CN105826459B - A kind of and Cu2The electrode and its Joining Technology that Se base thermoelectricity materials match - Google Patents
A kind of and Cu2The electrode and its Joining Technology that Se base thermoelectricity materials match Download PDFInfo
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Abstract
The present invention relates to a kind of and Cu2The electrode and its Joining Technology that Se base thermoelectricity materials match.The electrode is the mixture of Ni-Al alloys and metal simple-substance Al, and wherein the mass percentage of metal simple-substance Al is 40%-60%, and surplus is Ni-Al alloys.The electrode and Cu2The Joining Technology of Se base thermoelectricity materials is connected by discharge plasma sintering, is wherein provided with gradient transitional lay between electrode and thermoelectric material.Electrode and Cu of the present invention2Se base thermoelectricity material interface cohesions are very stable, and engagement surface resistance transition is very small, and preparation process is simple, and cost is also relatively low.
Description
Technical field
The present invention relates to a kind of and Cu2The electrode and its Joining Technology that Se base thermoelectricity materials match belong to thermoelectricity member device
The electrode of part selects and preparing technical field.
Background technology
Thermoelectric material is a kind of functional material that can be realized thermal energy and electric energy and mutually convert, it utilizes itself
Thermal energy can be converted into electric energy by Seebeck effects, and Peltier effects can convert electrical energy into thermal energy.By thermoelectric material
Have when the thermoelectric power generating component work of preparation without mechanical moving element, long lifespan, reliability are high, environmentally safe etc.
Advantage has prodigious application potential in fields such as aviation field, industrial exhaust heat, vehicle exhaust, underground heat.As global energy is endangered
Machine increasingly sharpens, and the research for being related to thermoelectric material and thermo-electric device receives the attention of various countries' scientific research.Currently, bismuth telluride
The thermoelectric material Element Technology of equal low temperature thermo-electric generation has been widely used in commodity production, and the thermoelectric material of high temperature is such as
The thermoelectricity component of the preparations such as PbTe, SiGe has started to be applied to space field.
Cu2Se compounds are a kind of p-type thermoelectric materials suitable for high temperature field, since the class I liquid I behavior of Cu generates
Shear wave damping effect make it with intrinsic lower thermal conductivity, in 1000K, its ZT is up to 1.8, in high temperature thermoelectric power generation
Field has huge application prospect, but its component technology is still far from perfect at present.The selection of wherein electrode material is first
The problem that must first face.Cu is mostly used greatly for low-temperature thermoelectric material as electrode material, but for high temperature thermoelectric material
Due to the use of the raising of temperature, selection and joint technology to electrode material suffer from higher requirement.
Cu2The electrode material of Se thermoelectric materials requires following characteristic：In use temperature range and Cu2Se compounds
Without serious phase counterdiffusion or chemical reaction, to ensure that thermoelectric material self performance is unaffected；With Cu2Se compounds are without electricity
Chemical reaction is (this is because Cu when high temperature2There are certain Cu for Se compounds+Conductance), to ensure thermoelectric material self performance
Stability between unaffected and thermoelectric material and electrode interface；With high conductivity and thermal conductivity utmostly will
The temperature difference passes to thermoelectric material；Coefficient of thermal expansion is wanted and Cu2Se compounds match to prevent thermal stress from leading to micro-crack；In addition
Also there is certain inoxidizability in use temperature range.
The country is for Cu at present2The electrode material and preparation process of Se base thermoelectricity materials do not have report also, and the bright Buddhist nun in the U.S.
Soviet Union reaches mines and manufacturing industry company, and the units such as General Electric Company study Cu in the seventies and eighties in last century2Se base thermoelectricity
It is used as electrode material, the combined process of electrode and thermoelectric material to use thermocompression bonding etc. using Mo-Re, W-Re alloy when power generating device
Mode.Mo-Re, W-Re alloy are expensive raw material price, material workability difference etc. as the shortcomings that electrode material.In addition to this,
External related Cu2The electrode material and preparation process of Se base thermoelectricity materials are showed no report.
