CN109360965A - A kind of Mo doping SnO2The preparation method of composite S nS material - Google Patents

A kind of Mo doping SnO2The preparation method of composite S nS material Download PDF

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Publication number
CN109360965A
CN109360965A CN201811322280.2A CN201811322280A CN109360965A CN 109360965 A CN109360965 A CN 109360965A CN 201811322280 A CN201811322280 A CN 201811322280A CN 109360965 A CN109360965 A CN 109360965A
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China
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preparation
reaction kettle
composite
sno
hydrothermal reaction
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CN201811322280.2A
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王依山
张学谦
温广武
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Shandong University of Technology
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Shandong University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of Mo to adulterate SnO2The preparation method of composite S nS material, comprising the following steps: (1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly；(2) it takes above-mentioned solution to be put into hydrothermal reaction kettle, is put into drying box and heats after hydrothermal reaction kettle sealing；(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, be centrifuged using deionized water；(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.

Description

A kind of Mo doping SnO2The preparation method of composite S nS material
Technical field
The present invention relates to field of material technology more particularly to a kind of Mo to adulterate SnO2The preparation side of composite S nS material Method.
Background technique
SnO2As transition metal oxide, there is the up to theoretical lithium storage content of 782 mAh/g, at the same have it is nontoxic, The cheap and simple feature of synthesis technology, therefore by the concern of scientific circles and industrial circle.However, SnO2It is aoxidized with other metals Object is similar, and the conductivity of material is lower, while material can generate huge volume change in charge and discharge process, and material is caused to hold The problem of granule atomization easily occur and reuniting, the final high rate performance and cyclical stability for influencing material.To improve SnO2Circulation Stability can effectively solve SnO by way of element doping2Volume expansion and the lower problem of conductivity.In multiple element In, Mo can enter SnO with Effective Doping2In lattice, improve SnO2Performance.
SnS is as transient metal sulfide, with SnO2Similar theoretical lithium storage content with higher, but SnS equally has There is the problem that conductivity is lower, and then influences its cyclical stability.Compared with a variety of modes for improving material electric conductivity, Ke Yitong Cross SnS and SnO2Compound mode effectively improves the whole conductivity of material.Therefore using Mo to SnO2It is doped, and with SnS progress is compound, can prepare excellent Mo doping SnO2Composite S nS material obtains having excellent lithium ion storage performance Material, however currently with simple process preparation Mo adulterate SnO2The preparation method of composite S nS material is also less.
Therefore, it is easy to operate to study one kind, technique requires not harsh, it can be achieved that high quality, large scale preparation Mo doping SnO2Composite S nS material has wide business application and scientific research value.
Summary of the invention
Technical purpose of the invention is to adulterate SnO for above-mentioned Mo2The status of composite S nS material preparation technology, provides A kind of Mo doping SnO of simple process2The method of composite S nS new structural material.
Technical solution of the present invention is as follows:
A kind of Mo doping SnO2The preparation method of composite S nS material, comprising the following steps:
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly；
(2) it takes above-mentioned solution to be put into hydrothermal reaction kettle, is put into drying box and heats after hydrothermal reaction kettle sealing；
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, be centrifuged using deionized water；
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
The concentration of solution after tin tetrachloride, ammonium molybdate and thiocarbamide is added in the step (1) for the preparation method For 1 ~ 10 mg/mL.
The preparation method, tin tetrachloride in the step (1): ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
The preparation method, mixing time is 0.5 ~ 5 h in the step (1).
The preparation method, the volume of reaction kettle is 50 or 100 mL in the step (2).
The preparation method, in the step (2) in a kettle the capacity of solution be reactor volume 70% ~ 90%。
The preparation method, drying box heating temperature is 180 ~ 200 DEG C in the step (2).
The preparation method, drying box heating time is 18 ~ 36 h in the step (2).
The preparation method, the middle centrifugation number of the step (3) is 3 ~ 5 times.
Detailed description of the invention
Fig. 1 is that Mo adulterates SnO in the embodiment of the present invention 12Composite S nS material XRD diagram piece.
Specific implementation method
Below in conjunction with attached drawing, present invention is further described in detail with embodiment, it should be pointed out that embodiment described below It is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1:
A kind of Mo doping SnO is provided in the present embodiment2The preparation method of composite S nS material, specific preparation method are as follows.
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly, mixing time is 1 h, and solution is dense Degree is 6 mg/mL, and tin tetrachloride: ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
(2) it takes above-mentioned 80 mL solution to be put into the hydrothermal reaction kettle that volume is 100 mL, is put into after hydrothermal reaction kettle sealing 24 h are heated in drying box, temperature is 200 DEG C.
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, is centrifuged 3 times using deionized water.
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
Fig. 1 is above-mentioned Mo doping SnO2Composite S nS material XRD diagram piece.As can be seen from the figure: multiple SnO occur2And SnS Peak position illustrates that prepared sample contains SnO2And SnS, and do not occur the Mo element in raw material ammonium molybdate in XRD diagram, show Mo, which is successfully adulterated, enters SnO2In lattice, illustrate successfully to synthesize Mo doping SnO2Composite S nS material.
Embodiment 2:
A kind of Mo doping SnO is provided in the present embodiment2The preparation method of composite S nS material, specific preparation method are as follows.
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly, mixing time is 1 h, and solution is dense Degree is 6 mg/mL, and tin tetrachloride: ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
(2) it takes above-mentioned 40 mL solution to be put into the hydrothermal reaction kettle that volume is 50 mL, is put into after hydrothermal reaction kettle sealing 24 h are heated in drying box, temperature is 200 DEG C.
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, is centrifuged 3 times using deionized water.
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
Embodiment 3:
A kind of Mo doping SnO is provided in the present embodiment2The preparation method of composite S nS material, specific preparation method are as follows.
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly, mixing time is 1 h, and solution is dense Degree is 5 mg/mL, and tin tetrachloride: ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
(2) it takes above-mentioned 40 mL solution to be put into the hydrothermal reaction kettle that volume is 50 mL, is put into after hydrothermal reaction kettle sealing 24 h are heated in drying box, temperature is 200 DEG C.
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, is centrifuged 3 times using deionized water.
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
Embodiment 4:
A kind of Mo doping SnO is provided in the present embodiment2The preparation method of composite S nS material, specific preparation method are as follows.
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly, mixing time is 1 h, and solution is dense Degree is 6 mg/mL, and tin tetrachloride: ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
(2) it takes above-mentioned 80 mL solution to be put into the hydrothermal reaction kettle that volume is 100 mL, is put into after hydrothermal reaction kettle sealing 18 h are heated in drying box, temperature is 200 DEG C.
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, is centrifuged 3 times using deionized water.
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
Embodiment 5:
A kind of Mo doping SnO is provided in the present embodiment2The preparation method of composite S nS material, specific preparation method are as follows.
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly, mixing time is 1 h, and solution is dense Degree is 6 mg/mL, and tin tetrachloride: ammonium molybdate: the mass ratio of thiocarbamide is 2:1:1.
(2) it takes above-mentioned 80 mL solution to be put into the hydrothermal reaction kettle that volume is 100 mL, is put into after hydrothermal reaction kettle sealing 30 h are heated in drying box, temperature is 190 DEG C.
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, is centrifuged 5 times using deionized water.
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention, Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.

