CN109956749A - A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material - Google Patents
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material Download PDFInfo
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- CN109956749A CN109956749A CN201910311214.3A CN201910311214A CN109956749A CN 109956749 A CN109956749 A CN 109956749A CN 201910311214 A CN201910311214 A CN 201910311214A CN 109956749 A CN109956749 A CN 109956749A
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The step of present invention provides a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, belongs to ceramic of compact preparation technical field, this method includes: (1) solution for preparing to be capable of oligodynamical cuprous sulfide powder as precursor solution.(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then the two is uniformly mixed with milling bar, obtains mixture；(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, heating sintering is then carried out under the pressure of 300 ~ 400Mpa.The sintering method is compared with the conventional sinterings method such as discharge plasma sintering, hot pressed sintering, have many advantages, such as energy loss it is low, it is highly-safe, be suitable for industrialized production, and it is high using cuprous sulfide thermoelectric ceramics consistency prepared by method of the invention, thermoelectricity capability is excellent.
Description
Technical field
The invention belongs to ceramic of compact preparation technical fields, more specifically to a kind of cuprous sulfide heat of copper missing
The sintered at ultra low temperature method of electric material.
Background technique
Ceramic material is with the excellent properties of its high temperature resistant, wear-resistant, electricity, mechanics, heat transfer etc., in every field
All have a wide range of applications.Determine that a whether excellent important factor of ceramic performance is that sintering process.Currently used for
The sintering method of cuprous sulfide is mainly hot pressed sintering, discharge plasma sintering.Both sintering methods require 500 DEG C with
Upper progress, this not only needs to consume more energy, but also all produces limitation for many researchs.For example, ceramic-polymer
Composite material.Ceramic-polymer Composite has a variety of design spaces, can improve material property and realize multifunctional equipment.
However, the process window to differ widely between polymer and ceramics limits the full scope of required performance.If can significantly drop
The temperature of low frit, then of this sort problem can be resolved.Sintered at ultra low temperature of the present invention can be in room
Temperature is highly beneficial for the research of cuprous sulfide composite function ceramics to being densified at 150 DEG C to powder, will greatly reduce
As different materials process window difference and caused by limit.
Summary of the invention
The object of the present invention is to provide a kind of sintered at ultra low temperature methods of cuprous sulfide thermoelectric material.With conventional compacting
Cuprous sulfide powder is similar, uniaxial machinery power drive densification, but liquid phase is added in the cuprous sulfide powder of copper missing in we
Afterwards, facilitate to enhance the lubricity between particle, there is also pressure drives on the local scale of the sharp small face contact of particle
The enhancing of dynamic solubility, this is conducive to the larger surface area of the filling in gap and particle sliding between powder granule.Continuing
High pressure under press certain temperature so that hydrothermal solution reaction-filling intergranular pore, powder grain occur for the liquid phase for having dissolved powder
Also continued propagation, final realize densify at such a temperature.
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) solution for preparing to be capable of oligodynamical cuprous sulfide powder is as precursor solution.It is mentioned herein micro in ability
Domain belongs to common sense；
(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then with milling bar by two
Person is uniformly mixed, and obtains mixture；
(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, so
Heating sintering is carried out under the pressure of 300 ~ 400Mpa afterwards.The mold that High Voltage is able to bear in reality can be used in this.
It is powder and mill under sintering process high temperature in order to prevent since mold common in existing other sintering methods is graphite jig
Tool reaction, but just without considering this problem in the low-temperature sintering of the application.
In the step (1), precursor solution is deionized water.
In the step (2), cuprous sulfide powder is nanometer grade powder, the nanometer grade powder and precursor solution
Mass ratio is 5:1.
In the step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is 10 ~ 30mm, a height of
The chromium cylindrical steel mold of 60 ~ 80mm.
In the step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating speed of 5 ~ 20 DEG C/min
Rate is directly raised to sintering temperature, and soaking time is 1 ~ 2 hour hour, later furnace cooling, unloading pressure after being cooled to room temperature.
Further, heating is specifically referred to from room temperature to sintering temperature in the step (3), and the sintering temperature is 150
℃。
Compared with the sintering technology of the cuprous sulfide of existing copper missing, the beneficial effects of the present invention are:
(1) due to the sintering temperature being greatly lowered, the energy consumption in sintering process is effectively reduced.
(2) sintered at ultra low temperature cuprous sulfide, it is possible to prevente effectively from due to not jljl in the research of copper sulphur compound composite ceramics
It is limited caused by matter process window is different.
Detailed description of the invention
Fig. 1 is the XRD spectrum for the cuprous sulfide thermoelectric ceramics being sintered using sintering method of the invention.
Fig. 2 is the SEM image for the cuprous sulfide thermoelectric ceramics being sintered using sintering method of the invention.
