CN102583272A - Vermicular Sb2Se3 hydrogen storage material and preparation method thereof - Google Patents

Vermicular Sb2Se3 hydrogen storage material and preparation method thereof Download PDF

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Publication number
CN102583272A
CN102583272A CN2012100194116A CN201210019411A CN102583272A CN 102583272 A CN102583272 A CN 102583272A CN 2012100194116 A CN2012100194116 A CN 2012100194116A CN 201210019411 A CN201210019411 A CN 201210019411A CN 102583272 A CN102583272 A CN 102583272A
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hydrogen storage
storage material
vermiform
preparation
sb2se3
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陈刚
邹贤
金仁成
邓明达
闫春爽
孙帅
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention discloses a vermicular Sb2Se3 hydrogen storage material and a preparation method thereof, and relates to a hydrogen storage material and a preparation method. The utility model aims at solving the technical problems that the requirement for equipment is strict, the energy consumption is larger and the product needs to be purified in the existing method for preparing the carbon nano tube hydrogen storage material. The vermicular Sb2Se3 hydrogen storage material is a vermicular Sb2Se3 which is prepared by adopting a solvothermal synthesis method for antimony potassium tartrate, sodium selenite, glucose and a mixed solvent. The preparation method comprises the following steps of: uniformly mixing the antimony potassium tartrate, the sodium selenite, the glucose and the mixed solvent, adding the mixture into a reactor for reaction, cleaning a product and obtaining the vermicular Sb2Se3 hydrogen storage material. The diameter of the vermicular Sb2Se3 hydrogen storage material is 1-2mum, and the length of the vermicular Sb2Se3 hydrogen storage material is tens of micrometers; each vermicular Sb2Se3 is formed by self assembly of numerous Sb2Se3 nanosheets. The discharging capacity of the vermicular Sb2Se3 hydrogen storage material is up to 248mAhg-1, and the purity of the vermicular Sb2Se3 hydrogen storage material is up to 99%-100%; and the vermicular Sb2Se3 hydrogen storage material can be applied in the field of large-scale hydrogen storage.