Claims (9)

1. a kind of Mo adulterates SnO2The preparation method of composite S nS material, comprising the following steps:
(1) tin tetrachloride, ammonium molybdate and thiocarbamide are added in deionized water, stirs evenly；
(2) it takes above-mentioned solution to be put into hydrothermal reaction kettle, is put into drying box and heats after hydrothermal reaction kettle sealing；
(3) stop heating, be cooled to room temperature to hydrothermal reaction kettle temperature, be centrifuged using deionized water；
(4) SnO is adulterated after the sample drying after being centrifuged to get Mo2Composite S nS material.
2. preparation method according to claim 1, which is characterized in that tin tetrachloride, ammonium molybdate are added in the step (1) Concentration with solution after thiocarbamide is 1 ~ 10 mg/mL.
3. preparation method according to claim 1, which is characterized in that tin tetrachloride in the step (1): ammonium molybdate: sulphur The mass ratio of urea is 2:1:1.
4. preparation method according to claim 1, which is characterized in that mixing time is 0.5 ~ 5 h in the step (1).
5. preparation method according to claim 1, which is characterized in that in the step (2) volume of reaction kettle be 50 or 100 mL。
6. preparation method according to claim 1, which is characterized in that the appearance of solution in a kettle in the step (2) Amount is the 70% ~ 90% of reactor volume.
7. preparation method according to claim 1, which is characterized in that drying box heating temperature is 180 in the step (2) ~200 ℃。
8. preparation method according to claim 1, which is characterized in that in the step (2) drying box heating time be 18 ~ 36 h。
9. preparation method according to claim 1, which is characterized in that centrifugation number is 3 ~ 5 times in the step (3).
CN201811322280.2A 2018-11-08 2018-11-08 A kind of Mo doping SnO2The preparation method of composite S nS material Pending CN109360965A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114577860A (en) * 2022-01-14 2022-06-03 浙江大学 Metal oxide low-temperature hydrogen sensitive material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2024525A4 (en) * 2006-06-06 2013-07-10 Coppe Ufrj Magnesium based-alloys for hydrogen storage
CN108448091A (en) * 2018-03-20 2018-08-24 济南大学 A kind of MoO2/SnS2Nanocomposite and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2024525A4 (en) * 2006-06-06 2013-07-10 Coppe Ufrj Magnesium based-alloys for hydrogen storage
CN108448091A (en) * 2018-03-20 2018-08-24 济南大学 A kind of MoO2/SnS2Nanocomposite and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HAOJIE LI 等: "Fabrication of MoS2@SnO2-SnS2 composites and their applications as anodes for lithium ion batteries", 《MATERIALS RESEARCH BULLETIN》 *
殷立雄 等: "Zn掺杂SnS2/SnO2复合材料的制备及其光催化性能", 《陕西科技大学学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114577860A (en) * 2022-01-14 2022-06-03 浙江大学 Metal oxide low-temperature hydrogen sensitive material and preparation method thereof
CN114577860B (en) * 2022-01-14 2024-01-30 浙江大学 Metal oxide low-temperature hydrogen sensitive material and preparation method thereof

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Application publication date: 20190219