CN102583271A - Spine-like SbSe3 semiconductor hydrogen storage material and preparation method thereof - Google Patents
Spine-like SbSe3 semiconductor hydrogen storage material and preparation method thereof Download PDFInfo
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- CN102583271A CN102583271A CN2012100194046A CN201210019404A CN102583271A CN 102583271 A CN102583271 A CN 102583271A CN 2012100194046 A CN2012100194046 A CN 2012100194046A CN 201210019404 A CN201210019404 A CN 201210019404A CN 102583271 A CN102583271 A CN 102583271A
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Abstract
The invention discloses a Sb2Se3 semiconductor hydrogen storage material and a preparation method thereof and relates to a semiconductor hydrogen material and a preparation method thereof. The invention aims at solving the technical problems that a traditional carbon nano tube electrochemcial hydrogen storage material has strict requirement on the equipment and high energy consumption and the products are required to be purified. The spine-like Sb2Se3 semiconductor hydrogen storage material is prepared from K(SbO)C4H4O6.0.5H2O, Na2SeO3, a surfactant, ethylene glycol, water and hydrazine hydrate by using a hydrothermal synthesis method. The preparation method comprises the following steps: mixing the K(SbO)C4H4O6.0.5H2O, the Na2SeO3, the surfactant, the ethylene glycol, the water and the hydrazine hydrate; carrying out the hydrothermal reaction; and filtering, washing and drying to obtain the Sb2Se3 semiconductor hydrogen storage material. The Sb2Se3 semiconductor hydrogen storage material has surface specific area of 4.3-4.5m<2>.g<-1>, discharge capacity of 203.3-210mA.h.g<-1> and the purity of 99-100 percent and can be used as an electrode material.
Description
Technical field
The present invention relates to a kind of semi-conductor hydrogen storage material and preparation method thereof.
Background technology
Current, the energy and environmental problem are two hang-ups that face in the world wide, and traditional energies such as coal, oil, Sweet natural gas face the gesture of the exhaustion that reduces day by day, and the environmental problem of using these energy to bring simultaneously also is on the rise.Therefore develop pollution-free, renewable energy source is imperative.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.The key issue that hinders the extensive use of Hydrogen Energy is the storage and the transportation of Hydrogen Energy.At present, the cost that liquid hydrogen stores is high, security is relatively poor, and the hydrogen-storage amount that obtains during hydride hydrogen-storing is limited, and storage hydrogen mass density is too low.Limited its range of application.
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.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 will solve existing carbon nanotube electrochemical hydrogen bearing material equipment requirements strictness, energy input are needed the technical problem of purifying than big and product, and thorn-like Sb is provided
2Se
3Semi-conductor hydrogen storage material and preparation method thereof.
Thorn-like Sb of the present invention
2Se
3The semi-conductor hydrogen storage material is by K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be the Sb that 85% Hydrazine Hydrate 80 adopts the thorn-like that the solvent thermal synthesis method processes
2Se
3K (SbO) C wherein
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 10~15mL.
Tensio-active agent wherein is Hydrocerol A or glucose;
Thorn-like Sb of the present invention
2Se
3The preparation method of semi-conductor hydrogen storage material carries out according to the following steps:
One, presses K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is that the ratio of 1g: 10~15mL takes by weighing K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be 85% Hydrazine Hydrate 80 and mix, and obtains mixing solutions;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, puts into baking oven after the sealing, in temperature is to react 16~20 hours under 160~190 ℃ the condition;
Three, reaction kettle being taken out after cool to room temperature use absolute ethanol washing with the solid product that obtains, is drying 10~16h in 50~70 ℃ the baking oven in temperature then, obtains thorn-like Sb
2Se
3The semi-conductor hydrogen storage material.
Thorn-like Sb of the present invention
2Se
3The semi-conductor hydrogen storage material is made up of the three-dimensional manometer band of picture hedgehog shape, and these nano belt are that 5um, diameter are that the nanometer rod of 150nm is formed by many length.Thorn-like Sb of the present invention
2Se
3The cost of material of semi-conductor hydrogen storage material method is low, device is simple and easy, and simple to operate, and energy input is low.Prepared thorn-like Sb
2Se
3Semi-conductor hydrogen storage material, specific surface area are 4.3~4.5m
2.g
-1, electrochemical hydrogen storage better performances, loading capacity are 203.3~210mA h g
-1, purity does not need purification process up to 99%~100%.Can be applicable in the electrode materials of multiple battery.
Description of drawings
Fig. 1 is the thorn-like Sb of test one preparation
2Se
3The X ray diffracting spectrum of semi-conductor hydrogen storage material;
Fig. 2 is the thorn-like Sb of test one preparation
2Se
3The low power scanning electron microscope diagram of semi-conductor hydrogen storage material;
Fig. 3 is the thorn-like Sb of test one preparation
2Se
3The high power scanning electron microscope diagram of semi-conductor hydrogen storage material;
Fig. 4 is the thorn-like Sb of test one preparation
2Se
3The charging and discharging curve figure of semi-conductor storage hydrogen material, wherein a is the curve of charging, b is a discharge curve.
