight, i.e. obtains black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 2 with the volume ratio (mL/mL) of n-hexane.
6 one kinds of sizes of embodiment, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 1.5mL oleic acid and 9mL octadecylene being mixed, obtain mixed liquor.
This mixed solution is stirred at room temperature and is passed through inert gas argon gas 12min with the flow velocity of 50mL/min, exists subsequently
It is heated to 130 DEG C with the speed of 12 DEG C/min under the protection of inert gas argon gas, and is incubated 35min at such a temperature.
After insulation terminates, continue to be heated to the speed of 12 DEG C/min under the protection of inert gas argon gas by mixed solution
Being rapidly injected 1.5mmol iron pentacarbonyl when 200 DEG C, insulation 40min follow-up continuing is warmed up to 280 DEG C the most at such a temperature, sooner
Speed injects 3mmol n-dodecyl mereaptan, is finally incubated 65min at 280 DEG C, through naturally cooling to room temperature, obtains cooling down solution.
(2) cooling solution adds 15mL absolute ethyl alcohol, obtain black behind ultrasonic centrifugal 75 seconds that supersonic frequency is 50kHz
Look sediment and reaction mother liquor；The absolute ethyl alcohol of black precipitate 7mL and the mixed liquor of n-hexane are with the centrifugal speed of 6500rpm
Centrifugal 5 times of rate washing, each 160 seconds, temperature be 45 DEG C, vacuum for-0.08MPa under conditions of be dried under vacuum to constant weight,
I.e. obtain black powder Fe1-XS。
Wherein: in the mixed liquor of absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 5 with the volume ratio (mL/mL) of n-hexane.
Claims (7)
1. a size, the Fe of morphology controllable1-XThe preparation method of S nano material, comprises the following steps:
(1), after 0.3 ~ 3mL oleic acid and 3 ~ 15mL oleyl amine being mixed, obtain mixed solution；This mixed solution is stirred at room temperature and leads to
Enter inert gas argon gas 10 ~ 15min, subsequently under the protection of inert gas argon gas with the speed of 5 ~ 20 DEG C/min be heated to 120 ~
140 DEG C, and it is incubated 15 ~ 60min at such a temperature；After insulation terminates, by described mixed solution in the protection of inert gas argon gas
Under be rapidly injected 0.3 ~ 3mmol iron pentacarbonyl, then in this temperature when continuing to be heated to 160 ~ 240 DEG C with the speed of 5 ~ 20 DEG C/min
The lower insulation 20 ~ 60min of degree is follow-up continuous is warmed up to 240 ~ 320 DEG C, then is rapidly injected 1 ~ 6mmol n-dodecyl mereaptan, finally 240 ~
320 DEG C of insulation 45 ~ 90min, through naturally cooling to room temperature, obtain cooling down solution；
The most described cooling solution adds 10 ~ 20mL absolute ethyl alcohol, after ultrasonic being centrifuged, obtains black precipitate and reaction mother liquor；
Described the black precipitate absolute ethyl alcohol of 4 ~ 10mL and the mixed liquor washing of n-hexane are centrifuged 3 ~ 6 times, vacuum dried to permanent
Weight, i.e. obtains black powder Fe1-XS；And product becomes rice krispies flower-shaped when sulphur is less with the molar ratio of iron, when sulphur and iron
Product globulate particle when molar ratio is bigger.
A kind of size the most as claimed in claim 1, the Fe of morphology controllable1-XThe preparation method of S nano material, it is characterised in that:
Step described in claim 1 is replaced (1) to prepare cooling solution by following preparation method: by 0.5 ~ 3mL oleic acid and 3 ~ 15mL 18
After alkene mixing, obtain mixed liquor；This mixed solution is stirred at room temperature and is passed through inert gas argon gas 10 ~ 15min, subsequently lazy
It is heated to 120 ~ 140 DEG C with the speed of 5 ~ 20 DEG C/min under the protection of property gases argon, and is incubated 15 ~ 60min at such a temperature；
After insulation terminates, by mixed solution under the protection of inert gas argon gas with the speed of 5 ~ 20 DEG C/min continue to be heated to 160 ~
Be rapidly injected 0.3 ~ 3mmol iron pentacarbonyl when 240 DEG C, be incubated the most at such a temperature 20 ~ 60min follow-up continuous be warmed up to 250 ~
310 DEG C, then it is rapidly injected 0.5 ~ 6mmol n-dodecyl mereaptan, finally it is incubated 45 ~ 90min at 250 ~ 310 DEG C, through naturally cooling to
Room temperature, obtains cooling down solution；And the product that the method obtains when sulphur is less with the molar ratio of iron becomes rice krispies flower-shaped, when sulphur with
The product slabbing crystal that when molar ratio of iron is bigger, the method obtains.
A kind of size the most as claimed in claim 1 or 2, the Fe of morphology controllable1-XThe preparation method of S nano material, its feature exists
In: the flow velocity of described step (1) middle inert gas argon gas is 20 ~ 80mL/min.
A kind of size the most as claimed in claim 1, the Fe of morphology controllable1-XThe preparation method of S nano material, it is characterised in that:
In the mixed liquor of described step (2) absolute ethyl alcohol and n-hexane, absolute ethyl alcohol is 2 ~ 8 with the volume ratio of n-hexane.
A kind of size the most as claimed in claim 1, the Fe of morphology controllable1-XThe preparation method of S nano material, it is characterised in that:
Described step (2) in ultrasonic centrifugal condition refer to that supersonic frequency is 40kHz ~ 60kHz, ultrasonic time is 20 ~ 120 seconds.