Fig. 3 is that the conductivity for the cuprous sulfide thermoelectric ceramics being sintered using sintering method of the invention varies with temperature curve
Figure；
Fig. 4 varies with temperature curve using the Seebeck coefficient of the cuprous sulfide thermoelectric ceramics of the sintering method sintering of the invention
Figure；
The power factor for the cuprous sulfide thermoelectric ceramics that Fig. 5 is sintered using sintering method of the invention varies with temperature curve graph.
The thermal conductivity for the cuprous sulfide thermoelectric ceramics that Fig. 6 is sintered using sintering method of the invention varies with temperature curve
Figure.
The thermoelectric figure of merit ZT for the cuprous sulfide thermoelectric ceramics that Fig. 7 is sintered using sintering method of the invention varies with temperature song
Line chart.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
Technical solution of the present invention is clearly and completely described in the embodiment of the present invention.Cuprous sulfide as described herein refers to
Cu2S、Cu1.9S and Cu1.8These three compounds of S.
Embodiment 1
(1) Cu of electronic balance weighing 1g is used2S powder is put into Yan Portland, then using liquid-transfering gun measure 200 μ L deionized waters with
Powder mixing；
(2) after completing step (1), milling bar milled mixtures repeatedly are used, it is ensured that powder is uniformly mixed with solution.
(3) after completing step (2), mixed uniformly ceramics precursor powder is put into chromium steel mold, then mold is placed
Under press machine；First press pressure precompressed 10 minutes of 400Mpa at room temperature, then under conditions of keeping pressure constant with
Temperature is risen to 150 DEG C by the heating rate of 10 DEG C/min；Finally (400Mpa, 150 DEG C) is sintered under conditions of the constant temperature and pressure
90 minutes；Keep pressure constant after the completion of sintering, unloading pressure after furnace cooling obtains Cu2S ceramics.
Embodiment 2
(1) Cu of electronic balance weighing 1g is used1.9S powder is put into Yan Portland, then measures 200 μ L deionized waters using liquid-transfering gun
It is mixed with powder.
(2) after completing step (1), milling bar milled mixtures repeatedly are used, it is ensured that powder is uniformly mixed with solution.
(3) after completing step (2), mixed uniformly ceramics precursor powder is put into chromium steel mold, then mold is placed
Under press machine；First press pressure precompressed 10 minutes of 400Mpa at room temperature, then under conditions of keeping pressure constant with
Temperature is risen to 150 DEG C by the heating rate of 10 DEG C/min；Finally (400Mpa, 150 DEG C) is sintered under conditions of the constant temperature and pressure
90 minutes；Keep pressure constant after the completion of sintering, unloading pressure after furnace cooling obtains Cu1.9S ceramics.
Embodiment 3
(1) Cu of electronic balance weighing 1g is used1.8S powder is put into Yan Portland, then measures 200 μ L deionized waters using liquid-transfering gun
It is mixed with powder.
(2) after completing step (1), milling bar milled mixtures repeatedly are used, it is ensured that powder is uniformly mixed with solution.
(3) after completing step (2), mixed uniformly ceramics precursor powder is put into chromium steel mold, then mold is placed
Under press machine；First press pressure precompressed 10 minutes of 400Mpa at room temperature, then under conditions of keeping pressure constant with
Temperature is risen to 150 DEG C by the heating rate of 10 DEG C/min；Finally (400Mpa, 150 DEG C) is sintered under conditions of the constant temperature and pressure
90 minutes；Keep pressure constant after the completion of sintering, unloading pressure after furnace cooling obtains Cu1.8S ceramics.