Embodiment
Embodiment one: the thorn-like Sb of this embodiment
2Se
3The semi-conductor hydrogen storage material is by K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be the Sb that 85% Hydrazine Hydrate 80 adopts the thorn-like that the solvent thermal synthesis method processes
2Se
3K (SbO) C wherein
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 10~15mL.
The thorn-like Sb of this embodiment
2Se
3The semi-conductor hydrogen storage material is made up of the three-dimensional manometer band of picture hedgehog shape, and these nano belt are that 5um, diameter are that the nanometer rod of 150nm is formed by many length.Thorn-like Sb of the present invention
2Se
3The cost of material of semi-conductor hydrogen storage material method is low, device is simple and easy, and simple to operate.Prepared thorn-like Sb
2Se
3Semi-conductor hydrogen storage material, specific surface area are 4.3~4.5m
2.g
-1, electrochemical hydrogen storage better performances, loading capacity are 203.3~210mA hg
-1., purity does not need purification process up to 99%~100%.Can be applicable in the electrode materials of multiple battery.
Embodiment two: what this embodiment and embodiment one were different is that tensio-active agent is Hydrocerol A or glucose.Other is identical with embodiment one.
Embodiment three: that this embodiment is different with embodiment one or two is K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.95~3.05, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 1~10, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 146~149mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 71~74mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 11~14mL.Other is identical with embodiment one or two.
Embodiment four: that this embodiment is different with embodiment one or two is K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 3, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 5, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 148mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 73mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 13mL.Other is identical with embodiment one or two.
Embodiment five: the thorn-like Sb of this embodiment
2Se
3The preparation method of semi-conductor hydrogen storage material carries out according to the following steps:
One, presses K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is that the ratio of 1g: 10~15mL takes by weighing K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be 85% Hydrazine Hydrate 80 and mix, and obtains mixing solutions;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, puts into baking oven after the sealing, in temperature is to react 16~20 hours under 160~190 ℃ the condition;
Three, reaction kettle being taken out after cool to room temperature use absolute ethanol washing with the solid product that obtains, is drying 10~16h in 50~70 ℃ the baking oven in temperature then, obtains thorn-like Sb
2Se
3The semi-conductor hydrogen storage material.
The thorn-like Sb of this embodiment preparation
2Se
3The semi-conductor hydrogen storage material is made up of the three-dimensional manometer band of picture hedgehog shape, and these nano belt are that 5um, diameter are that the nanometer rod of 150nm is formed by many length.Thorn-like Sb of the present invention
2Se
3The cost of material of semi-conductor hydrogen storage material method is low, device is simple and easy, and simple to operate.Prepared thorn-like Sb
2Se
3Semi-conductor hydrogen storage material, specific surface area are 4.3~4.5m
2.g
-1, electrochemical hydrogen storage better performances, loading capacity are 203.3~210mAh g
-1, purity does not need purification process up to 99%~100%.Can be applicable in the electrode materials of multiple battery.
Embodiment six: that this embodiment and embodiment five are different is K in the step 1 (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.95~3.05, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 1~10, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 146~149mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 71~74mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 11~14mL.Other is identical with embodiment five.
Embodiment seven: that this embodiment and embodiment five are different is K in the step 1 (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 3, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 5, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 148mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 73mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 13mL.Other is identical with embodiment five.
Embodiment eight: what this embodiment was different with one of embodiment five to seven is tensio-active agent Hydrocerol A or the glucose in the step 1.Other is identical with one of embodiment five to seven.
Embodiment nine: this embodiment is different with one of embodiment five to seven is that temperature in the step 2 is that 165~185 ℃, reaction times are 17~19 hours.Other is identical with one of embodiment five to seven.
Embodiment ten: this embodiment is different with one of embodiment five to seven is that drying temperature in the step 3 is that 55~65 ℃, time of drying are 12~15h.Other is identical with one of embodiment five to seven.
With following verification experimental verification beneficial effect of the present invention:
Test one: the thorn-like Sb of this test
2Se
3The preparation method of semi-conductor hydrogen storage material carries out according to the following steps:
One, takes by weighing 0.135g K (SbO) C
4H
4O
60.5H
2O, 0.086g Na
2SeO
3, 0.6g Hydrocerol A, 20mL terepthaloyl moietie, 10mL water and 2mL quality percentage composition be 85% Hydrazine Hydrate 80 and mix, and obtains mixing solutions;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, puts into baking oven after the sealing, is reaction 18 hours under 180 ℃ the condition in temperature;
Three, reaction kettle being taken out after cool to room temperature is used absolute ethanol washing with the solid product that obtains, is dry 12h in 60 ℃ the baking oven in temperature then, obtains thorn-like Sb
2Se
3The semi-conductor hydrogen storage material.