A kind of size the most as claimed in claim 1, the Fe of morphology controllable1-XThe preparation method of S nano material, it is characterised in that:
Described step (2) in centrifugal condition refer to that centrifugation rate is 4500 ~ 9000rpm, the time is 120 ~ 200 seconds.
A kind of size the most as claimed in claim 1, the Fe of morphology controllable1-XThe preparation method of S nano material, it is characterised in that:
Described step (2) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C, vacuum be-0.07 ~-0.09MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410627218.XA CN104445440B (en) | 2014-11-10 | 2014-11-10 | A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410627218.XA CN104445440B (en) | 2014-11-10 | 2014-11-10 | A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104445440A CN104445440A (en) | 2015-03-25 |
| CN104445440B true CN104445440B (en) | 2016-08-24 |
Family
ID=52892301
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410627218.XA Expired - Fee Related CN104445440B (en) | 2014-11-10 | 2014-11-10 | A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104445440B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105709781B (en) * | 2016-01-24 | 2018-06-22 | 太原理工大学 | A kind of DCL/Direct coal liquefaction catalyst, preparation method and application |
| CN105945303B (en) * | 2016-05-17 | 2018-11-16 | 西北师范大学 | A kind of preparation method of nanometer of α-Fe metal powder |
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923790A (en) * | 2011-09-15 | 2013-02-13 | 华东理工大学 | Synthetic method of FeS2 pyrite photoelectric material |
| CN103936057A (en) * | 2014-04-02 | 2014-07-23 | 西北师范大学 | Preparation method of cadmium sulfide quantum dots with controllable sizes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6962685B2 (en) * | 2002-04-17 | 2005-11-08 | International Business Machines Corporation | Synthesis of magnetite nanoparticles and the process of forming Fe-based nanomaterials |
-
2014
- 2014-11-10 CN CN201410627218.XA patent/CN104445440B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923790A (en) * | 2011-09-15 | 2013-02-13 | 华东理工大学 | Synthetic method of FeS2 pyrite photoelectric material |
| CN103936057A (en) * | 2014-04-02 | 2014-07-23 | 西北师范大学 | Preparation method of cadmium sulfide quantum dots with controllable sizes |
Non-Patent Citations (1)
| Title |
|---|
| Diverse-shaped iron sulfide nanostructures synthesized from a single source precursor approach;Yejun Zhang等;《CrystEngComm》;20100707;第3658-3663页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104445440A (en) | 2015-03-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104445440B (en) | A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material | |
| Xu et al. | A comparative study of crystalline and amorphous Li0. 5La0. 5TiO3 as surface coating layers to enhance the electrochemical performance of LiNi0. 815Co0. 15Al0. 035O2 cathode | |
| CN104600258B (en) | Composite negative electrode material of lithium ion battery and preparation method thereof | |
| Lei et al. | Strengthening valuable metal recovery from spent lithium-ion batteries by environmentally friendly reductive thermal treatment and electrochemical leaching | |
| CN102185141A (en) | Modification method for improving high-temperature cycle performance and ionic conductance of lithium iron phosphate material | |
| CN103560232A (en) | Preparation method of S-C positive pole composite material of high cycle performance lithium sulfur battery | |
| CN109192936B (en) | Preparation method of lithium iron phosphate | |
| CN103904307A (en) | Silicon-carbon composite material, preparation method and application thereof | |
| CN107658447A (en) | A kind of N doping carbon-coating cladding flower ball-shaped V2O5Preparation method | |
| CN107732245B (en) | A kind of preparation method of hard carbon/graphene composite negative pole for lithium battery | |
| CN104058453A (en) | Size-controllable spherical anatase type TiO2 mesocrystal and preparation method thereof | |
| CN106602023A (en) | Method for in-situ synthesis of graphite phase carbon nitride-copper oxide composite material | |
| CN102412393B (en) | Method and application of synthesis of Mg2V2O7 nanoparticles employing high temperature solid phase method | |
| CN108467021A (en) | A kind of method that liquid nitrogen stripping black phosphorus prepares nanometer black phosphorus | |
| CN103326009A (en) | Process for preparing high capacity lithium titanate anode material | |
| Lipson et al. | Stabilizing NMC 811 Li-Ion battery cathode through a rapid coprecipitation process | |
| CN103779549B (en) | The preparation method of even particulate dispersion lithium ion battery electrode material nano lithium titanate | |
| CN103094549A (en) | Supercritical hydro-thermal synthesizing method of lithium ion battery negative material lithium titanate | |
| CN105776353B (en) | Sulphur iron compound and preparation method thereof | |
| CN107342407A (en) | A kind of loaded mesoporous SiO of porous carbonx/ C composite negative pole materials and preparation method thereof | |
| Guan et al. | Improved electrochemical performance of a Li1. 2Ni0. 2Mn0. 6O2 cathode by a hydrothermal method with a metal–organic framework as a precursor | |
| CN107910541A (en) | A kind of preparation method of the spherical composite material of negative electrode of lithium ion battery | |
| Zubair et al. | High-temperature electrochemical performance enhancement of lithium-rich layered oxides by surface modification | |
| CN104124430B (en) | Vanadium pentoxide nanometer material that a kind of ruthenic oxide quantum dot is modified and its preparation method and application | |
| CN102180513B (en) | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160824 Termination date: 20161110 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |