CN109285940B - With the matched electrode of thermoelectric material and attaching method thereof - Google Patents
With the matched electrode of thermoelectric material and attaching method thereof Download PDFInfo
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- CN109285940B CN109285940B CN201810832305.7A CN201810832305A CN109285940B CN 109285940 B CN109285940 B CN 109285940B CN 201810832305 A CN201810832305 A CN 201810832305A CN 109285940 B CN109285940 B CN 109285940B
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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
- H10N10/80—Constructional details
- H10N10/81—Structural details of the junction
- H10N10/817—Structural details of the junction the junction being non-separable, e.g. being cemented, sintered or soldered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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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
- H10N10/01—Manufacture or treatment
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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
- H10N10/80—Constructional details
- H10N10/82—Connection of interconnections
Abstract
The invention belongs to electrochemical technology fields, and in particular to a kind of and matched electrode of thermoelectric material and attaching method thereof.It should be silver-nickel with the matched electrode of thermoelectric material, and the thermoelectric material is FeNb0.88Hf0.12Sb base thermoelectricity material.The silver-nickel and FeNb0.88Hf0.12After the connection of Sb base thermoelectricity material, the metallic compound that linkage interface generates after timeliness keeps stablizing, do not extend influence further the performance of thermoelectric material, compared to existing common Cu electrode material, silver-nickel of the invention will not reduce the performance of thermoelectric material after imitating at high temperature, and the electric conductivity of silver-nickel is more preferable, to keep external resistor smaller, device it is more efficient, therefore, silver-nickel is highly suitable as FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of and the matched electrode of thermoelectric material and its connection side
Method.
Background technique
Pyroelectric technology realizes the direct conversion of thermal energy and electric energy by Seebeck effect.Not with other energy conversion technologies
Together, the entire conversion process of pyroelectric technology all carries out in the solid state, have it is small in size, pollution-free, without transmission parts, without making an uproar
Sound and reliability height etc. are excellent.In view of above-mentioned advantage, pyroelectric technology has great application prospect, and it is each to can be not only used for recycling
The low-grade waste heat of class, waste heat, are also used as the power supply of military equipment, aerospace vehicle etc..
Since the 1950s, a variety of materials have been studied, including traditional thermoelectric material:
Bi2Te3, PbTe and Si1-xGex, they respectively room temperature, in have good performance under mild high temperature.FeNb0.88Hf0.12Sbization
Closing object is a kind of thermoelectric material suitable for high temperature field, and the Seebeck coefficient and power factor of alloy are all bigger, 325
DEG C power factor can reach 6200 μ Wm-1·K-1；And its fusing point is high, and high-temperature stability is also fine, this is hot to expand
The use temperature range of electric material provides advantage, therefore has very big development space, FeNb0.88Hf0.12Sb thermoelectric material exists
High temperature thermoelectric power generation field has huge application prospect.But its component technology is still far from perfect at present, wherein electrode
The selection of material is the problem that must be faced first.Mostly use Cu as electrode material greatly low-temperature thermoelectric material, but for
High temperature thermoelectric material, due to using the raising of temperature, Cu is reacted with thermoelectric material in linkage interface during imitating at high temperature
Seriously, the performance for having seriously affected thermoelectric material, increases contact resistance, so the choosing of centering high temperature thermoelectric device electrode material
With and joint technology suffer from higher requirement.
The electrode material of thermoelectric material requires following characteristic: (1) in use temperature range with thermoelectric material matrix
Without serious phase counterdiffusion or chemical reaction, to guarantee that thermoelectric material is able to maintain the thermoelectric conversion of itself during military service
Efficiency；There are certain conductances for thermoelectric material when due to high temperature, can guarantee thermoelectric material certainly without electrochemical reaction with thermoelectric material
Body performance is unaffected and stability between thermoelectric material and electrode interface；(2) there is high conductivity and thermal conductivity, with
The temperature difference is utmostly passed into thermoelectric material；(3) thermal expansion coefficient will match with thermoelectric material, to prevent thermal stress from causing
Micro-crack reduces device power to generate biggish contact resistance；(4) in addition, also to have in use temperature range certain
Inoxidizability.
