CN106898691A - A kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material - Google Patents
A kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material Download PDFInfo
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- CN106898691A CN106898691A CN201510961008.9A CN201510961008A CN106898691A CN 106898691 A CN106898691 A CN 106898691A CN 201510961008 A CN201510961008 A CN 201510961008A CN 106898691 A CN106898691 A CN 106898691A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
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- C01G39/06—Sulfides
Abstract
The invention discloses a kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material.The preparation method of oxygen doping molybdenum bisuphide thermoelectric material is comprised the following steps：The MoS of certain mass is weighed first2Powder, it is laid in corundum boat, then it is put into the quartz ampoule of horizontal pipe furnace, it is raised to certain temperature, constant temperature regular hour in air atmosphere, the molybdenum disulfide powder of oxygen doping is obtained, the bulk thermoelectric material of densification is finally sintered into using discharge plasma sintering technology (SPS).Substantially, with conductance higher and Seebeck coefficients, thermoelectricity capability is preferable for the polycrystalline oxygen doping molybdenum bisuphide thermoelectric material preferred orientation that preparation method of the invention is obtained.In addition, oxygen doping molybdenum bisuphide also can be applicable to the fields such as electrochemistry, photoelectrocatalysis, electronic device.
Description
Technical field
The present invention relates to thermoelectric material field, more particularly to a kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material.
Background technology
More than the 50% of the today's society energy is all lost in the form of used heat, and thermoelectric material can be realized between heat energy and electric energy
The development of mutually conversion, therefore thermoelectric material will may consequently contribute to solve energy crisis.Evaluating the parameter of pyroelectric material performance quality is
Thermoelectric figure of merit ZT, ZT=S2σ T/ κ, wherein S represent Seebeck coefficients, and σ represents electrical conductivity, and T represents absolute temperature, κ
Represent thermal conductivity, S2σ is referred to as power factor (Power Factor).ZT values are higher, and thermoelectric energy transformation efficiency is higher.Improve
ZT values are, it is necessary to improve Seebeck coefficients and conductance, while reducing thermal conductivity.At present, performance thermoelectric material high generally contains
Poisonous and expensive metal, such as Te, Pb, hinder their large-scale practical application.Therefore, develop new
Nontoxic cheap thermoelectric material turn into thermoelectricity field study hotspot.
Molybdenum bisuphide is a kind of two-dimensional semiconductor material of stratiform.Current molybdenum bisuphide be not as the research of thermoelectric material it is a lot,
And it is concentrated mainly on the research of film, such as 2013 Michele Buscema et al. can be by the sulphur of individual layer two by extra electric field
Change the Seebeck coefficient adjustments of molybdenum to -4 × 102To -1 × 105μV K-1Between；Wu Jing in 2014 et al. pass through Applied gate
The carrier concentration of the individual layer molybdenum bisuphide of voltage-regulation CVD growth, makes its Seebeck value can reach~30mV K-1.Although
Although in this way, they also indicate that the Seebeck coefficients of individual layer molybdenum bisuphide are very big in article, as thermoelectric material
It is exactly too big resistance to still suffer from a very big challenge.Two groups of Shi Li and Zhang Xiang in 2015 have studied few layer respectively
The thermoelectricity capability of molybdenum bisuphide, be obtained in the in-plane direction power factor very high (>5mW m-1K-2), but because
Thermal conductivity (the 30-50W m higher in this direction-1K-1), ZT values also only only have 0.05.
The content of the invention
The problem to be solved in the present invention is：Overcome the deficiencies in the prior art, there is provided a kind of oxygen doping molybdenum bisuphide thermoelectric material
Preparation method, in the case where molybdenum bisuphide Seebeck coefficients are not reduced, improve molybdenum bisuphide conductance, while energy
Enough effectively to reduce thermal conductivity, the final thermoelectricity capability for causing material is greatly enhanced.
The invention provides a kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material, it is characterised in that the preparation method
Comprise the following steps：
(1) molybdenum disulfide powder of certain mass is weighed, is put into container；
(2) container in step (1) is put into quartz ampoule；
(3) quartz ampoule in step (2) is put into horizontal pipe furnace, suitable temperature is warming up under argon gas atmosphere, then change
It is air, the constant temperature regular hour, is then replaced by argon gas Temperature fall, obtains the molybdenum disulfide powder sample of oxygen doping；
(4) the oxygen doping molybdenum disulfide powder sample for obtaining step (3) carries out discharge plasma sintering, first mixes oxygen
Miscellaneous molybdenum disulfide powder is fitted into graphite jig, is put into discharge plasma sintering furnace, pressurization, vacuumizes, and works as vacuum
During less than 5Pa, sintering is started to warm up, insulation a period of time when being raised to maximum temperature, then direct release, Temperature fall, obtain
To fine and close oxygen doping molybdenum bisuphide thermoelectric material.
The molybdenum disulfide powder of the certain mass in the step (1) is 2-6g；The particle diameter of molybdenum disulfide powder is less than 6um.
The MoS of this particle diameter2Oxygen doping effect is relatively good in oxygen doping method of the present invention, and preferred orientation after SPS sintering
Also it is obvious.Container select be corundum boat, because corundum boat under experimental temperature of the present invention (200-500 DEG C) with
MoS2Do not react.
Quartz tube in the step (2) is 40-60mm, and a length of 0.8-1.5m, optimum diameter is 50mm, a length of
1m。
Temperature in the step (3) is 200-500 DEG C；Constant temperature time is 4min-10h；Lead to all in the gentle temperature-fall period of liter
It is argon gas, argon gas flow velocity is 70-80sccm (optimal is 76sccm)；What is led in thermostatic process is air, and air velocity is
100sccm.The content of oxygen when the size of air velocity determines oxidation reaction, is to determine MoS2Degree of oxidation is oxygen doping journey
One of essential condition of degree, when air velocity is 100sccm in the present invention, oxygen content is most suitable, is gone again under this flow conditions
The temperature and time of oxidation is adjusted, the data of the thermoelectricity capability for obtaining can well illustrate change of the thermoelectricity capability with oxygen doping degree
Trend.
The a diameter of 12.7-20mm of graphite jig used by sintering process in the step (4), is highly 30-35mm.Added
Pressure is 40-60MPa, and sintering temperature is 1100-1400 DEG C, and heating rate is 50-100 DEG C/min, and soaking time is
10-180min.Under this sintering condition, the density of material can reach more than the 95% of body phase material density, and when needs
When sintering obtains the material of comparing (12mm or so) high, will not be broken with this sintering condition material.
The degree of grain alignment of the oxygen doping molybdenum bisuphide thermoelectric material is more than or equal to 0.9.
In an instantiation, argon gas flow velocity is 76sccm when rising gentle cooling, and constant temperature time is 5h, and air velocity is
100sccm.The oxygen doping MoS obtained under the conditions of this2Thermoelectricity capability be best.
In an instantiation, comprise the following steps：
The molybdenum disulfide powder of the oxygen doping that a. will be obtained is fitted into the graphite jig of diameter 12.7mm.
B. mould is put into SPS sintering furnaces, pressurize 50MPa, vacuumizes.
C. when vacuum is less than 5Pa, stream intensification sintering, 50-100 DEG C of heating rate/min, sintering temperature are begun to power up