Description

Vermiform Sb 2Se 3Hydrogen storage material and preparation method thereof
Technical field
The present invention relates to a kind of hydrogen storage material and preparation method.
Background technology
Current, the whole world has all given great attention to the energy and environmental problem.Along with expanding economy; People increase the increasing demand of resource; Fossil oil can not satisfy people to demands for energy, and the human simultaneously excessive exploitation to nature has caused serious environmental to pollute and environmental disruption; " Greenhouse effect " and Organic pollutants that the carbonic acid gas isothermal chamber gas that combustion of fossil fuels produces causes are serious day by day, and exploitation is clean, new forms of energy are extremely urgent efficiently.Hydrogen Energy is as unique pollution-free reproducible energy, and a new generation is by the energy that extensively adopts after the non-renewable energies such as oil, coal and Sweet natural gas that continue beyond doubt.And the most critical issue that hinders the extensive use of Hydrogen Energy is the storage and the transportation of Hydrogen Energy.All there is major defect in present hydrogen storage technology, and wherein the quality hydrogen-storage density and the volume hydrogen-storage density of liquid hydrogen storing technology are the highest, but the poor stability of high-pressure liquefaction, cost is high.The volume hydrogen-storage density of metal hydride storing technology is higher, but the quality hydrogen-storage density is minimum.Therefore hydrogen storage material is imperative with the hydrogen storage technology of safety efficiently for development of new.
In order to develop hydrogen storage material efficiently, numerous countries and investigator are carrying out unremitting effort.1991, the Electronic Speculum expert of Japanese NEC Corporation chanced on carbon nanotube when preparation C60, because it has characteristics such as lower density and higher specific surface area and has caused investigator's extensive concern.1992, thus Hamada N. finds that this material has excellent electrochemical hydrogen storage performance and started the upsurge of hydrogen Storage in Carbon Nanotubes research, and obtained important progress.And discover that different specific surface has bigger influence for the hydrogen storage property of material, its hydrogen storage capability of big specific surface area is also bigger.Preparation carbon nanotube method is a lot of at present, as: arc process, laser evaporation method and vapour deposition process etc., but these methods are strict to equipment requirements, and energy input is bigger, and product needs purifying.Many shortcomings have also hindered the process of its practicability.Therefore seeking new and effective, the simple hydrogen storage material of preparation method will be the inexorable trend that practicability is moved towards in the Chu Qing development.
Summary of the invention
Invention is to solve that the method for existing preparation carbon nanometer tube hydrogen-storage material is strict to equipment requirements, energy input is big and product needs the technical problem of purifying, and vermiform Sb is provided 2Se 3Hydrogen storage material and preparation method thereof.
Vermiform Sb of the present invention 2Se 3Hydrogen storage material is by antimonypotassium tartrate (K (SbO) C 4H 4O 60.5H 2O), Sodium Selenite (Na 2SeO 35H 2O), glucose and mixed solvent adopt the vermiform Sb that the solvent thermal synthesis method is processed 2Se 3Wherein the mol ratio of antimonypotassium tartrate and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL, and described mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume.
Above-mentioned vermiform Sb 2Se 3The preparation method of hydrogen storage material carries out according to the following steps:
One, takes by weighing antimonypotassium tartrate (K (SbO) C in the ratio that the mol ratio of antimony tartrate potassium and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL 4H 4O 60.5H 2O), Sodium Selenite (Na 2SeO 35H 2O), glucose and mixed solvent and mix, obtain mixing solutions; Wherein said mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, and being placed on temperature is to react 1.5～18h in 140～200 ℃ of baking ovens;
Three, reaction kettle is taken out, naturally cool to room temperature, pour out product and clean, be placed on temperature then and be drying 10～16h in 40～70 ℃ the vacuum drying oven, obtain vermiform Sb with absolute ethyl alcohol and distilled water wash 2Se 3Hydrogen storage material.
