CN105272206B - A kind of preparation method of C and Ni codopes ZnO thermoelectric materials - Google Patents
A kind of preparation method of C and Ni codopes ZnO thermoelectric materials Download PDFInfo
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Abstract
A kind of preparation method of C and Ni codopes ZnO thermoelectric materials, belongs to technical field of energy material.The preparation method is using zinc chloride and nickel nitrate as raw material, and the mole of the zinc chloride and nickel nitrate is according to chemical general formula Zn1‑xNixO is configured, wherein, 0.005≤x≤0.6mol, and add C sources, using hydro-thermal method combination discharge plasma sintering method, C the and Ni codope ZnO block thermoelectric materials that relative density is more than 95% are made, the power factor of the C and Ni codopes ZnO block thermoelectric materials is 4 × 10‑4~8 × 10‑4Wm‑ 1K‑2.The present invention is by hydro-thermal method and higher with reference to C the and Ni codope ZnO block thermoelectric material relative densities that discharge plasma sintering method is prepared, more than 95%, sintering temperature height is at 950~1300 DEG C in preparation process, and the selection for passing through adulterated C sources overcomes the limitation that sintering temperature high in routine techniques is unfavorable for C doping ZnO；And further increase the thermoelectricity capability of ZnO material.
Description
Technical field
The invention belongs to technical field of energy material, it is related to a kind of preparation method of C and Ni codopes ZnO thermoelectric materials.
Background technology
With the quickening of process of industrialization and falling sharply for regenerative resource, in the urgent need to finding new green power.Heat
Electric material is as a kind of novel energy material that can be directly converted heat energy and electric energy, and the thermo-electric device being made from it has
Small volume, noiseless, movement-less part, high reliability, cause extensive pass in the field such as thermo-electric generation and thermoelectric cooling
Note.The performance of thermoelectric material can weigh ZT=α with dimensionless thermoelectric figure of merit ZT2σ T/ κ, wherein α are Seebeck coefficients, and σ is
Electrical conductivity, κ is thermal conductivity, and T is absolute temperature, α2σ is defined as the power factor of material, and high performance thermoelectric material needs high
σ and α and low κ.
ZnO thermoelectric materials are because its cost is low, abundant raw material, high-temperature stability are good and the advantages of nontoxic pollution-free, is considered as
It is one of a few cheap, cleaning, green novel energy source thermoelectric material, there is preferable development prospect in high-temperature field.Doping
Modification is that researcher is commonly used to improve the method for ZnO pyroelectric material performances, still, current several doping modification methods there are still
Some defects：
One：By the A positions Zn for replacing ZnO2+To optimize its thermoelectricity capability：When passing through Al3+、Ni2+、Ga3+、Bi3+、Ti4+With
Sb3+Usually replace ZnO A positions Zn Deng member2+When, due to doped chemical solid solubility low in ZnO, when doping reaches necessarily
During degree, often there is the second phase, its electrical transmission performance is deteriorated, and limits the further lifting of ZnO pyroelectric material performances.
For example, Ni2+With Zn2+With the ionic radius being closer to, Ni2+It is more easy to be solid-solution in ZnO compared to other Doped ions.On
Replace ZnO A positions Zn2+To optimize the existing research of its thermoelectricity capability：Research one uses liquid phase synthesis combination normal sintering legal system
For Ni doping ZnO thermoelectric ceramicses, higher Seebeck coefficients, about 350~400 μ VK are obtained-1.But because of Ni2+Doping is
Increase carrier concentration by way of changing energy level, its contribution to carrier is limited, it is impossible to obtain higher electrical conductivity；Grind
Study carefully two and Al and Ni codope ZnO thermoelectric ceramicses, Ni are prepared for using synthesis in solid state combination conventional sintering2+Preferentially it is solid-solution in ZnO
In, due to the limitation of solid solubility, Al3+It is difficult to be solidly soluted into ZnO, often with the second phase ZnAl2O4Form segregation in crystal boundary, limitation
The further liftings of ZnO thermoelectricity capabilities；Researchers also once attempted selection Al3+、Fe3+、Sm3+And Ga3+It is right etc. other ions
ZnO A positions Zn2+Progress is co-doped with substitution, but many limitations because of A substitution solid solubility can not significantly lift ZnO thermoelectricity capabilities.