Invention content
The technical problem to be solved by the present invention is to provide a kind of and Cu in view of the deficiency of the prior art2Se
The electrode and its Joining Technology that base thermoelectricity material matches, bond strength is high, thermal stability is good, interface electrical property transition is good and
Preparation process is simple.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
A kind of and Cu2The electrode that Se base thermoelectricity materials match, the electrode are the mixed of Ni-Al alloys and metal simple-substance Al
Object is closed, the wherein mass percentage of metal simple-substance Al is 40%-60%, and surplus is Ni-Al alloys.
By said program, the mass percentage of Ni is 48% in the Ni-Al alloys, remaining is Al.
By said program, the thickness of the electrode is 0.5-3mm.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials is connected by discharge plasma sintering,
Gradient transitional lay is wherein provided between electrode and thermoelectric material, wherein gradient transitional lay is Cu2Se base thermoelectricity materials and electrode
According to volume ratio 1:1 mixes.
By said program, the thickness of the gradient transitional lay is 0.1-0.3mm.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials, specific process step are：
(1) according to the ratio that the mass percent of metal simple-substance Al powder is 40%-60%, surplus is Ni-Al alloyed powders, claim
Metal simple-substance Al powder and Ni-Al alloyed powders are taken, is uniformly mixed and obtains electrode layer powder；
(2) according to Cu2The volume ratio 1 of electrode material powder obtained by Se powders, step (1):1, weigh Cu2Se base thermoelectricity
Material powder, electrode material powder are uniformly mixed and obtain gradient transitional lay powder；
(3) according to electrode layer powder, gradient transitional lay powder, Cu2Se base thermoelectricity materials powder, gradient transitional lay powder,
The sequence of electrode layer powder, by Cu2Gradient transitional lay powder obtained by Se base thermoelectricity materials powder, step 2) and electrode layer powder paving
It is sintered in graphite jig, obtains electrode and Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize
Cu2The connection of Se base thermoelectricity materials and the electrode.
By said program, by Cu in step 3)2Gradient transitional lay powder and electricity obtained by Se base thermoelectricity materials powder, step 2)
Pole layer powder is layed in graphite jig before sintering, further includes pressing step.Wherein, the precompressed is by Cu2Se base thermoelectricity materials
Feed powder body is uniformly layered in graphite jig, carries out precompressed；In Cu2Se base thermoelectricity material powder layer upper and lower ends are uniformly laid with
Gradient transitional lay powder carries out precompressed；It is uniformly spread respectively in step (1) on the gradient transitional lay powder of upper and lower side again
Electrode layer powder carries out precompressed.
Described to be sintered to discharge plasma sintering by said program, vacuum degree is 10pa-15pa, sintering pressure when sintering
For 30- 50MPa, sintering temperature is 470-550 DEG C.
By said program, the heating rate of the discharge plasma sintering is 60-80 DEG C/min.
By said program, the soaking time of the discharge plasma sintering is 3-5min.
Compared with prior art, the beneficial effects of the invention are as follows：
First, the present invention selects the combination electrode of Ni-Al alloys and metal simple-substance Al mixing, compares single Al electrodes, boundary
Micro-crack at face is less, to contact resistance smaller；
Second, gradient mistake is provided with when electrode of the present invention is connect with thermoelectric material, between electrode and thermoelectric material
Layer is crossed, the micro-crack of interface will be further reduced so that contact resistance further decreases；
Third, electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials is connected by discharge plasma sintering
It connects, once sintered realization is successfully connected, while realizing Cu2The densification of Se base thermoelectricity materials and good connection with electrode,
Joint surface interface resistance transition is very small, and combination interface is good, good reliability and technological operation simplicity.
Description of the drawings
Fig. 1 is electrode and Cu in embodiment 22The backscattered electron image of Se thermoelectric material linkage interfaces.
Fig. 2 is electrode corresponding with Fig. 1 and Cu2Se thermoelectric material linkage interface distribution of resistance situations of change, wherein horizontal
Coordinate is test position, and unit mm, ordinate is resistance, unit mohm.
Fig. 3 is electrode and Cu in control group 12The backscattered electron image of Se thermoelectric material linkage interfaces.