Vermiform Sb of the present invention 2Se 3The cost of material that the preparation method of hydrogen storage material adopts is low, device is simple and easy and simple to operate., utilize in the solvent-thermal method building-up process as solvent with quadrol and ethylene glycol mixtures, the hydroxyl of solvent and the effect of product particle suppress the growth of particular crystal plane, are vermiform Sb thereby obtain microscopic appearance 2Se 3This vermiform Sb 2Se 3" worm " of hydrogen storage material, its diameter are 1～2 μ m, and length is tens of microns; Each vermiform Sb 2Se 3Be by many slick Sb 2Se 3Nanometer sheet (diameter is about 1 μ m, and thickness is about 40nm) self-assembly forms.This vermiform Sb 2Se 3The loading capacity of hydrogen storage material is up to 248mAh g -1, the electrochemical hydrogen storage performance is strong, and microscopic appearance uniqueness, even particle size, sample purity do not need purification process once more up to 99%～100%, can be applicable to mass-producing Chu Qing field.
Description of drawings
Fig. 1 is the vermiform Sb of test one preparation 2Se 3The XRD spectra of hydrogen storage material;
Fig. 2 is the vermiform Sb of test one preparation 2Se 3The low resolution SEM spectrogram of hydrogen storage material;
Fig. 3 is the vermiform Sb of test one preparation 2Se 3The high resolving power SEM spectrogram of hydrogen storage material.
Fig. 4 is the vermiform Sb of preparation 2Se 3The charging and discharging curve figure of hydrogen storage material, wherein a is a charging curve, b is a discharge curve.
Embodiment
Embodiment one: this embodiment vermiform Sb of the present invention 2Se 3Hydrogen storage material is by antimonypotassium tartrate (K (SbO) C 4H 4O 60.5H 2O), Sodium Selenite (Na 2SeO 35H 2O), glucose and mixed solvent adopt the vermiform Sb that the solvent thermal synthesis method is processed 2Se 3Wherein the mol ratio of antimonypotassium tartrate and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL, and described mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume.
The vermiform Sb of this embodiment 2Se 3The cost of material that the preparation method of hydrogen storage material adopts is low, device is simple and easy and simple to operate.This vermiform Sb 2Se 3The microscopic appearance of hydrogen storage material is a vermiform, and its diameter is 1～2 μ m, and length is tens of microns; Each vermiform Sb 2Se 3Be by many slick Sb 2Se 3Nanometer sheet (diameter is about 1 μ m, and thickness is about 40nm) self-assembly forms.This vermiform Sb 2Se 3The loading capacity of hydrogen storage material is up to 248mA h g -1, the electrochemical hydrogen storage performance is strong, and microscopic appearance uniqueness, even particle size, sample purity can be applicable to mass-producing Chu Qing field up to 99%～100%.
Embodiment two: the vermiform Sb of this embodiment 2Se 3The preparation method of hydrogen storage material carries out according to the following steps:
One, takes by weighing antimonypotassium tartrate (K (SbO) C in the ratio that the mol ratio of antimony tartrate potassium and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL 4H 4O 60.5H 2O), Sodium Selenite (Na 2SeO 35H 2O), glucose and mixed solvent and mix, obtain mixing solutions; Described mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, and being placed on temperature is to react 1.5～18h in 140～200 ℃ of baking ovens;
Three, reaction kettle is taken out, naturally cool to room temperature, pour out product and clean, be placed on temperature then and be drying 10～16h in 40～70 ℃ the vacuum drying oven, obtain vermiform Sb with absolute ethyl alcohol and distilled water wash 2Se 3Hydrogen storage material.
The vermiform Sb of this embodiment preparation 2Se 3The cost of material that the preparation method of hydrogen storage material adopts is low, device is simple and easy and simple to operate.This vermiform Sb 2Se 3The microscopic appearance of hydrogen storage material is a vermiform, and its diameter is 1～2 μ m, and length is tens of microns; Each vermiform Sb 2Se 3Be by many slick Sb 2Se 3Nanometer sheet (diameter is about 1 μ m, and thickness is about 40nm) self-assembly forms.This vermiform Sb 2Se 3The loading capacity of hydrogen storage material is up to 248mA h g -1, the electrochemical hydrogen storage performance is strong, and microscopic appearance uniqueness, even particle size, sample purity can be applicable to mass-producing Chu Qing field up to 99%～100%.
Embodiment three: this embodiment and embodiment two are different is that the mol ratio of step 1 unresolvable tartaric acid antimony potassium and Sodium Selenite is 2: 2.95～3.05, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.5～3.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 235～245mL.Other are identical with embodiment two.