Two：For ZnO B positions O2-Replace, replaced more than researchers using C element.C doping can reduce ZnO taboo
Bandwidth, increase electronics is transitted to the probability of conduction band by valence band.Meanwhile, according to defect equationCan
Know, C doping can directly provide extra electron, increase ZnO carrier concentration and electrical conductivity.For preparing C doping ZnO materials,
Due to the problems such as C sources select C unstability in difficult and high temperature sintering preparation process under high temperature so that C doping ZnO materials
Research is confined to film and powder sample, and the research of block sample is less.For the film for thermo-electric device and block material
For material, block materials make it in the application side of thermoelectric material because of the advantage such as preparation technology is simple, stability is good, assembling is convenient
Face has more advantage compared with thin-film material.Because C doping ZnO block materials prepare difficulty, it is also limited in block thermoelectric material
Research.On the B positions O to ZnO2-The existing research of substitution：Research one is using zinc acetate, cetyl trimethylammonium bromide as original
Material, Precursor Powder is made through hydro-thermal reaction, carries out calcining discovery at 500 DEG C and 700 DEG C respectively, and obtaining C during 500 DEG C of calcinings mixes
Miscellaneous ZnO powders, C is not almost solid-solution in ZnO at 700 DEG C, and high sintering temperature is unfavorable for C doping；For C doping ZnO
The report of block is less, and research two is using graphite as carbon source, C and Mn codope ZnO blocks are made in high annealing 12h at 800 DEG C, but
The sintering temperature that this method is used is 800 DEG C, far below ZnO sintering densifications temperature (950~1300 DEG C), is unfavorable for block material
The compact structure of material.
So far, the fine and close C and Ni codope ZnO block thermoelectric materials of preparation structure are not under 950~1300 DEG C of high temperature
Appear in the newspapers.
The content of the invention
The present invention provides a kind of preparation method of C and Ni codopes ZnO block thermoelectric materials and combines electric discharge using hydro-thermal method
Plasma agglomeration method, preparation structure densification, C and Ni codope ZnO of the relative density more than 95% under 950~1300 DEG C of high temperature
Block thermoelectric material.The energy gap of prepared C and Ni codope ZnO block thermoelectric materials of the invention is 2.0~2.7eV, brilliant
Particle size is 1~10 μm, and power factor is 4 × 10-4~8 × 10-4Wm-1K-2。
The present invention is achieved by the following technical solutions：
A kind of preparation method of C and Ni codopes ZnO thermoelectric materials, the preparation method is using zinc chloride and nickel nitrate as original
Material, the mole of the zinc chloride and nickel nitrate is according to chemical general formula Zn1-xNixO is configured, wherein, 0.005≤x≤
0.6mol, and C sources are added, using hydro-thermal method combination discharge plasma sintering method, C and Ni of the relative density more than 95% is made and is total to
Adulterate ZnO block thermoelectric materials.
Further, the preparation method specifically includes following steps：
(1) hydro-thermal reaction：Using mass fraction be all higher than 99% zinc chloride and nickel nitrate as raw material, the zinc chloride and nitre
The mole of sour nickel is according to chemical general formula Zn1-xNixO is configured, wherein, 0.005≤x≤0.6mol, using deionized water to be molten
Agent, configuration solubility is 0.1~1mol/L solution, and adds C sources progress hydro-thermal reaction, obtains mixed solution；
(2) preparation of Precursor Powder：The mixed solution that step (1) is obtained is filtered, and obtains filter residue, the mistake
Centrifuge washing is not carried out to the obtained filter residue during filter, before being made after then the filter residue is dried at 50~60 DEG C
Drive powder；
(3) discharge plasma sintering：Using discharge plasma sintering method, the front axle shell that step (2) is prepared
End carries out discharge plasma sintering, prepares C and Ni codope ZnO block thermoelectric materials.
