CN101136450A - Pi type CoSb3 based thermoelectric converting device and method for producing the same - Google Patents
Pi type CoSb3 based thermoelectric converting device and method for producing the same Download PDFInfo
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Abstract
This invention relates to a Pa-type CoSb3-base thermoelectric converting device including: a Mo-Cu alloy electrode at an end of high temperature, a welding layer of the high temperature end, a diffusion blocking layer, thermoelectric pins, a metal layer, a welding layer and an electrode of the low temperature end, in which, the thermoelectric pins are made of P or N-type CoSb3-base thermoelectric material and are connected with the Mo-Cu alloy electrode into one unit by the welding layer of the high temperature end to form a high temperature end, the low temperature end of the pins are connected with the electrode of its end by the metal layer and the welding layer of the low temperature end, which utilizes a SPS quick welding technology to realize heat match as much as possible and no obvious crack exists at the high temperature end.
Description
Technical field
The present invention relates to a kind of π type CoSb
3Based thermoelectric converting device and preparation method, the particularly technology that is connected of antimony cobalt thermoelectric material and electrode belongs to the preparing technical field of thermoelectric device.
Background technology
Thermoelectric material is a kind of functional material that directly heat energy and electric energy is transformed mutually, and the Seebeck effect of its utilization itself is converted into electric energy with heat energy.Serious day by day along with global environmental pollution and energy crisis makes design and preparation thermoelectric device more and more receive the attention of countries in the world.Refrigeration and the power generating device volume made by thermoelectric material are little, in light weight, do not have any mechanical driving part, noiseless in the work, and long service life is particularly suitable for space flight, used heat cogeneration, vehicle exhaust, fields such as underground heat.
At present, about the thermoelectric device technology of preparing of low temperature thermo-electric generation and refrigeration suitable maturation such as bismuth telluride for example, multistage thermoelectric device also and be widely used in commodity production, as patent documentation CN1839486, US005966939A, US005936192A etc.Antimony brill based compound thermoelectric material because of its special electronic structure be considered to the most promising in warm electricity generation material, and its thermoelectric figure of merit of antimony cobalt-based compound (ZT) of P type or N type has all reached more than 1.0 at present, demonstrate at industrial waste heat, the vehicle exhaust aspect has broad application prospects.Because low temperature thermoelectric unit spare adopts the Sn-Pb solder usually, and the Sn in the Sn-Pb solder will diffuse into thermoelectric semiconductor when temperature is higher than 80 ℃, influence thermoelectricity capability thereby will form mixes or react with thermoelectric semiconductor, the electrode interconnection technique of key technology has been subjected to great challenge in therefore preparing as device in the preparation of middle elevated temperature heat electric device.The cobalt stibium antimonide based thermoelectric device high temperature electrode is connected the mode that the spring pressure contact has generally been adopted in U.S. JPL laboratory at present, and the mode interface contact resistance and the contact heat resistance of the contact of this kind pressure are all bigger, greatly reduces the power generation performance of device integral body.Because thermoelectric power generation device general size is less, the influence that brings of small interface is just big more more for size, therefore in the preparation of elevated temperature heat electric device the direct connection of temperature end electrode remain the technological difficulties that present countries in the world need be broken through.The domestic research that concentrates on thermoelectric material about the research of cobalt stibium antimonide based thermoelectric device in a large number, done a large amount of work on the preparation of silicon place antimony cobalt-based thermoelectric material and the element manufacturing in the Chinese Academy of Sciences, as patent CN1585145A, US20060017170Al.200710037778.X etc.The present invention is intending formerly providing a kind of π type cobalt stibium antimonide based thermoelectric device and preparation method on the working foundation, the temperature end electrode is selected the Mo-Cu alloy electrode for use, temperature end connects the Ag-Cu weld tabs that adopts nearly eutectic, diffusion impervious layer such as Mo, W forms by plasma spraying, thermoelectric device is welded by discharge plasma sintering process (SPS), and low-temperature end adopts traditional Sn scolder to be connected with Cu sheet soldering on the ceramic substrate.