In this embodiment, glucose is tensio-active agent.
Embodiment four: this embodiment and embodiment two are different is that the mol ratio of step 1 unresolvable tartaric acid antimony potassium and Sodium Selenite is that the mass ratio of 2: 3, antimonypotassium tartrate and glucose is that the mass volume ratio of 1: 3, antimonypotassium tartrate and mixed solvent is 1g: 240mL.Other are identical with embodiment two.
Embodiment five: this embodiment is different with one of embodiment two to four is that mixed solvent in the step 1 is 1: 2.2～2.8 to mix by quadrol and terepthaloyl moietie by volume.Other are identical with one of embodiment two to four.
Embodiment six: this embodiment is different with one of embodiment two to four is that mixed solvent in the step 1 is to mix at 1: 2.5 by quadrol and terepthaloyl moietie by volume.Other are identical with one of embodiment two to four.
Embodiment seven: what this embodiment was different with one of embodiment two to six is that temperature of oven is 160～180 ℃ in the step 2, and the reaction times is 3～12h.Other are identical with one of embodiment two to six.
Embodiment eight: what this embodiment was different with one of embodiment two to six is that temperature of oven is 180 ℃ in the step 2, and the reaction times is 9h.Other are identical with one of embodiment two to six.
Embodiment nine: what this embodiment was different with one of embodiment two to eight is that vacuum drying temperature is 45～60 ℃ in the step 3, and the vacuum drying time is 12～14h.Other are identical with one of embodiment two to eight.
Embodiment ten: what this embodiment was different with one of embodiment two to eight is that vacuum drying temperature is 60 ℃ in the step 3, and the vacuum drying time is 12h.Other are identical with one of embodiment two to eight.
The present invention adopts following verification experimental verification beneficial effect of the present invention:
Test one: the vermiform Sb of this test 2Se 3The preparation method of hydrogen storage material carries out according to the following steps:
One, takes by weighing 0.134g antimonypotassium tartrate (K (SbO) C 4H 4O 60.5H 2O), 0.16g Sodium Selenite (Na 2SeO 35H 2O), the quadrol of 0.45g glucose and 21mL terepthaloyl moietie and 11mL and mixing, obtain mixing solutions;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, and being placed on temperature is to react 9h in 180 ℃ of baking ovens;
Three, reaction kettle is taken out, naturally cool to room temperature, pour out product and wash 3 times, use distilled water wash again 3 times, be placed on temperature then and be 60 ℃, vacuum tightness and be dry 12h in the vacuum drying oven of 0.095MPa, obtain vermiform Sb with absolute ethyl alcohol 2Se 3Hydrogen storage material.
The vermiform Sb that this test obtains 2Se 3Hydrogen storage material is from be seen as the Sb of black in appearance 2Se 3Powder, this vermiform Sb 2Se 3The X-ray diffraction spectrogram of hydrogen storage material is as shown in Figure 1, as can beappreciated from fig. 1, and vermiform Sb 2Se 3Hydrogen storage material be by pure Sb 2Se 3, do not have other element.
The vermiform Sb that this test obtains 2Se 3The low resolution SEM spectrogram of hydrogen storage material is as shown in Figure 2, as can beappreciated from fig. 2 vermiform Sb 2Se 3Diameter be about 2 μ m, length is tens of micron.
The vermiform Sb that this test obtains 2Se 3The high resolving power SEM spectrogram of hydrogen storage material is as shown in Figure 3, as can beappreciated from fig. 3 each vermiform Sb 2Se 3Be by many slick Sb 2Se 3The nanometer sheet self-assembly forms, and the diameter of nanometer sheet is about 1 μ m, and thickness is about 40nm.
Vermiform Sb with this test preparation 2Se 3Hydrogen storage material is that the condition of 20Mpa is depressed on the nickel foam thin slice as working electrode at pressure, and the length of working electrode is 12mm, and thickness is 1mm, with Ni (OH) 2/ NiOOH is as counter electrode, and Hg/HgO takes off N as reference electrode 2The KOH solution of the 6M that handles is gone up with three-electrode system test vermiform Sb at Land batterysystem (CT2001A) as electrolyte solution 2Se 3The loading capacity of hydrogen storage material, keeping the temperature of electrolyte solution during test is 25 ℃, working electrode is at 50mA g -1The 4h that charges under the current density, the charging and discharging curve figure that intermittently discharge obtains under same current density behind the 5s is as shown in Figure 4, and wherein a is a charging curve, and b is a discharge curve, and as can beappreciated from fig. 4, this sample loading capacity is up to 248mA h g -1, shown the remarkable hydrogen storage ability of this sample potential.