1300 DEG C, 2h, then direct release, Temperature fall are incubated at 1300 DEG C.
The advantage of the invention is that：
(1) method of the present invention by aoxidizing in atmosphere, introduces oxygen in molybdenum bisuphide, is greatly improved two
The conductance of molybdenum sulfide, can at least improve more than 1000 times, and the Seebeck coefficients of the molybdenum bisuphide after oxygen doping are absolute
Without reducing, the absolute value range of Seebeck coefficients is 50-586 μ V K to value before doping-1, scope is after doping
300-500μV K-1, or even some temperature spots are than originally also high, so having obtained power factor higher.Power before doping
Level of factor is 10-10-10-5W m-1K-2Between, scope is 250-500W m after doping-1K-2。
(2) oxygen doping reduces the thermal conductivity of molybdenum bisuphide in the present invention.In MoS2In crystal layer on direction, thermal conductivity minimum value by
19W m originally-1K-1It is reduced to 12W m-1K-1, minimum value is by original 2.8W m on interlayer direction-1K-1Drop to 1.9W
m-1K-1.It can be seen that the present invention obtains the thermoelectric material with substantially orientation, orientation factor by the method that SPS is sintered
More than 0.9, so the thermal conductivity on interlayer direction is more lower, so that ZT values are greatly improved this side up.Mix
Miscellaneous preceding ZT is 0.003 to the maximum, and 0.14 has been brought up to after doping.
(3) preparation method of the invention is simple, easily a large amount of to prepare.
(4) oxygen doping molybdenum bisuphide thermoelectric material of the invention applies also for the neck such as electrochemistry, photoelectrocatalysis, electronic device
Domain.
Brief description of the drawings
Fig. 1 is the flow chart of preparation method of the present invention；
Fig. 2 is the conductance datagram of embodiment 1, embodiment 2 and embodiment 3；
Fig. 3 is the Seebeck coefficient data figures of embodiment 1, embodiment 2 and embodiment 3；
Fig. 4 is power factor (Power Factor) datagram of embodiment 1, embodiment 2 and embodiment 3；
Fig. 5 is the thermal conductivity datagram of embodiment 1, embodiment 2 and embodiment 3；
Fig. 6 is thermoelectric figure of merit (ZT) figure of embodiment 1, embodiment 2 and embodiment 3；
Fig. 7 is X-ray diffraction (XRD) figure of embodiment 1, embodiment 2 and embodiment 3.
Specific implementation method
Below in conjunction with the accompanying drawings and specific embodiment is discussed in detail the present invention.But following embodiment is only limitted to explain the present invention,
Protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
The specific preparation method of oxygen doping molybdenum bisuphide thermoelectric material of the invention is comprised the following steps：
(1) 5g molybdenum disulfide powders are weighed to be placed in corundum boat.Molybdenum disulfide powder particle diameter is less than 6um, corundum boat
Size is 3mm*6mm.Herein, molybdenum disulfide powder dispersion of trying one's best is laid in corundum boat, and should not be compacted,
Keep loose, be so able to effectively be contacted with atmosphere, and react uniform.
(2) above-mentioned corundum boat is put into the quartz ampoule of horizontal pipe furnace.Proper quartzy pipe size is diameter
50mm, length is 1m.
(3) toward atmosphere is passed through in quartz ampoule, 300 DEG C are warming up to, and constant temperature is for a period of time, then lowers the temperature.Before intensification,
First to lead to argon gas 1-2h scavenging pipelines, atmosphere is pure in keeping pipeline.Lead to argon gas in temperature-rise period, flow velocity is 76sccm,
Heating rate is 5 DEG C/min, when temperature is raised to 300 DEG C, switches to air, flow velocity to be adjusted to 100sccm, constant temperature at once
Regular hour (can be 4min-10h, constant temperature time is different, the degree of oxidation is different, by the time for changing constant temperature
Length changes the number that the degree of oxidation mixes oxygen, the thermoelectricity of the molybdenum bisuphide thermoelectric material of oxygen doping obtained from
Performance also can be different), last atmosphere switches to argon gas, flow velocity to be adjusted to 76sccm, starts Temperature fall, when temperature is dropped to
Sample is further taken out after room temperature, that is, obtains the molybdenum disulfide powder sample of oxygen doping.