Further, the concentration is added water heating kettle by the hydrothermal reaction process for 0.1~1mol/L solution first
In, it is subsequently added C sources, and the pH value using the C sources to adjust solution in water heating kettle treats water heating kettle temperature liter to 7.0~9.0
After up to 120~200 DEG C, 2~20h is incubated, mixed solution is obtained.
Further, PH conditioning agent C sources described in step (1) are diethanol monoisopropanolamine, dimethylethanolamine and three
Any one in isopropanolamine.
Further, the condition of step (3) described discharge plasma sintering is：950~1300 DEG C of temperature, pressure 50~
100MPa, 5~10min of sintering time, 1~15V of voltage, 10~500A of electric current.
A kind of C and Ni codopes ZnO thermoelectric materials, according to a kind of preparation side of C and Ni codopes ZnO thermoelectric materials
Method is prepared to be obtained, C the and Ni codopes ZnO thermoelectric materials relative density is more than 95%, and C the and Ni codopes ZnO
The energy gap of block thermoelectric material is 2.0~2.7eV, and crystallite dimension is 1~10 μm, and power factor is 4 × 10-4~8 × 10-4Wm-1K-2。
The advantageous effects of the present invention：
C the and Ni codope ZnO blocks heat that the present invention is prepared by hydro-thermal method and with reference to discharge plasma sintering method
Electric material has three clear advantages：One be by strictly controlling hydrothermal reaction condition and discharge plasma sintering condition,
The obtained C and Ni codope ZnO thermoelectric materials for making preparation are block, and its relative density is more than 95%；Two be electric discharge etc.
Although up to 900~1300 DEG C of ion sintering process temperature, present invention selection diethanol monoisopropanolamine, dimethyl ethanol
Any one in amine and triisopropanolamine is as C sources, and the selection of C sources and plasma discharging Fast Sintering technology overcomes often
High sintering temperature is unfavorable for C doping ZnO limitation in rule technology；Three be that C and Ni codope ZnO materials prepared by the present invention are
Block, and replace ZnO B positions O during C and Ni doping respectively2-With A Zn2+, therefore the A positions Zn to ZnO can be reached2+Carry out
High solid solubility Ni2+In the case of substitution, while completing to B O2-Carry out C4-The substitution of high solid solubility, realize ZnO A positions and
B high solid solubility substitutions simultaneously, further increase the carrier concentration and electrical conductivity of block, so as to improve ZnO material
Thermoelectricity capability.
Prepared by the present inventionC and Ni codope ZnO block thermoelectric materials have good performance, and its energy gap is 2.0
~2.7eV, crystallite dimension is 1~10 μm, and power factor is 4 × 10-4~8 × 10-4Wm-1K-2。
Brief description of the drawings
Fig. 1：The X-ray diffractogram for the C and Ni codope ZnO blocks that embodiment 9 is obtained, X-ray diffractogram shows, C and
Ni codope ZnO blocks are shown and pure ZnO standard cards (PD#36-1451) identical X-ray diffractogram, and are not detected by containing C
Or Ni the second phase；
Fig. 2：The field emission scanning electron microscope figure for the C and Ni codope ZnO blocks that embodiment 9 is obtained, field emission scanning electron microscope
Chart is bright, C and Ni codope ZnO block structures are fine and close；
Fig. 3：The UV-Visible absorption figure for the C and Ni codope ZnO blocks that embodiment 9 is obtained, ultraviolet-visible light is inhaled
Receive chart bright, C and Ni codope ZnO blocks are to have stronger absorption in the range of 400~800nm in wavelength；
Fig. 4：The energy gap for the C and Ni codope ZnO blocks that embodiment 9 is obtained, energy gap chart is bright, and C and Ni are common
It is about 2.3eV that the ZnO blocks that adulterate, which obtain smaller energy gap,；
Fig. 5：Embodiment 9 obtain C and Ni codope ZnO blocks Raman collection of illustrative plates, generally, for undoped with or Ni
Single doping ZnO blocks are in the wave-length coverage, almost without absorption.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiied
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also understand the present invention completely.