Existing electrode material is difficult to and FeNb0.88Hf0.12The matching of Sb thermoelectric material, therefore the prior art has much room for improvement.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, provide it is a kind of with the matched electrode of thermoelectric material and
Its connection method, it is intended to solve existing electrode material and be difficult to and FeNb0.88Hf0.12The technical issues of Sb base thermoelectricity material matches.
For achieving the above object, The technical solution adopted by the invention is as follows:
One aspect of the present invention provides a kind of with the matched electrode of thermoelectric material, and the electrode is silver-nickel, and the heat
Electric material is FeNb0.88Hf0.12Sb base thermoelectricity material.
The present invention provides one kind can be with FeNb0.88Hf0.12The silver-nickel electrode of Sb base thermoelectricity material good match, should
Silver-nickel and FeNb0.88Hf0.12After the connection of Sb base thermoelectricity material, the metallic compound that linkage interface generates after timeliness is kept
Stablize, the performance for the thermoelectric material that do not extend influence further, compared to existing common Cu electrode material, silver-colored nickel of the invention is closed
Gold will not reduce the performance of thermoelectric material after imitating at high temperature, and the electric conductivity of silver-nickel is more preferable, to make external resistor
It is smaller, device it is more efficient, therefore, silver-nickel is highly suitable as FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material.
Another aspect of the present invention provides a kind of connection method of electrode, includes the following steps:
By silver powder and nickel powder mixed processing, mixed powder is obtained；
FeNb is provided0.88Hf0.12Sb base thermoelectricity material matrix；
The mixed powder is laid on the FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface, is sintered,
It obtains and FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material matrix connection；
Wherein, the electrode is silver-nickel.
In the connection method of electrode provided by the invention, the mixed powder containing silver powder and nickel powder is laid on
FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface is sintered, and can be obtained and FeNb0.88Hf0.12Sb base thermoelectricity material base
The silver-nickel electrode that body is successfully connected；The Joining Technology is simple, at low cost, final silver-nickel and FeNb0.88Hf0.12Sb
Base thermoelectricity material matrix is completely embedded no crack, and interface cohesion is secured, very small in conjunction with surface resistance transition, and linkage interface
The metallic compound generated after timeliness keeps stablizing, the performance for the thermoelectric material that do not extend influence further, normal compared to existing
The Cu electrode material seen, the silver-nickel that the present invention connects will not reduce the performance of thermoelectric material, Er Qieyin after imitating at high temperature
The electric conductivity of nickel alloy is more preferable, to keep external resistor smaller, device it is more efficient.
Detailed description of the invention
Fig. 1 is FeNb in the embodiment of the present invention 20.88Hf0.12Sb/ silver-nickel linkage interface, the microcosmic shape under different multiples
Looks figure；Wherein, (a) 5k multiple；(b) 10k multiple；(c) 20k multiple；
Fig. 2 is FeNb in the embodiment of the present invention 20.88Hf0.12Sb/ silver-nickel linkage interface, EDS elemental composition analysis chart；
Fig. 3 is FeNb in the embodiment of the present invention 20.88Hf0.12Sb/ silver-nickel linkage interface, the SEM with timeliness variation scheme；
Fig. 4 is FeNb in the embodiment of the present invention 20.88Hf0.12After Sb/ silver-nickel timeliness 192h, contact resistance test result
Figure.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
On the one hand, the embodiment of the invention provides a kind of and matched electrode of thermoelectric material, the electrode is silver-nickel,
And the thermoelectric material is FeNb0.88Hf0.12Sb base thermoelectricity material.