The thorn-like Sb that this test obtains
2Se
3The X ray diffracting spectrum of semi-conductor hydrogen storage material is as shown in Figure 1, as can beappreciated from fig. 1, and the thorn-like Sb of this test preparation
2Se
3Crystal is pure phase.
The thorn-like Sb that this test obtains
2Se
3The stereoscan photograph of semi-conductor hydrogen storage material low range is as shown in Figure 2, as can beappreciated from fig. 2, and thorn-like Sb
2Se
3The semi-conductor hydrogen storage material is made up of the three-dimensional manometer band of picture hedgehog shape, and these nano belt are about the nanometer rod that 5um, diameter be about 150nm by many length and form.
The thorn-like Sb that this test obtains
2Se
3The powerful stereoscan photograph of semi-conductor hydrogen storage material is as shown in Figure 3, as can beappreciated from fig. 3, and thorn-like Sb
2Se
3Nanometer rod length is that the 150nm diameter is 5um in the semi-conductor hydrogen storage material.
Thorn-like Sb with this test preparation
2Se
3The semi-conductor hydrogen storage material is that the condition of 20Mpa is depressed on the nickel foam thin slice as anode at pressure, and anodic is long to be 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 thorn-like Sb at Land battery system (CT2001A) as electrolyte solution
2Se
3The loading capacity of semi-conductor 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 the curve of charging, and b is a discharge curve, and as can beappreciated from fig. 4, this sample loading capacity is up to 203.3mAh g
-1, shown the remarkable hydrogen storage ability of this sample potential.
Claims (9)
1. thorn-like Sb
2Se
3The semi-conductor hydrogen storage material is characterized in that thorn-like Sb
2Se
3The semi-conductor hydrogen storage material is by K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be the Sb that 85% Hydrazine Hydrate 80 adopts the thorn-like that the solvent thermal synthesis method processes
2Se
3K (SbO) C wherein
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 10~15mL.
2. thorn-like Sb according to claim 1
2Se
3The semi-conductor hydrogen storage material is characterized in that tensio-active agent is Hydrocerol A or glucose.
3. thorn-like Sb according to claim 1 and 2
2Se
3The semi-conductor hydrogen storage material is characterized in that K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.95~3.05, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 1~10, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 146~149mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 71~74mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 11~14mL.
4. prepare thorn-like Sb as claimed in claim 1
2Se
3The method of semi-conductor hydrogen storage material is characterized in that thorn-like Sb
2Se
3The preparation method of semi-conductor hydrogen storage material carries out according to the following steps:
One, presses K (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.9~3.1, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 0.5~11, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 145~150mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 70~75mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is that the ratio of 1g: 10~15mL takes by weighing K (SbO) C
4H
4O
60.5H
2O, Na
2SeO
3, tensio-active agent, terepthaloyl moietie, water and quality percentage composition be 85% Hydrazine Hydrate 80 and mix, and obtains mixing solutions;
Two, the mixing solutions that step 1 is obtained is transferred in the reaction kettle, puts into baking oven after the sealing, in temperature is to react 16~20 hours under 160~190 ℃ the condition;
Three, reaction kettle being taken out after cool to room temperature use absolute ethanol washing with the solid product that obtains, is drying 10~16h in 50~70 ℃ the baking oven in temperature then, obtains thorn-like Sb
2Se
3The semi-conductor hydrogen storage material.
5. thorn-like Sb according to claim 4
2Se
3The preparation method of semi-conductor hydrogen storage material is characterized in that K in the step 1 (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 2.95~3.05, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 1~10, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 146~149mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 71~74mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 11~14mL.
6. thorn-like Sb according to claim 4
2Se
3The preparation method of semi-conductor hydrogen storage material is characterized in that K in the step 1 (SbO) C
4H
4O
60.5H
2O and Na
2SeO
3Mol ratio be 2: 3, K (SbO) C
4H
4O
60.5H
2The mass ratio of O and tensio-active agent is 1: 5, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and terepthaloyl moietie is 1g: 148mL, K (SbO) C
4H
4O
60.5H
2The mass volume ratio of O and water is 1g: 73mL, K (SbO) C
4H
4O
60.5H
2O and quality percentage composition are that the mass volume ratio of 85% Hydrazine Hydrate 80 is 1g: 13mL.
7. according to claim 4,5 or 6 described thorn-like Sb
2Se
3The preparation method of semi-conductor hydrogen storage material is characterized in that tensio-active agent Hydrocerol A or glucose in the step 1.
8. according to claim 4,5 or 6 described thorn-like Sb
2Se
3The preparation method of semi-conductor hydrogen storage material is characterized in that temperature in the step 2 is that 165~185 ℃, reaction times are 17~19 hours.
9. according to claim 4,5 or 6 described thorn-like Sb
2Se
3The preparation method of semi-conductor hydrogen storage material is characterized in that drying temperature in the step 3 is that 55~65 ℃, time of drying are 12~15h.
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