Fig. 4 is electrode corresponding with Fig. 3 and Cu2Se thermoelectric material linkage interface distribution of resistance situations of change, wherein horizontal
Coordinate is test position, and unit mm, ordinate is resistance, unit mohm.
Fig. 5 is Al electrodes and Cu in control group 22The backscattered electron image of Se thermoelectric material linkage interfaces.
Fig. 6 is Al electrodes corresponding with Fig. 5 and Cu2Se thermoelectric material linkage interface distribution of resistance situations of change, wherein
Abscissa is test position, and unit mm, ordinate is resistance, unit mohm.
Specific implementation mode
In order to better understand the present invention, carry out the content that the present invention is furture elucidated with reference to example, but the present invention
Content is not limited only to the following examples.
Cu used in the present invention2The group of Se base thermoelectricity materials becomes Cu2Se, for the Cu of other components2Se base thermoelectricity materials are made
The thermoelectric element of matrix, electrode of the present invention are equally applicable.
Cu employed in following embodiments2Se thermoelectric material powders can be reacted by self-propagating high-temperature to be synthesized, and can be joined
Examine Chinese patent application 2013100875206.
The mass percentage of Ni is 48% in Ni-Al alloys employed in following embodiments, remaining is Al.
Graphite jig internal diameter is 15mm in following embodiments.
Embodiment 1
A kind of and Cu2The electrode that Se base thermoelectricity materials match, the electrode are the mixed of Ni-Al alloys and metal simple-substance Al
Object is closed, the wherein mass percentage of metal simple-substance Al is 40%, and surplus is Ni-Al alloys.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials, specific process step are：
(1) according to the ratio that the mass percent of metal simple-substance Al powder is 40%, surplus is Ni-Al alloyed powders, gold is weighed
Belong to simple substance Al powder and Ni-Al alloyed powders, is uniformly mixed and obtains electrode layer powder；
(2) according to Cu2The volume ratio 1 of electrode material powder obtained by Se powders, step (1):1, weigh Cu2Se base thermoelectricity
Material powder, electrode material powder grind 30min and are uniformly mixed, obtain gradient transitional lay powder in the agate mortar；
(3) 2 parts of electrode layer powder in step (1), every part of 1g are weighed；Weigh 2 parts, every part of gradient transitional lay powder
0.20g；Weigh Cu2Se thermoelectric material powders 12.0g；
The Cu that will be weighed2Se powders are uniformly layered in graphite jig, carry out precompressed；Then in Cu2Se base thermoelectricity material powder
Body layer upper and lower ends are uniformly laid with gradient transitional lay material powder, and carry out precompressed；Again two above and below gradient transitional lay powder
End is uniform respectively to be laid with electrode layer powder, and carries out precompressed, and each layer is according to electrode layer powder, gradient mistake in gained graphite jig
Cross a layer powder, Cu2The sequence distribution of Se base thermoelectricity materials powder, gradient transitional lay powder, electrode layer powder；
Then discharge plasma sintering will be carried out in the graphite jig, vacuum degree 13pa, 70 DEG C/min of heating rate are burnt
Junction temperature is 540 DEG C, sintering pressure 30MPa, and soaking time finishes cooled to room temperature, obtain electrode in 3min, sintering
With Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize Cu2The connection of Se base thermoelectricity materials and the electrode.
The present embodiment the electrode obtained thickness 1.5-2mm, gradient transition layer thickness are about 0.2mm, and thermoelectric material layer thickness is about
For 10mm.