(4) the molybdenum disulfide powder sample of the oxygen doping that will be obtained carries out discharge plasma (SPS) sintering：First will
Powder sample is attached to diameter 12.7mm, is compacted in the graphite jig of 30mm high, then the bag last layer carbon outside mould
, finally be put into for mould by felt (because sintering temperature is higher, the effect of carbon felt is, in order to be incubated, to prevent temperature to scatter and disappear)
In SPS sintering furnaces.Pressure is added to 50MPa, in order to molybdenum bisuphide is oxidized in preventing sintering process, first vacuumizes, very
When reciprocal of duty cycle is less than 5Pa, stream intensification sintering is begun to power up.Heating rate is tried one's best and is maintained at 50-100 DEG C/min, by 20min
Left and right temperature is raised to 1300 DEG C, and then for a period of time (10min-180min), constant temperature time has constant temperature to thermoelectricity capability
Influence.After constant temperature terminates, direct release, Temperature fall.
Embodiment 1
The molybdenum bisuphide thermoelectric material of oxygen doping, specific preparation method is as follows：
(1) 5g molybdenum disulfide powders are weighed to be placed in corundum boat, is put into the quartz ampoule of horizontal pipe furnace, quartz ampoule is straight
Footpath 50mm, a length of 1m；
(2) argon gas purging 2h is led in quartz ampoule, argon gas flow velocity is adjusted to 76sccm, and the heating rate of 5 DEG C/min rises to 300
DEG C, then gas switches to air, flow velocity 100sccm, constant temperature 0.5h, last gas to switch to argon gas, and flow velocity is 76sccm,
Start Temperature fall；
(3) powder sample that step (2) is obtained is fitted into the graphite jig of diameter 12.7mm, is put into SPS sintering furnaces
In, pressurize 50MPa, is evacuated to vacuum less than 5Pa, begins to power up stream intensification sintering, 20min or so and is warming up to
1300 DEG C, it is incubated 2h, then direct release, Temperature fall.
Embodiment 2
The molybdenum bisuphide thermoelectric material of oxygen doping, specific preparation method is as follows：
(1) 5g molybdenum disulfide powders are weighed to be placed in corundum boat, is put into the quartz ampoule of horizontal pipe furnace.
(2) argon gas purging 2h is led in quartz ampoule, argon gas flow velocity is adjusted to 76sccm, and the heating rate of 5 DEG C/min rises to 300
DEG C, then gas switches to air, flow velocity 100sccm, constant temperature 5h, last gas to switch to argon gas, and flow velocity is 76sccm,
Start Temperature fall.
(3) powder sample that step (2) is obtained is fitted into the graphite jig of diameter 12.7mm, is put into SPS sintering furnaces
In, pressurize 50MPa, is evacuated to vacuum less than 5Pa, begins to power up stream intensification sintering, 20min or so and is warming up to
1300 DEG C, it is incubated 2h, then direct release, Temperature fall.
Embodiment 3
The molybdenum bisuphide thermoelectric material of oxygen doping, specific preparation method is as follows：
(1) 5g molybdenum disulfide powders are weighed to be placed in corundum boat, is put into the quartz ampoule of horizontal pipe furnace.
(2) argon gas purging 2h is led in quartz ampoule, argon gas flow velocity is adjusted to 76sccm, and the heating rate of 5 DEG C/min rises to 300
DEG C, then gas switches to air, flow velocity 100sccm, constant temperature 10h, last gas to switch to argon gas, and flow velocity is 76sccm,
Start Temperature fall.
(3) powder sample that step (2) is obtained is fitted into the graphite jig of diameter 12.7mm, is put into SPS sintering furnaces
In, pressurize 50MPa, is evacuated to vacuum less than 5Pa, begins to power up stream intensification sintering, 20min or so and is warming up to