A kind of preparation method of C and Ni codopes ZnO thermoelectric materials, the preparation method specifically includes following steps：
(1) hydro-thermal reaction：It is more than 99% zinc chloride (ZnCl with mass fraction2·2H2O) and mass fraction be more than 99%
Nickel nitrate (Ni (NO3)2·2H2O it is) raw material, the mole of the zinc chloride and nickel nitrate is according to chemical general formula Zn1-xNixO
Configured, wherein, 0.005≤x≤0.6mol, using deionized water as solvent, the solution that configuration solubility is 0.1~1mol/L,
Add C sources and carry out hydro-thermal reaction, obtain mixed solution；
The C sources are diethanol monoisopropanolamine (C7H17NO3), dimethylethanolamine (C4H11) and triisopropanolamine NO
(C9H21NO3) in any one；
The hydrothermal reaction process first adds the concentration in water heating kettle for 0.1~1mol/L solution, then adds
Enter C sources, and the pH value using the C sources to adjust solution in water heating kettle is to 7.0~9.0, treat water heating kettle temperature be increased to 120~
After 200 DEG C, 2~20h is incubated, mixed solution is obtained.
(2) preparation of Precursor Powder：The mixed solution that step (1) is obtained is filtered, and obtains filter residue, the mistake
Centrifuge washing is not carried out to obtained filter residue during filter, front axle shell is made after then the filter residue is dried at 50~60 DEG C
End；
(3) discharge plasma sintering：Using conventional discharge plasma sintering method, by step (2) prepare it is described
Precursor Powder carries out discharge plasma sintering, prepares C and Ni codope ZnO block thermoelectric materials；The plasma discharging
The condition of sintering is：950~1300 DEG C of temperature, 50~100MPa of pressure, 5~10min of sintering time, 1~15V of voltage, electric current
10~500A.
In order to prepare C doping ZnO materials, the B positions substitution of ZnO thermoelectric materials is realized, the present invention is tested by substantial amounts of
Demonstrate,prove diethanol monoisopropanolamine (C7H17NO3), dimethylethanolamine (C4H11) and triisopropanolamine (C NO9H21NO3) be three kinds can
Capable C sources, overcome the phenomenon that sintering temperature high in routine techniques is unfavorable for C doping ZnO；Secondly, as shown in figure 1, this hair
The X-ray diffractogram of bright C and Ni codopes ZnO blocks is shown：C and Ni codope ZnO blocks and be not detected by containing C second
Phase；Finally, the present invention is prepared by strictly controlling the condition of hydro-thermal reaction and the reaction condition of discharge plasma sintering process
Obtained C and Ni codope ZnO thermoelectric materials are block, and block materials stability is good, assemble the advantage such as convenient, and it is in thermoelectricity material
The application aspect of material has more advantage compared with film-like material and dusty material.
A kind of C and Ni codopes ZnO thermoelectric materials, Fig. 1-5 is represents the figure of its feature, according to above-mentioned C and Ni codopes
The preparation method of ZnO thermoelectric materials is prepared to be obtained, as shown in Fig. 2 C and Ni codope ZnO block structures are very fine and close；It is described
C and Ni codope ZnO thermoelectric materials relative density is more than 95%, and the forbidden band of the C and Ni codopes ZnO block thermoelectric materials
Width is 2.0~2.7eV, and crystallite dimension is 1~10 μm, and power factor is 4 × 10-4~8 × 10-4Wm-1K-2。
Several embodiments of the C and Ni codopes ZnO thermoelectric materials of the present invention of table 1
Note：All embodiments in table：Discharge plasma sintering step in C and Ni codope ZnO thermoelectric material preparation methods
Rapid voltage 1~15V, 10~500A of electric current.
And the feature of the C and Ni codope ZnO blocks obtained to embodiment 9 in table 1 is analyzed, Fig. 1-5 difference
It is X-ray diffractogram, field emission scanning electron microscope figure, the ultraviolet-visible light for C the and Ni codope ZnO blocks that embodiment 9 is obtained
Absorb figure, energy gap and Raman collection of illustrative plates.