Summary of the invention
The invention provides a kind of cobalt stibium antimonide based thermoelectric device and preparation method, by the thin diffusion impervious layer of plasma spraying on thermoelectric block body one, the one or more elemental diffusion that effectively stopped the thermoelectric semiconductor device make device have reliable hot property.Secondly the use of diffusion impervious layer makes that with the connection procedure that is converted into metal and metal that is connected between thermoelectric semiconductor and the metal electrode welding of device is easier.The Ag-Cu weld tabs of the nearly eutectic that adopts not only only can satisfy the temperature scope of application of 500-600 ℃ of cobalt stibium antimonide based thermoelectric device temperature end, more warm electric material preparation of devices provides good welding material in other, and electrode material is selected the Mo-Cu alloy material close with antimony cobalt thermal coefficient of expansion for use, farthest realize hot coupling, reduced the thermal stress that produces because of thermal mismatching.
Characteristic part of the present invention has been to select the Ag-Cu weld tabs of suitable electrode Mo-Cu material and the electrode welding material of high temperature-nearly eutectic, solved the problem of welding difficulty owing to the serviceability temperature of temperature end is too high, thermoelectric block body plasma spraying one deck diffusion impervious layer at sintering, not only be to stop the counterdiffusion mutually of element and welding material in the thermoelectric material, also be metal and semi-conductive Welding Problems have been changed into the Welding Problems of metal and metal, make and utilize the SPS welding to be easier to carry out, the intensity of the device welding that obtains is also higher.
The preparation method of cobalt stibium antimonide based thermoelectric device provided by the invention comprises following steps:
A) utilize SPS to prepare the CoSb of P type and N type
3Base thermoelectric semiconductor, its concrete sintering parameter is vacuum degree 5-15Pa, and sintering pressure is 50-60MPa, and heating rate is 120-180 ℃/min, and sintering temperature is 580-600 ℃, is incubated 10-30min then, the SPS sintering finishes, the CoSb that obtains
3The thermoelectric cylinder of base is shown in Fig. 1 (a).
B) thermoelectric block body that sinters requires to carry out the line cutting according to the device optimization design size, obtain the cylindrical or square thermoelectric pin of P type and N type, shown in Fig. 1 (b), utilize sand-blast that two end face is handled then, make its end face obtain certain surface roughness, the ultrasonic impurity particle that cleans out end face, end face is as Fig. 2 (a) with shown in Fig. 2 (b).
C) at the CoSb of P type and N type
3A diffusion impervious layer that approaches on the plasma spraying on the both ends of the surface of base thermoelectric semiconductor, barrier layer thickness is at 5-40 μ m, the barrier layer element contains at least a element of selecting among Mo, W, Ti, Nb and the Ta etc. to be formed, with Ag-Cu alloy weld tabs element or the Sn-Pb scolder elemental diffusion that prevents the thermoelectric material element and be used to connect, the concrete technological parameter of plasma spraying is work arc voltage 75V, operating current 300A, and spray is apart from 100mm, for powder amount 40g/min, for powder throughput 0.56m
3/ h.
D) be written on the thermoelectric foot face diffusion impervious layer after selecting Ag-Cu alloy weld tabs absolute ethyl alcohol cleaning for use, put into then and CoSb
3The Mo-Cu alloy electrode that the base thermoelectricity material thermal coefficient of expansion is complementary, utilize SPS to carry out rapid welding, it is vacuum degree 5-15Pa that SPS welds concrete technological parameter, sintering pressure is 10-25MPa, and heating rate is 200-250 ℃/min, is incubated 30-60 second at 550 ℃, slowly cooling then, rate of temperature fall is controlled at 80-150 ℃/min, and SPS welds end, and thermoelectric pin cross section is shown in Fig. 2 (c) and Fig. 2 (d) in the sintering process.