1300 DEG C, it is incubated 2h, then direct release, Temperature fall.
Test case
Electrical conductivity and Seebeck coefficients are tested
By embodiment 1, the fine and close block oxygen doping molybdenum bisuphide thermoelectricity material that SPS sintering is obtained in embodiment 2 and embodiment 3
Testing conductivity and Seebeck coefficients after material cutting, tester is ZEM-3.Range of measuring temp is 52-486 DEG C, is obtained
Electrical conductivity and Seebeck coefficients as shown in Figures 2 and 3.The conductance of embodiment 1, embodiment 2 and embodiment 3 is at 52 DEG C
When be respectively 1532S m-1、2137.6S m-1、2400.8S m-1, more than 1000 times are all improved before oxygen than not mixing.With temperature
The rising of degree, conductance reduction, is respectively 1357.3S m at 486 DEG C-1、1701.2S m-1、1774.7S m-1.Three embodiments
Seebeck coefficients all be negative value, explanation is N-shaped doped thermoelectric material.At 52 DEG C, Seebeck coefficients are respectively -403.1 μ V
K-1、-376.8μV K-1、-373.1μV K-1, being raised with temperature, absolute value increase is respectively -504.9 μ V K at 486 DEG C-1、
-464.0μV K-1、-464.2μV K-1。
Fig. 4 is the power factor being calculated by electrical conductivity and Seebeck coefficients.Raised with temperature, power factor increase, but
It is to be tended towards stability substantially to high temperature section.The power factor of embodiment 1 at 486 DEG C, embodiment 2 and embodiment 3 is respectively 346 μ W
m-1K-2、366.3μW m-1K-2、382.4μW m-1K-2。
Thermal conductivity is tested
By embodiment 1, embodiment 2 and the fine and close block oxygen doping molybdenum bisuphide thermoelectricity material that obtains of SPS sintering in embodiment 3
Thermal diffusion coefficient and specific heat are tested after material cutting, thermal conductivity is then calculated.Test thermal diffusion coefficient instrument is Germany
The laser of NETZSCH companies shines instrument (LFA457), and test specific heat instrument is the synchronization of German NETZSCH companies
Thermal analyzer (STA449), Range of measuring temp is 52-486 DEG C.Thermal conductivity result is as shown in Figure 5.Oxygen doping is reduced
MoS2Thermal conductivity.3.2W m are respectively during 52 DEG C of the thermal conductivity of embodiment 1, embodiment 2 and embodiment 3-1K-1、3.1W m-1
K-1、3.2W m-1K-1.Raised with temperature, thermal conductivity reduction is reduced to 2.1W m respectively to thermal conductivity at 486 DEG C-1K-1、1.9W m-1
K-1、2.1W m-1K-1。
Fig. 6 is the ZT values for finally giving.ZT values are especially low relative to improve more than 50 times before oxygen doping after oxygen doping
During warm 327K, improve more.486 DEG C, ZT values are maximum, embodiment 1, embodiment 2 and embodiment 3 be respectively 0.12,
0.14、0.13。
X-ray diffraction (XRD) is characterized
By embodiment 1, embodiment 2 and the fine and close block oxygen doping molybdenum bisuphide thermoelectricity material that obtains of SPS sintering in embodiment 3
Material cuts into suitably sized directly taking away and does XRD signs, and instrument is Rigaku D/Max-2500, XRD test knots
Fruit is as shown in Figure 7.Molybdenum bisuphide thermoelectric material after result display oxygen doping has obvious MoO2Peak occur.
Various embodiments above and test case are only intended to the explanation present invention, and those skilled in the art can be with according to the narration of the above
Fully achieve all the elements of claim, the same the various embodiments described above of embodiment method.
In a word, it is bright that oxygen doping molybdenum bisuphide thermoelectric material for being provided by the present invention and preparation method thereof can obtain preferred orientation
It is aobvious, the excellent oxygen doping molybdenum bisuphide thermoelectric material of thermoelectricity capability.By to oxygen is mixed in molybdenum bisuphide, in Seebeck
In the case that coefficient is not reduced, the conductance of molybdenum bisuphide is greatly improved, while thermal conductivity is reduced, so as to effectively carry
The thermoelectricity capability of molybdenum bisuphide high.