Embodiment 2
A kind of and Cu2The electrode that Se base thermoelectricity materials match, the electrode are the mixed of Ni-Al alloys and metal simple-substance Al
Object is closed, the wherein mass percentage of metal simple-substance Al is 40%, and surplus is Ni-Al alloys.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials, specific process step are：
(1) according to the ratio that the mass percent of metal simple-substance Al powder is 40%, surplus is Ni-Al alloyed powders, gold is weighed
Belong to simple substance Al powder and Ni-Al alloyed powders, is uniformly mixed and obtains electrode layer powder；
(2) according to Cu2The volume ratio 1 of electrode material powder obtained by Se powders, step (1):1, weigh Cu2Se base thermoelectricity
Material powder, electrode material powder grind 30min and are uniformly mixed, obtain gradient transitional lay powder in the agate mortar；
(3) 2 parts of electrode layer powder in step (1), every part of 0.5g are weighed；Weigh 2 parts, every part of gradient transitional lay powder
0.20g；Weigh Cu2Se thermoelectric material powders 12.0g；
The Cu that will be weighed2Se powders are uniformly layered in graphite jig, carry out precompressed；Then in Cu2Se base thermoelectricity material powder
Body layer upper and lower ends are uniformly laid with gradient transitional lay material powder, and carry out precompressed；Again two above and below gradient transitional lay powder
End is uniform respectively to be laid with electrode layer powder, and carries out precompressed, and each layer is according to electrode layer powder, gradient mistake in gained graphite jig
Cross a layer powder, Cu2The sequence distribution of Se base thermoelectricity materials powder, gradient transitional lay powder, electrode layer powder；
Then discharge plasma sintering will be carried out in the graphite jig, vacuum degree 12pa, 80 DEG C/min of heating rate are burnt
Junction temperature is 500 DEG C, sintering pressure 40MPa, and soaking time finishes cooled to room temperature, obtain electrode in 4min, sintering
With Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize Cu2The connection of Se base thermoelectricity materials and the electrode.
The present embodiment the electrode obtained thickness 0.5-0.9mm, gradient transition layer thickness are about 0.2mm, thermoelectric material layer thickness
About 13mm.
Fig. 1 is Cu2The backscattered electron image of Se component connection joints interface.It can be seen that combination electrode and gradient mistake
It crosses between layer, gradient transitional lay and Cu2Interface cohesion between Se is good, without apparent micro-crack.
Fig. 2 is Cu corresponding with Fig. 12The resistance change curves of Se component connection joints vicinity, contact cross-section be 5mm ×
5mm.It can be seen that joint contact resistance (including interface resistance between electrode resistance, electrode and gradient transitional lay,
Gradient transitional lay resistance, gradient transitional lay and Cu2Interface resistance between Se) in 0.1mohm or so, i.e. contact resistivity exists
25uohm*cm2Left and right.
Control group 1：It is in place of the control group and the difference of embodiment 2：It is not provided with gradient transitional lay.
Control group 2：It is in place of the control group and the difference of embodiment 2：It is not provided with gradient transitional lay, electrode layer powder
Using Al powder.
Fig. 3 is Cu in control group 12The backscattered electron image of Se component connection joints interface.It can be seen that combination electrode
With Cu2Interface cohesion between Se is preferable, but has a small amount of micro-crack to occur.
Fig. 4 is Cu corresponding with Fig. 32The resistance change curves of Se component connection joints vicinity, contact cross-section be 5mm ×
5mm.It can be seen that contact resistance (including electrode resistance, electrode and the Cu of joint2Interface resistance between Se)
0.3mohm or so, i.e., contact resistivity is in 75uohm*cm2Left and right.
Fig. 5 is Cu in control group 12The backscattered electron image of Se component connection joints interface.It can be seen that Al electrodes with
Cu2Interface cohesion between Se is preferable, but has more micro-crack to occur.
Fig. 6 is Cu corresponding with Fig. 52The resistance change curves of Se component connection joints vicinity, contact cross-section be 5mm ×
5mm.It can be seen that contact resistance (including electrode resistance, electrode and the Cu of joint2Interface resistance between Se)
0.4mohm or so, i.e., contact resistivity is in 100uohm*cm2Left and right.