Before SPS, need carry out sandblasting pretreatment in advance at the Mo-Cu alloy electrode, make its surface have certain surface roughness, the ultrasonic surface impurity of getting rid of.
E) at the CoSb of P type and N type
3The low-temperature end of base thermoelectric semiconductor is electroplated on the barrier layer or the Ni layer of the about 30 μ m of vacuum sputtering one layer thickness, adopts the Sn-Pb scolder that Cu sheet on low-temperature end and the ceramic substrate is carried out soldering then and is connected, and the thermoelectric element for preparing as shown in Figure 3.
The invention provides the method for plasma spraying diffusion impervious layer, not only can effectively stop thermoelectric material element and the counterdiffusion mutually of welding element, after more being the plasma spraying diffusion layer, the device shear strength is greatly improved, the thermoelectric device for preparing is carried out the test of shear strength, the device interfaces shear strength that discovery does not spray the Mo diffusion layer is 12.92MPa, and after waiting particle spraying Mo diffusion impervious layer, device is 19.24 MPa along electrode and material interface place shear strength, has not improved 48.9% than spraying diffusion impervious layer.
As shown in the figure, π type CoSb provided by the invention
3Based thermoelectric converting device is characterised in that:
Described thermoelectric device is made up of Mo-Cu alloy electrode (1), high-temperature soldering layer (2), temperature end diffusion impervious layer (3), thermoelectric pin (4), low-temperature end diffusion impervious layer (5), low-temperature end metal Ni layer (6), low-temperature end weld layer (7) and low-temperature end electrode (8); Wherein, thermoelectric pin (4) is P type and N type CoSb
3Base thermoelectricity material, they are by high-temperature soldering layer (2) and Mo-Cu alloy electrode (1) the formation temperature end that fuses, and the P type then is connected with low-temperature end electrode (8) by low-temperature end metal level (6), low-temperature end weld layer (7) with the low-temperature end of the thermoelectric pin of N type.The mass percent of Cu is 45%-60% in the described Mo-Cu alloy electrode (1), and all the other are Mo and small amount of impurities element; Described diffusion impervious layer (3,5) is at least a element of selecting among Mo, W, Ti, Nb and the Ta etc. is formed; Temperature end weld layer (2) is an Ag-Cu alloy weld tabs, Cu quality percentage composition 30%-60% wherein, and surplus is Ag and small amount of impurities element; Low-temperature end weld layer (7) is the Sn-Pb scolder, and wherein the Sn constituent content is at 25%-60%; Low-temperature end is electrode with the copper sheet, and copper sheet thickness is 0.15-0.5mm, and copper sheet overlays on the electric insulation ceramics substrate, and ceramic substrate material is Al
2O
3Perhaps AlN, substrate thickness is at 0.5-1.5mm.
The temperature end diffusion impervious layer is between P type and N type thermoelectric material pin and the high-temperature soldering layer, and thickness is 5-40 μ m.
The low-temperature end diffusion impervious layer is between P type and thermoelectric pin of N type and the low-temperature end metal Ni layer, and thickness is 5-40 μ m.
Temperature end weld layer thickness is at 0.1-1mm.
Described thermoelectric pin is square or cylindrical.
The temperature end electrode that the present invention selects for use is MoCu alloy and CoSb
3The thermal coefficient of expansion of alloy is very approaching, and this is reduced to minimum with regard to having guaranteed when the long-time hot operation with the thermal stress at interface, has farthest prolonged the life-span of thermoelectric device.The temperature end Ag-Cu alloy weld tabs that adopts utilizes the fast characteristics of SPS programming rate to be connected with thermoelectric pin fast, has solved the shortcoming that general common weld tabs can not bear hot operation.As shown in Figure 5, temperature end ESEM at the interface shows that the interface does not have tangible crackle or micro-crack to occur in conjunction with good.
Description of drawings
Fig. 1 is the process schematic diagram of the thermoelectric pin of preparation, and Fig. 1 (a) is the thermoelectric cylinder block schematic diagram behind the SPS sintering, and Fig. 1 (b) is the thermoelectric pin schematic diagram of well cutting.