In order to further detect the performance for the cuprous sulfide thermoelectric ceramics that the embodiment of the present invention 1~3 is sintered, we are carried out
Dependence test and analysis, particular content are as follows:
Include to be made of multiphase by the resulting sample of sintering known to the XRD spectrum of Fig. 1, mainly includes monocline Cu2S phase (PDF#
83-1462) and four directions Cu1.96S(PDF#29-0578).It is burnt from the SEM image of Fig. 2 it will be seen that being cold-pressed using low temperature
Knot technique is sintered powder at 150 DEG C, is successfully realized the densification to sample, three groups of sample surfaces all holes are deposited
The crystallite dimension difference of each group sample is little under identical amplification factor.To the ceramics sample of three kinds of different powder sinterings
Carry out thermoelectricity capability test.Fig. 3 is conductivity variation with temperature curve, and the conductivity of sample has as the temperature rises first to be subtracted
It is small to increase the last variation reduced again again.Fig. 4 is that Seebeck coefficient varies with temperature curve, is gradually increased as the temperature rises
Greatly.Fig. 5 is that power factor varies with temperature curve, and the power factor of all samples is all to be gradually increased as the temperature rises,
Cu1.8The power factor of S sample reaches 13.9 μ W/cmK of maximum value in 823K2.Fig. 6 is that thermal conductivity varies with temperature curve
Scheme, there is four directions Cu in all samples1.96S phase, Cu1.96There are Cu ionic vacancies, and its carrier concentration is increased for S phase, from
And its carrier thermal conductivity is increased, Cu2S reaches the smallest thermal conductivity 0.60Wm in 673K-1·K.Fig. 7 is that thermoelectricity is excellent
Value ZT variation with temperature curve, the ZT value of all samples are all to be gradually increased as the temperature rises.It, can be in cold stage
Find out sample Cu1.8The thermoelectricity capability of S is more preferable compared to other samples, has arrived sample Cu after high temperature1.9The thermoelectric figure of merit of S by
Gradually surmount other samples.In all samples, Cu1.8The power factor of S sample reaches 13.9 μ W/cm of maximum value in 823K
K2, but due to its relatively high thermal conductivity, when ZT value 823K, has only reached 0.81.And Cu1.9S sample, the ZT value in 823K
Reach maximum value 1.27.By being analyzed above it is found that cuprous sulfide ceramics sample prepared by sintering method of the invention has
Excellent thermoelectricity capability can be used as thermoelectric material application.
In conclusion the beneficial effects of the present invention are:
(1) sintering temperature obtains the reduction (in the densification that 150 DEG C can complete to powder) of high degree, for production process
The saving of the middle energy has very great meaning.
(2) sintered at ultra low temperature cuprous sulfide, it is possible to prevente effectively from due to not jljl in the research of copper sulphur compound composite ceramics
It is limited caused by matter process window is different.
Embodiment 4
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) preparing being capable of oligodynamical Cu2S、Cu1.9S and Cu1.8The solution of these three compound powders of S is as precursor solution.
It is mentioned herein micro to belong to common sense in this field；
(2) the three kinds of powder referred in step (1) and precursor solution obtained in step (1) are all put into Yan Portland, then
The two is uniformly mixed with milling bar, obtains mixture；
(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, so
Heating sintering is carried out under the pressure of 300 ~ 400Mpa afterwards.The mold that High Voltage is able to bear in reality can be used in this.
It is powder and mill under sintering process high temperature in order to prevent since mold common in existing other sintering methods is graphite jig
Tool reaction, but just without considering this problem in the low-temperature sintering of the application.
In the step (1), precursor solution is deionized water.
In the step (2), Cu2S、Cu1.9S and Cu1.8These three powder of S are nanometer grade powder, the nanoscale powder
The mass ratio of body and precursor solution is 5:1.
In the step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is 10 ~ 30mm, a height of
The chromium cylindrical steel mold of 60 ~ 80mm.
In the step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating speed of 5 ~ 20 DEG C/min
Rate is directly raised to sintering temperature, and soaking time is 1 ~ 2 hour hour, later furnace cooling, unloading pressure after being cooled to room temperature.
Further, heating is specifically referred to from room temperature to sintering temperature in the step (3), and the sintering temperature is 150
℃。
Embodiment 5
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) solution for preparing to be capable of oligodynamical cuprous sulfide powder is as precursor solution.It is mentioned herein micro in ability
Domain belongs to common sense；
(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then with milling bar by two
Person is uniformly mixed, and obtains mixture；
(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, so
Heating sintering is carried out under the pressure of 300 ~ 400Mpa afterwards.The mold that High Voltage is able to bear in reality can be used in this.
It is powder and mill under sintering process high temperature in order to prevent since mold common in existing other sintering methods is graphite jig
Tool reaction, but just without considering this problem in the low-temperature sintering of the application.
In the step (1), precursor solution is deionized water.
In the step (2), cuprous sulfide powder is nanometer grade powder, the nanometer grade powder and precursor solution
Mass ratio is 5:1.
In the step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is 10 ~ 30mm, a height of 60
The chromium cylindrical steel mold of ~ 80mm.
In the step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating speed of 5 ~ 20 DEG C/min
Rate is directly raised to sintering temperature, and soaking time is 1 ~ 2 hour hour, later furnace cooling, unloading pressure after being cooled to room temperature.
Further, heating specifically refers to be sintered at room temperature in the step (3).
Embodiment 6
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) solution for preparing to be capable of oligodynamical cuprous sulfide powder is as precursor solution.It is mentioned herein micro in ability
Domain belongs to common sense.
(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then use milling bar
The two is uniformly mixed, mixture is obtained；
(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, so
Heating sintering is carried out under the pressure of 300 ~ 400Mpa afterwards.The mold that High Voltage is able to bear in reality can be used in this.