The embodiment of the present invention provides one kind can be with FeNb0.88Hf0.12The silver-nickel electricity of Sb base thermoelectricity material good match
Pole, the silver-nickel and FeNb0.88Hf0.12After the connection of Sb base thermoelectricity material, metallic compound that linkage interface generates after timeliness
It keeps stablizing, the performance for the thermoelectric material that do not extend influence further, compared to existing common Cu electrode material, the present invention is implemented
The silver-nickel of example will not reduce the performance of thermoelectric material after imitating at high temperature, and the electric conductivity of silver-nickel is more preferable, thus
Keep external resistor smaller, device it is more efficient, therefore, which is highly suitable as FeNb0.88Hf0.12Sb base thermoelectricity
The electrode of material.
Further, in the electrode of the embodiment of the present invention, by the gross mass of the silver-nickel be 100% in terms of, it is described
The mass percentage of Ag is 85-95%, surplus Ni in silver-nickel.Silver-nickel within the scope of the mass percentage,
Can preferably with FeNb0.88Hf0.12The matching of Sb base thermoelectricity material.It is highly preferred that the quality percentage of Ag contains in the silver-nickel
Amount is 90%, and surplus is Ni (i.e. 10%).
Further, in the electrode of the embodiment of the present invention, the electrode with a thickness of 0.1-0.4mm.In
FeNb0.88Hf0.12The silver-nickel electrode that Sb base thermoelectricity material surface is formed with a thickness of 0.1-0.4mm, both can be improved electric conductivity
The performance of thermoelectric material is not influenced again.
On the other hand, the embodiment of the invention also provides a kind of connection method of electrode, include the following steps:
S01: by silver powder and nickel powder mixed processing, mixed powder is obtained；
S02: FeNb is provided0.88Hf0.12Sb base thermoelectricity material matrix；
S03: the mixed powder is laid on the FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface, is sintered
Processing, obtains and FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material matrix connection；
Wherein, the electrode is silver-nickel.
In the connection method of electrode provided in an embodiment of the present invention, the mixed powder containing silver powder and nickel powder is laid on
FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface is sintered, and can be obtained and FeNb0.88Hf0.12Sb base thermoelectricity material base
The silver-nickel electrode that body is successfully connected；The Joining Technology is simple, at low cost, final silver-nickel and FeNb0.88Hf0.12Sb
Base thermoelectricity material matrix is completely embedded no crack, and interface cohesion is secured, very small in conjunction with surface resistance transition, and linkage interface
The metallic compound generated after timeliness keeps stablizing, the performance for the thermoelectric material that do not extend influence further, normal compared to existing
The Cu electrode material seen, the embodiment of the present invention and FeNb0.88Hf0.12The silver-nickel of Sb base thermoelectricity material matrix connection, in high temperature
The performance of thermoelectric material will not be reduced after timeliness, and the electric conductivity of silver-nickel is more preferable, thus keep external resistor smaller, device
It is more efficient.
Further, in above-mentioned steps S01, the mass ratio of the silver powder and the nickel powder is (85-95): (5-15).It will
Two kinds of metal simple-substance powder are uniformly mixed in the ratio, obtain the mixed powder for being used to form electrode layer, follow-up sintering can be formed
It is connected to FeNb0.88Hf0.12The silver-colored nickel composite electrode of Sb base thermoelectricity material matrix surface.The quality is closed than the silver-colored nickel obtained in range
Gold, can preferably with FeNb0.88Hf0.12The matching of Sb base thermoelectricity material.Finally in FeNb0.88Hf0.12Sb base thermoelectricity material matrix
The silver-nickel layer that surface is formed with a thickness of 0.1-0.4mm.
Further, in above-mentioned steps S02, FeNb0.88Hf0.12Sb base thermoelectricity material matrix can use SPS (Spark
Plasma Sintering, i.e. discharge plasma sintering) hot pressed sintering preparation, include the following steps: to weigh thermoelectricity material according to the ratio
Simple substance element required for expecting carries out smelting in suspension and obtains ingot casting；Ingot casting is put into vitreosil pipe and is annealed；It is ground to
200 mesh powders；By powder sintering at block；FeNb is obtained after SPS hot pressed sintering0.88Hf0.12Sb base thermoelectricity material block.More into
One step, the mixed powder is being laid on the FeNb0.88Hf0.12Before the step of Sb base thermoelectricity material matrix surface, first
By the FeNb0.88Hf0.12Sb base thermoelectricity material matrix successively carries out sanding and polishing and ultrasonic treatment.Make in this way
FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface is cleaner and tidier, is more advantageous to and connect with silver-nickel.