Claims (4)
1. a kind of preparation method of C and Ni codopes ZnO thermoelectric materials, it is characterised in that the preparation method with zinc chloride and
Nickel nitrate is raw material, and the mole of the zinc chloride and nickel nitrate is according to chemical general formula Zn1-xNixO is configured, wherein,
0.005≤x≤0.6mol, and C sources are added, using hydro-thermal method combination discharge plasma sintering method, obtained relative density is more than
95% C and Ni codope ZnO block thermoelectric materials；
The preparation method specifically includes following steps：
(1) hydro-thermal reaction：Using mass fraction be all higher than 99% zinc chloride and nickel nitrate as raw material, the zinc chloride and nickel nitrate
Mole according to chemical general formula Zn1-xNixO is configured, wherein, 0.005≤x≤0.6mol, using deionized water as solvent,
Configuration concentration is 0.1~1mol/L solution, and adds C sources progress hydro-thermal reaction, obtains mixed solution, C sources are diethanol list
Any one in isopropanolamine, dimethylethanolamine and triisopropanolamine；
(2) preparation of Precursor Powder：The mixed solution that step (1) is obtained is filtered, and obtains filter residue, the filtering
During centrifuge washing is not carried out to the obtained filter residue, front axle shell is made after then the filter residue is dried at 50~60 DEG C
End；
(3) discharge plasma sintering：Using discharge plasma sintering method, the Precursor Powder that step (2) is prepared enters
Row discharge plasma sintering, prepares C and Ni codope ZnO block thermoelectric materials.
2. a kind of preparation method of C and Ni codopes ZnO thermoelectric materials according to claim 1, it is characterised in that the water
Thermal process reactor first adds the concentration in water heating kettle for 0.1~1mol/L solution, is subsequently added C sources, and utilize institute
The pH value that C sources are stated to adjust solution in water heating kettle after water heating kettle temperature is increased to 120~200 DEG C, is incubated 2 to 7.0~9.0
~20h, obtains mixed solution.
3. a kind of preparation method of C and Ni codopes ZnO thermoelectric materials according to claim 1, it is characterised in that step
(3) condition of the discharge plasma sintering is：950~1300 DEG C of temperature, 50~100MPa of pressure, sintering time 5~
10min, 1~15V of voltage, 10~500A of electric current.
4. a kind of C and Ni codopes ZnO thermoelectric materials, according to a kind of one of claim 1-3 C and Ni codopes ZnO heat
The preparation method of electric material is prepared to be obtained, it is characterised in that C the and Ni codopes ZnO thermoelectric material relative densities are more than
95%, and the energy gap of the C and Ni codopes ZnO block thermoelectric materials is 2.0~2.7eV, crystallite dimension is 1~10 μ
M, power factor is 4 × 10-4~8 × 10-4Wm-1K-2。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496733A (en) * | 2013-09-30 | 2014-01-08 | 陕西科技大学 | Method for preparing carbon doped zinc oxide |
| CN103626220A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing carbon-doped zinc oxide microsphere with multilevel structure |
| CN103715349A (en) * | 2013-12-30 | 2014-04-09 | 北京科技大学 | Manufacturing method for Ni-doped ZnO texture thermoelectric material |
-
2015
- 2015-10-13 CN CN201510671114.3A patent/CN105272206B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496733A (en) * | 2013-09-30 | 2014-01-08 | 陕西科技大学 | Method for preparing carbon doped zinc oxide |
| CN103626220A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing carbon-doped zinc oxide microsphere with multilevel structure |
| CN103715349A (en) * | 2013-12-30 | 2014-04-09 | 北京科技大学 | Manufacturing method for Ni-doped ZnO texture thermoelectric material |
Non-Patent Citations (1)
| Title |
|---|
| 碳掺杂ZnO的制备及光电性能;张凌云等;《东北师大学报（自然科学版）》;20120331;第44卷(第1期);摘要 * |
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