It is powder and mill under sintering process high temperature in order to prevent since mold common in existing other sintering methods is graphite jig
Tool reaction, but just without considering this problem in the low-temperature sintering of the application.
In the step (1), precursor solution is deionized water.
In the step (2), cuprous sulfide powder is nanometer grade powder, the matter of the nanometer grade powder and precursor solution
Measuring ratio is 5:1.
In the step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is 10 ~ 30mm, a height of 60
The chromium cylindrical steel mold of ~ 80mm.
In the step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating speed of 5 ~ 20 DEG C/min
Rate is directly raised to sintering temperature, and soaking time is 1 ~ 2 hour hour, later furnace cooling, unloading pressure after being cooled to room temperature.
Further, heating is specifically referred to from room temperature to sintering temperature in the step (3), and the sintering temperature is 150
℃。
Embodiment 7
A kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) solution for preparing to be capable of oligodynamical cuprous sulfide powder is as precursor solution.It is mentioned herein micro in ability
Domain belongs to common sense；
(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then with milling bar by two
Person is uniformly mixed, and obtains mixture；
(3) mixture that step (2) obtains is fitted into mold, then in 350Mpa, at room temperature precompressed 12min, is then existed
Heating sintering is carried out under the pressure of 350Mpa.The mold that High Voltage is able to bear in reality can be used in this.Due to existing
Common mold is graphite jig in other sintering methods, is that powder is reacted with grinding tool under sintering process high temperature in order to prevent,
But just without considering this problem in the low-temperature sintering of the application.
In the step (1), precursor solution is deionized water.
In the step (2), cuprous sulfide powder is nanometer grade powder, the nanometer grade powder and precursor solution
Mass ratio is 5:1.
In the step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is 20mm, a height of 70mm
Chromium cylindrical steel mold.
In the step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating rate of 10 DEG C/min
It is directly raised to sintering temperature, soaking time is 1.5 hour hour, later furnace cooling, unloading pressure after being cooled to room temperature.
Further, heating is specifically referred to from room temperature to sintering temperature in the step (3), and the sintering temperature is 150
℃。
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (8)
1. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material, it is characterised in that: the step of this method includes:
(1) solution for preparing to be capable of oligodynamical cuprous sulfide powder is as precursor solution；
(2) cuprous sulfide powder and precursor solution obtained in step (1) are all put into Yan Portland, then with milling bar by two
Person is uniformly mixed, and obtains mixture；
(3) mixture that step (2) obtains is fitted into mold, then in 300 ~ 400Mpa, at room temperature 10 ~ 15min of precompressed, so
Heating sintering is carried out under the pressure of 300 ~ 400Mpa afterwards.
2. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
The step of (1) in, precursor solution is deionized water.
3. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
In step (2), cuprous sulfide powder is nanometer grade powder, and the mass ratio of the nanometer grade powder and precursor solution is 5:1.
4. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
In step (3), the mold is chromium steel mold, and the diameter that the chromium steel mold is is the cylinder of 10 ~ 30mm, a height of 60 ~ 80mm
Shape chromium steel mold.
5. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
Heating is specifically referred to from room temperature to sintering temperature in step (3), and the sintering temperature is 150 DEG C.
6. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
Heating specifically refers to start to be sintered at room temperature in step (3).
7. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
Heating is specifically referred to from room temperature to sintering temperature in step (3), and the sintering temperature is less than 150 DEG C.
8. a kind of sintered at ultra low temperature method of cuprous sulfide thermoelectric material according to claim 1, it is characterised in that: described
In step (3), the temperature program(me) that is sintered specifically: with heating rate: the heating rate of 5 ~ 20 DEG C/min is directly raised to burning
Junction temperature, soaking time are 1 ~ 2 hour, furnace cooling later, unloading pressure after being cooled to room temperature.
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| CN110627502A (en) * | 2019-10-22 | 2019-12-31 | 中南大学 | Low-temperature p-type composite thermoelectric material and preparation method thereof |
| CN111269014A (en) * | 2020-01-20 | 2020-06-12 | 昆明理工大学 | Cu-S-based composite thermoelectric material and preparation method thereof |
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| CN110444656B (en) * | 2019-08-20 | 2022-10-04 | 上海第二工业大学 | Preparation method of cuprous sulfide composite silicon carbide block thermoelectric material |
| CN110627502A (en) * | 2019-10-22 | 2019-12-31 | 中南大学 | Low-temperature p-type composite thermoelectric material and preparation method thereof |
| CN111269014A (en) * | 2020-01-20 | 2020-06-12 | 昆明理工大学 | Cu-S-based composite thermoelectric material and preparation method thereof |
| CN111269014B (en) * | 2020-01-20 | 2021-06-08 | 昆明理工大学 | Cu-S-based composite thermoelectric material and preparation method thereof |
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