Further, in above-mentioned steps S03, the sintering processes are discharge plasma sintering.I.e. silver-nickel also by
SPS technique is connected to FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface.Further, the discharge plasma sintering is true
Reciprocal of duty cycle is 0.5 × 10-2-1.5×10-2MPa, preferably 1 × 10-2MPa；The pressure of the discharge plasma sintering is 35-45Mpa,
It is preferred that 40Mpa；The temperature of the discharge plasma sintering is 650-700 DEG C, preferably 680 DEG C；The discharge plasma sintering
Time is 18-20min, preferably 20min.Within the scope of above-mentioned vacuum degree, pressure, temperature and time, silver-nickel can be made more
Add and is securely attached to FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface, and will not be to the performance for reducing thermoelectric material.Into
One step, it, can be with the heating of 50 DEG C/min in the discharge plasma sintering in order to carry out entire sintering process orderly
Rate is warming up to 650-700 DEG C and is sintered, in this way can be excessively fierce to avoid reaction, finally keeps the temperature 18-20min and completes
Sintering.
The present invention successively carried out test of many times, and it is further detailed as reference pair invention progress now to lift A partial experiment result
Thin description, is described in detail combined with specific embodiments below.
Embodiment 1
FeNb0.88Hf0.12The preparation of Sb base thermoelectricity material matrix:
a)FeNb0.88Hf0.12The stoichiometric ratio of Sb measures each source metal (being accurate to after decimal point 4), weighs according to the ratio
Simple substance element required for thermoelectric material, which is put into the sample cell of suspension smelting furnace, carries out smelting in suspension, Sb on the basis of claim more
5% mass fraction obtains ingot casting after smelting in suspension；
When vacuum degree reaches 10-3Protection gas argon gas is filled with when Pa or less, it is molten then to establish beginning suspension by cable in electric current for 50A decentralization
Sample is refined, until each source metal raw material is melt into liquid.In order to ensure melting is uniform, each sample melting at least 3 times, each time
For 5min, and sample is overturn to another side after melting every time, tube sealing then is carried out to melted sample.
B) above-mentioned ingot casting is put into vitreosil pipe and is annealed；Annealing temperature is 900 DEG C, and the time is 168h (7 days)；
C) after being furnace-cooled to room temperature, the block sample that melting is obtained in mortar hand-ground at 200 mesh powder；
D) being correspondingly placed into diameter with electronic balance weighing about 5g powder sample is that SPS heat is carried out in the graphite jig of 15mm
Pressure sintering it is blocking: the temperature of SPS hot pressing be 850 DEG C, sintering pressure 60MPa, maximum sintering temperature hold time for
15min.It is 15mm, the long 40mm of die sleeve, graphite pressure head outer diameter 14.6mm with internal diameter, the graphite jig of length 25mm, above and below sample
Upper graphite paper is padded respectively；
E) sintered block is polished off into graphite paper, polishing, ultrasonic clean surface.
Embodiment 2
FeNb0.88Hf0.12The Joining Technology of Sb base thermoelectricity material and silver-nickel electrode
A) electrode material mixed powder: silver powder (200 mesh), nickel powder (200 mesh), wherein the quality percentage of metal simple-substance Ag contains
Amount is 90wt%, and surplus is Ni (10wt%)；
B) in the graphite jig for being 15mm to diameter, electrode material mixed powder, embodiment 1 are successively packed into
FeNb0.88Hf0.12Sb base thermoelectricity material block, electrode material mixed powder, will by the method for SPS hot pressed sintering
FeNb0.88Hf0.12Sb base thermoelectricity material block is sintered together with electrode material；Wherein, vacuum degree is 1 × 10 when sintering- 3MPa, sintering pressure 40Mpa, sintering temperature are 680 DEG C.