Fig. 2 is thermoelectric pin high temperature end face SPS welding process schematic diagram.Fig. 2 (a) is the preceding thermoelectric pin temperature end schematic cross-section of welding, Fig. 2 (b) is schematic cross-section after the sandblast, Fig. 2 (c) for end face spray diffusion impervious layer after, add Ag-Cu weld tabs schematic diagram, Fig. 2 (d) connects schematic cross-section behind Mo-Cu electrode and the thermoelectric pin fast for SPS.
Fig. 3 is the thermoelectric element structural representation for preparing.
Fig. 4 is the sem photograph in thermoelectric device low-temperature end cross section.
Fig. 5 is the sem photograph in thermoelectric device temperature end cross section.
Embodiment
Below by instantiation substantive distinguishing features of the present invention and obvious improvement are described.
The thermoelectric pin of the P type of well cutting and N type is at first roughly ground two end faces, carries out ultrasonic cleaning then in ethanol, then to the both ends of the surface plasma spraying, forms the Mo diffusion impervious layer (3) that thickness is about 30 μ m.P type and the thermoelectric pin of N type (4) are put into special mould, the Ag-Cu weld tabs (2) and the Mo-Cu electrode (1) of well cutting are put on the thermoelectric pin of mould successively, carrying out SPS connects, sintering pressure is 15MPa, heating rate is 200 ℃/min, 550 ℃ of insulations 30 seconds, and slowly cooling then, rate of temperature fall is controlled at 100 ℃/min, and the welding of temperature end electrode finishes.With the π type device that the begins to take shape Ni layer (6) of the about 20 μ m of vacuum sputtering thickness again on the Mo of low-temperature end diffusion impervious layer (3), be beneficial to better carry out soldering, adopt Sn-Pb scolder (7) that Cu sheet (8) on low-temperature end and the ceramic substrate is carried out soldering 180 ℃ of temperature then and be connected.The π type device interfaces that forms does not find that in conjunction with good crackle exists, and the test of temperature end shear strength is 19.24MPa, and it is used for thermoelectric device and is fine.
With with embodiment 1 in identical method and condition the thermoelectric pin of well cutting is handled and plasma spraying, P type and the thermoelectric pin of N type (4) are put into special mould, the Ag-Cu weld tabs (2) and the Mo-Cu electrode (1) of well cutting are put on the thermoelectric pin of mould successively, carry out SPS and connect, sintering pressure is 25MPa, and heating rate is 250 ℃/min, 550 ℃ of insulations 45 seconds, slowly cooling then, rate of temperature fall is controlled at 150 ℃/min, and the welding of temperature end electrode finishes.With the π type device that the begins to take shape Ni layer (6) of the about 30 μ m of vacuum sputtering thickness again on the Mo of low-temperature end diffusion impervious layer (3), be beneficial to better carry out soldering, adopt Sn-Pb scolder (7) that Cu sheet (8) on low-temperature end and the ceramic substrate is carried out soldering 180 ℃ of temperature then and be connected.The π type device interfaces that forms does not find that in conjunction with good crackle exists.
With with embodiment 1 in identical method and condition the thermoelectric pin of well cutting is handled, then to the both ends of the surface plasma spraying, form the W diffusion impervious layer (3) that thickness is about 20 μ m.P type and the thermoelectric pin of N type (4) are put into special mould, the Ag-Cu weld tabs (2) and the Mo-Cu electrode (1) of well cutting are put on the thermoelectric pin of mould successively, carrying out SPS connects, sintering pressure is 15MPa, heating rate is 250 ℃/min, 550 ℃ of insulations 60 seconds, and slowly cooling then, rate of temperature fall is controlled at 100 ℃/min, and the welding of temperature end electrode finishes.With the π type device that the begins to take shape Ni layer (6) of the about 25 μ m of vacuum sputtering thickness again on the Mo of low-temperature end layer, be beneficial to better carry out soldering, adopt Sn-Pb scolder (7) that Cu sheet (8) on low-temperature end and the ceramic substrate is carried out soldering 180 ℃ of temperature then and be connected.The π type device interfaces that forms does not find that in conjunction with good crackle exists.