Embodiment 3
A kind of and Cu2The electrode that Se base thermoelectricity materials match, the electrode are the mixed of Ni-Al alloys and metal simple-substance Al
Object is closed, the wherein mass percentage of metal simple-substance Al is 60%, and surplus is Ni-Al alloys.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials, specific process step are：
(1) according to the ratio that the mass percent of metal simple-substance Al powder is 60%, surplus is Ni-Al alloyed powders, gold is weighed
Belong to simple substance Al powder and Ni-Al alloyed powders, is uniformly mixed and obtains electrode layer powder；
(2) according to Cu2The volume ratio 1 of electrode material powder obtained by Se powders, step (1):1, weigh Cu2Se base thermoelectricity
Material powder, electrode material powder grind 30min and are uniformly mixed, obtain gradient transitional lay powder in the agate mortar；
(3) 2 parts of electrode layer powder in step (1), every part of 0.5g are weighed；Weigh 2 parts, every part of gradient transitional lay powder
0.20g；Weigh Cu2Se thermoelectric material powders 12.0g；
The Cu that will be weighed2Se powders are uniformly layered in graphite jig, carry out precompressed；Then in Cu2Se base thermoelectricity material powder
Body layer upper and lower ends are uniformly laid with gradient transitional lay material powder, and carry out precompressed；Again two above and below gradient transitional lay powder
End is uniform respectively to be laid with electrode layer powder, and carries out precompressed, and each layer is according to electrode layer powder, gradient mistake in gained graphite jig
Cross a layer powder, Cu2The sequence distribution of Se base thermoelectricity materials powder, gradient transitional lay powder, electrode layer powder；
Then discharge plasma sintering will be carried out in the graphite jig, vacuum degree 12pa, 80 DEG C/min of heating rate are burnt
Junction temperature is 500 DEG C, sintering pressure 30MPa, and soaking time finishes cooled to room temperature, obtain electrode in 5min, sintering
With Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize Cu2The connection of Se base thermoelectricity materials and the electrode.
The present embodiment the electrode obtained thickness 0.4-0.7mm, gradient transition layer thickness are about 0.2mm, thermoelectric material layer thickness
About 10mm.
Embodiment 4
A kind of and Cu2The electrode that Se base thermoelectricity materials match, the electrode are the mixed of Ni-Al alloys and metal simple-substance Al
Object is closed, the wherein mass percentage of metal simple-substance Al is 50%, and surplus is Ni-Al alloys.
Electrode and Cu of the present invention2The Joining Technology of Se base thermoelectricity materials, specific process step are：
(1) according to the ratio that the mass percent of metal simple-substance Al powder is 50%, surplus is Ni-Al alloyed powders, gold is weighed
Belong to simple substance Al powder and Ni-Al alloyed powders, grinding 30min, which is uniformly mixed, in the agate mortar obtains electrode layer powder；
(2) according to Cu2The volume ratio 1 of electrode material powder obtained by Se powders, step (1):1, weigh Cu2Se base thermoelectricity
Material powder, electrode material powder grind 30min and are uniformly mixed, obtain gradient transitional lay powder in the agate mortar；
(3) 2 parts of electrode layer powder in step (1), every part of 0.5g are weighed；Weigh 2 parts, every part of gradient transitional lay powder
0.20g；Weigh Cu2Se thermoelectric material powders 12.0g；
The Cu that will be weighed2Se powders are uniformly layered in graphite jig, carry out precompressed；Then in Cu2Se base thermoelectricity material powder
Body layer upper and lower ends are uniformly laid with gradient transitional lay material powder, and carry out precompressed；Again two above and below gradient transitional lay powder
End is uniform respectively to be laid with electrode layer powder, and carries out precompressed, and each layer is according to electrode layer powder, gradient mistake in gained graphite jig
Cross a layer powder, Cu2The sequence distribution of Se base thermoelectricity materials powder, gradient transitional lay powder, electrode layer powder；
Then discharge plasma sintering will be carried out in the graphite jig, vacuum degree 12pa, 80 DEG C/min of heating rate are burnt
Junction temperature is 490 DEG C, sintering pressure 50MPa, and soaking time finishes cooled to room temperature, obtain electrode in 5min, sintering
With Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize Cu2The connection of Se base thermoelectricity materials and the electrode.
The present embodiment the electrode obtained thickness 0.5-0.8mm, gradient transition layer thickness are about 0.2mm, thermoelectric material layer thickness
About 10mm.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to the present invention's
Protection domain.