C) the sample body for forming sintering polishes off after the graphite paper of surface by diamond wire saw, is cut into device regulation
Length and width, formed half-Heusler thermo-electric device high temperature electrode silver-nickel.
Fig. 1 is FeNb in the embodiment of the present invention0.88Hf0.12Microcosmic shape of the Sb/ silver-nickel linkage interface under different multiples
Looks figure；It was found from figure: silver-nickel and FeNb0.88Hf0.12Sb base thermoelectricity material block is completely embedded no crack.Fig. 2 is this hair
FeNb in bright embodiment0.88Hf0.12The EDS elemental composition analysis chart of Sb/ silver-nickel linkage interface；From Ag after sintering known to figure
(d) thermoelectric material is not diffused into largely, and the element of thermoelectric material does not also diffuse into electrode material；Fig. 3 is this
FeNb in inventive embodiments0.88Hf0.12Sb/ silver-nickel linkage interface is schemed with the SEM that timeliness changes, and is spread as can be seen from Fig.
Layer tends towards stability after 96h, final to stablize at 20 μm or so；Fig. 4 is FeNb in the embodiment of the present invention0.88Hf0.12Sb/ silver nickel closes
Contact resistance test result figure after golden timeliness 192h is about 0.4116 μ Ω cm from contact resistance known to figure2。
It was found from above-mentioned figure: silver-nickel electrode and FeNb0.88Hf0.12Sb base thermoelectricity material forms the densification being well combined
Change block, and FeNb0.88Hf0.12Metallic compound that Sb/ silver nickel linkage interface generates after timeliness keeps stablizing, not into
One step extends influence the performance of thermoelectric material, thus silver-nickel imitate at high temperature after will not reduce the performance of thermoelectric material, and
And the electric conductivity of silver-nickel is more preferable, external resistor is smaller, device it is more efficient, therefore, silver-nickel is highly suitable as
FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of connection method of electrode, which comprises the steps of:
By silver powder and nickel powder mixed processing, mixed powder is obtained；
FeNb is provided0.88Hf0.12Sb base thermoelectricity material matrix；
The mixed powder is laid on the FeNb0.88Hf0.12Sb base thermoelectricity material matrix surface, is sintered, obtains
With FeNb0.88Hf0.12The electrode of Sb base thermoelectricity material matrix connection；
Wherein, the electrode is silver-nickel, is Ag in the silver-nickel in terms of 100% by the gross mass of the silver-nickel
Mass percentage be 85-95%, surplus Ni.
2. the connection method of electrode as described in claim 1, which is characterized in that the sintering processes are plasma discharging burning
Knot.
3. the connection method of electrode as claimed in claim 2, which is characterized in that the vacuum degree of the discharge plasma sintering is
0.5×10-2-1.5×10-2MPa；And/or
The pressure of the discharge plasma sintering is 35-45Mpa；And/or
The temperature of the discharge plasma sintering is 650-700 DEG C；And/or
The time of the discharge plasma sintering is 18-20min.
4. the connection method of electrode as claimed in claim 2, which is characterized in that in the discharge plasma sintering, with 50 DEG C/
The heating rate of min is warming up to 650-700 DEG C and is sintered.
5. the connection method of electrode as described in claim 1, which is characterized in that described the mixed powder to be laid on
FeNb0.88Hf0.12Before the step of Sb base thermoelectricity material matrix surface, first by the FeNb0.88Hf0.12Sb base thermoelectricity material base
Body successively carries out sanding and polishing and ultrasonic treatment.
6. the connection method of electrode as described in any one in claim 1-5, which is characterized in that the silver powder and the nickel powder
Mass ratio is (85-95): (5-15)；And/or
The electrode with a thickness of 0.1-0.4mm.
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