Above example is provided just for the sake of the description purpose of the present invention, and is not intended to limit the scope of the present invention.This hair
Bright scope is defined by the following claims.The various equivalents that do not depart from spirit and principles of the present invention and make and repair
Change, all should cover within the scope of the present invention.
Claims (11)
1. a kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material, it is characterised in that comprise the following steps：
(1) molybdenum disulfide powder of certain mass is weighed, is put into container；
(2) container in step (1) is put into quartz ampoule；
(3) quartz ampoule in step (2) is put into horizontal pipe furnace, uniform temperature is warming up under argon gas atmosphere, then be replaced by
Air, the constant temperature regular hour, is then replaced by argon gas Temperature fall, obtains the molybdenum disulfide powder sample of oxygen doping；
(4) the oxygen doping molybdenum disulfide powder sample for obtaining step (3) carries out discharge plasma sintering (SPS), first
The molybdenum disulfide powder of oxygen doping is fitted into graphite jig, pressurization in discharge plasma sintering furnace is put into, vacuumized, surely
When reciprocal of duty cycle is less than 5Pa, sintering is started to warm up, insulation a period of time when being raised to maximum temperature, then direct release, Temperature fall,
Obtain the block oxygen doping molybdenum bisuphide thermoelectric material of densification.
2. preparation method according to claim 1, it is characterised in that：Molybdenum disulfide powder in the step (1)
Quality is 2-6g；The particle diameter of molybdenum disulfide powder is less than 6um.
3. preparation method according to claim 1, it is characterised in that：Container in the step (1) is corundum boat.
4. preparation method according to claim 1, it is characterised in that：Quartz tube in the step (2) is
40-60mm, a length of 0.8-1.5m.
5. preparation method according to claim 1, it is characterised in that：Temperature in the step (3) is 200-500
℃。
6. preparation method according to claim 1, it is characterised in that：Constant temperature time in the step (3) is 4min-10h.
7. preparation method according to claim 1, it is characterised in that：In the step (3) in the gentle temperature-fall period of liter
Logical is all argon gas, and argon gas flow velocity is 70-80sccm；What is led in thermostatic process is air, and air velocity is 100sccm.
8. preparation method according to claim 1, it is characterised in that：Graphite used by sintering process in the step (4)
Mould diameter is 12.7-20mm, is highly 30-35mm.
9. preparation method according to claim 1, it is characterised in that：Pressure in the step (4) added by sintering process
Power is 40-60MPa.
10. preparation method according to claim 1, it is characterised in that：Sintering temperature is 1100-1400 in the step (4)
DEG C, heating rate is 50-100 DEG C/min, and soaking time is 10-180min.
11. preparation methods according to claim 1, it is characterised in that：The crystalline substance of the oxygen doping molybdenum bisuphide thermoelectric material
The grain degree of orientation is more than or equal to 0.9.
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| CN107302050A (en) * | 2017-06-30 | 2017-10-27 | 江西科技师范大学 | High conductivity molybdenum disulfide nano film and preparation method thereof |
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| CN108190854B (en) * | 2018-01-22 | 2019-12-27 | 西南交通大学 | Super-doped layer sub-pore carbon material and preparation method thereof |
| CN112978800A (en) * | 2019-12-17 | 2021-06-18 | 山东海科创新研究院有限公司 | High-conductivity molybdenum disulfide material and preparation method and application thereof |
| CN112978800B (en) * | 2019-12-17 | 2022-12-20 | 山东海科创新研究院有限公司 | High-conductivity molybdenum disulfide material and preparation method and application thereof |
| CN113929138A (en) * | 2021-10-12 | 2022-01-14 | 青岛科技大学 | Mo/O co-doped VS4 magnesium ion battery positive electrode material and application thereof |
| CN115894058A (en) * | 2022-11-25 | 2023-04-04 | 南京航空航天大学 | Method for flash-burning rapid densification of SiC/SiC composite material |
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Application publication date: 20170627 |