Claims (7)
1. a kind of and Cu2The electrode that Se base thermoelectricity materials match, it is characterised in that the electrode is Ni-Al alloys and metal list
The mixture of matter Al, the wherein mass percentage of metal simple-substance Al are 40%-60%, and surplus is Ni-Al alloys；The electrode
With Cu2Se base thermoelectricity materials are connected by discharge plasma sintering, are wherein provided with gradient transition between electrode and thermoelectric material
Layer；The thickness of the gradient transitional lay is 0.1-0.3mm；The gradient transitional lay is Cu2Se base thermoelectricity materials powder and electrode
Powder according to volume ratio 1:1 mixes.
2. a kind of and Cu according to claim 12The electrode that Se base thermoelectricity materials match, it is characterised in that the Ni-Al
The mass percentage of Ni is 48% in alloy, remaining is Al.
3. a kind of and Cu according to claim 12The electrode that Se base thermoelectricity materials match, it is characterised in that the electrode
Thickness be 0.5-3mm.
4. electrode and Cu according to claim 12The Joining Technology of Se base thermoelectricity materials, it is characterised in that its processing step is：
（1）The ratio that mass percent according to metal simple-substance Al powder is 40%-60%, surplus is Ni-Al alloyed powders, weighs metal
Simple substance Al powder and Ni-Al alloyed powders are uniformly mixed and obtain electrode layer powder；
（2）According to Cu2Se powders, step（1）The volume ratio 1 of the electrode material powder of gained:1, weigh Cu2Se base thermoelectricity materials
Powder, electrode material powder are uniformly mixed and obtain gradient transitional lay powder；
（3）According to electrode layer powder, gradient transitional lay powder, Cu2Se base thermoelectricity materials powder, gradient transitional lay powder, electrode layer
The sequence of powder, by Cu2Se base thermoelectricity materials powder, step 2）Gained gradient transitional lay powder and electrode layer powder are layed in stone
It is sintered in black mold, obtains electrode and Cu2The densification block that Se base thermoelectricity materials are well combined, that is, realize Cu2Se base heat
The connection of electric material and the electrode.
5. electrode and Cu according to claim 42The Joining Technology of Se base thermoelectricity materials, it is characterised in that step 3）It is middle to incite somebody to action
Cu2Se base thermoelectricity materials powder, step 2）Gained gradient transitional lay powder and electrode layer powder are layed in graphite jig and are sintered
Before, further include pressing step.
6. electrode and Cu according to claim 42The Joining Technology of Se base thermoelectricity materials, it is characterised in that true when the sintering
Reciprocal of duty cycle is 10pa-15pa, and sintering pressure 30-50MPa, sintering temperature is 470-550 DEG C.
7. electrode and Cu according to claim 42The Joining Technology of Se base thermoelectricity materials, it is characterised in that described be sintered to is put
Electric plasma agglomeration, heating rate are 60-80 DEG C/min, soaking time 3-5min.
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| CN111864043B (en) * | 2020-08-06 | 2023-02-28 | 武汉理工大学 | P-type Cu2 Se-based thermoelectric element and integrated preparation process thereof |
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| CN101022149A (en) * | 2007-03-02 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | Alloy electrod matched with cobalt antimonide thermoelectric component and one-step process connecting technology |
| CN102412366A (en) * | 2011-09-30 | 2012-04-11 | 中国科学院上海硅酸盐研究所 | Bismuth-telluride-based thermoelectric element and preparation method thereof |
| CN103219456A (en) * | 2013-04-02 | 2013-07-24 | 武汉理工大学 | Electrode matched with Mg-Si-Sn-based thermoelectric element and connecting process thereof |
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| CN101022149A (en) * | 2007-03-02 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | Alloy electrod matched with cobalt antimonide thermoelectric component and one-step process connecting technology |
| CN102412366A (en) * | 2011-09-30 | 2012-04-11 | 中国科学院上海硅酸盐研究所 | Bismuth-telluride-based thermoelectric element and preparation method thereof |
| CN103219456A (en) * | 2013-04-02 | 2013-07-24 | 武汉理工大学 | Electrode matched with Mg-Si-Sn-based thermoelectric element and connecting process thereof |
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