Claims (10)

1. vermiform Sb 2Se 3Hydrogen storage material is characterized in that vermiform Sb 2Se 3Hydrogen storage material is the vermiform Sb that adopts the solvent thermal synthesis method to process by antimonypotassium tartrate, Sodium Selenite, glucose and mixed solvent 2Se 3Wherein the mol ratio of antimonypotassium tartrate and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL, and described mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume.
2. prepare vermiform Sb as claimed in claim 1 2Se 3The method of hydrogen storage material is characterized in that vermiform Sb 2Se 3The preparation method of hydrogen storage material carries out according to the following steps:
One, takes by weighing antimonypotassium tartrate, Sodium Selenite, glucose and mixed solvent in the ratio that the mol ratio of antimony tartrate potassium and Sodium Selenite is 2: 2.9～3.1, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.1～4.5, the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 230～250mL and mix, obtain mixing solutions; Described mixed solvent is 1: 2～3 to mix by quadrol and terepthaloyl moietie by volume;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, and being placed on temperature is to react 1.5～18h in 140～200 ℃ of baking ovens;
Three, reaction kettle is taken out, naturally cool to room temperature, pour out product and clean, be placed on temperature then and be drying 10～16h in 40～70 ℃ the vacuum drying oven, obtain vermiform Sb with absolute ethyl alcohol and distilled water wash 2Se 3Hydrogen storage material.
3. vermiform Sb according to claim 2 2Se 3The preparation method of hydrogen storage material, the mol ratio that it is characterized in that step 1 unresolvable tartaric acid antimony potassium and Sodium Selenite are 2: 2.95～3.05, the mass ratio of antimonypotassium tartrate and glucose is 1: 1.5～3.5), the mass volume ratio of antimonypotassium tartrate and mixed solvent is 1g: 235～245mL.
4. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material, the mol ratio that it is characterized in that step 1 unresolvable tartaric acid antimony potassium and Sodium Selenite are that the mass ratio of 2: 3, antimonypotassium tartrate and glucose is that the mass volume ratio of 1: 3, antimonypotassium tartrate and mixed solvent is 1g: 240mL.
5. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that the mixed solvent in the step 1 is 1: 2.2～2.8 to mix by quadrol and terepthaloyl moietie by volume.
6. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that the mixed solvent in the step 1 is to mix at 1: 2.5 by quadrol and terepthaloyl moietie by volume.
7. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that temperature of oven is 160～180 ℃ in the step 2, and the reaction times is 3～12h.
8. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that temperature of oven is 180 ℃ in the step 2, and the reaction times is 9h.
9. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that vacuum drying temperature is 45～60 ℃ in the step 3, and the vacuum drying time is 12～14h.
10. according to claim 2 or 3 described vermiform Sb 2Se 3The preparation method of hydrogen storage material is characterized in that vacuum drying temperature is 60 ℃ in the step 3, and the vacuum drying time is 12h.
CN2012100194116A 2012-01-21 2012-01-21 Vermicular Sb2Se3 hydrogen storage material and preparation method thereof Pending CN102583272A (en)

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Cited By (5)

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CN105603532A (en) * 2016-03-23 2016-05-25 岭南师范学院 Preparation method of antimony selenide monocrystal microparticles
CN106848386A (en) * 2017-01-23 2017-06-13 陕西科技大学 A kind of sodium-ion battery negative pole nest like Sb2Se3The preparation method of electrode material
CN107055489A (en) * 2017-05-27 2017-08-18 陕西科技大学 It is a kind of to prepare the method that nano wire weaves spherical antimony selenide anode material of lithium-ion battery
CN107140608A (en) * 2017-05-27 2017-09-08 陕西科技大学 A kind of ultrasonic assistant hydro-thermal prepares method of the sodium-ion battery negative pole with ultra-dispersed antimony selenide nano wire
CN107959024A (en) * 2017-11-07 2018-04-24 陕西科技大学 A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105603532A (en) * 2016-03-23 2016-05-25 岭南师范学院 Preparation method of antimony selenide monocrystal microparticles
CN105603532B (en) * 2016-03-23 2018-05-22 岭南师范学院 A kind of preparation method of antimony selenide micron single crystal grain
CN106848386A (en) * 2017-01-23 2017-06-13 陕西科技大学 A kind of sodium-ion battery negative pole nest like Sb2Se3The preparation method of electrode material
CN106848386B (en) * 2017-01-23 2019-09-03 陕西科技大学 A kind of sodium-ion battery cathode nest like Sb2Se3The preparation method of electrode material
CN107055489A (en) * 2017-05-27 2017-08-18 陕西科技大学 It is a kind of to prepare the method that nano wire weaves spherical antimony selenide anode material of lithium-ion battery
CN107140608A (en) * 2017-05-27 2017-09-08 陕西科技大学 A kind of ultrasonic assistant hydro-thermal prepares method of the sodium-ion battery negative pole with ultra-dispersed antimony selenide nano wire
CN107959024A (en) * 2017-11-07 2018-04-24 陕西科技大学 A kind of sodium-ion battery anode sheet Sb2Se3Nanocrystalline preparation method

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Application publication date: 20120718