Claims (10)
1. π type CoSb
3Based thermoelectric converting device is characterized in that described thermoelectric device is made up of Mo-Cu alloy electrode (1), temperature end weld layer (2), temperature end diffusion impervious layer (3), thermoelectric pin (4), low-temperature end diffusion impervious layer (5), low-temperature end metal Ni layer (6), low-temperature end weld layer (7) and low-temperature end electrode (8);
Wherein, 1. thermoelectric pin (4) is P type and N type CoSb
3Base thermoelectricity material, they are by temperature end weld layer (2) and Mo-Cu alloy electrode (1) the formation temperature end that fuses;
2. the P type then is connected with low-temperature end electrode (8) by low-temperature end metal level (6), low-temperature end weld layer (7) with the low-temperature end of the thermoelectric pin of N type;
3. the temperature end diffusion impervious layer is between P type and thermoelectric pin of N type and the temperature end weld layer;
4. the low-temperature end diffusion impervious layer is between P type and thermoelectric pin of N type and the low-temperature end metal Ni layer.
2. by the described π type of claim 1 CoSb
3Based thermoelectric converting device, the quality percentage composition that it is characterized in that Cu in the described Mo-Cu alloy electrode is 45%-60%, all the other are Mo and small amount of impurities element.
3. by the described π type of claim 1 CoSb
3Based thermoelectric converting device is characterized in that the diffusion impervious layer of described temperature end or low-temperature end is made up of at least a element of selecting among Mo, W, Ti, Nb and the Ta.
4. by claim 1 or 3 described described π type CoSb
3Based thermoelectric converting device is characterized in that the thickness of the diffusion impervious layer of described temperature end or low-temperature end is respectively 5-40 μ m.
5. by the described π type of claim 1 CoSb
3Based thermoelectric converting device is characterized in that described temperature end weld layer is an Ag-Cu alloy weld tabs, and wherein the quality percentage composition of Cu is 30%-60%, and surplus is Ag and small amount of impurities element.
6. by claim 1 or 6 described π type CoSb
3Based thermoelectric converting device is characterized in that temperature end thickness is 0.1-1mm.
7. by the described π type of claim 1 CoSb
3Based thermoelectric converting device is characterized in that described thermoelectric pin is square or cylindrical.
8. by the described π type of claim 1 CoSb
3Based thermoelectric converting device is characterized in that described low-temperature end electrode is a copper sheet, and thickness is between the 0.5-1.5mm, and copper sheet overlays on the electric insulation ceramics substrate, and substrate thickness is 0.5-1.5mm.
9. prepare π type CoSb as claimed in claim 1
3The method of based thermoelectric converting device is characterized in that concrete steps are:
A) utilize stripped sintering such as discharge to prepare the CoSb of P type and N type
3Base thermoelectric semiconductor, sintering parameter are vacuum degree 5-15Pa, and sintering pressure is 50-60MPa, and heating rate is 120-180 ℃/min, and sintering temperature is 580-600 ℃, is incubated 10-30min then;
B) thermoelectric block body that sinters of step a) requires to carry out the line cutting according to the device optimization design size, obtain the cylindrical or square thermoelectric pin of P type and N type, utilize sand-blast that two end face is handled then, make its end face obtain certain surface roughness, the ultrasonic impurity particle that cleans out end face;
C) at the CoSb of P type and N type
3A diffusion impervious layer that approaches on the plasma spraying on the both ends of the surface of base thermoelectric semiconductor, the parameter of plasma spraying is work arc voltage 75V, operating current 300A, spray is apart from 100mm, for powder amount 40g/min, for powder throughput 0.56m
3/ h;
D) Ag-Cu alloy weld tabs is written on the thermoelectric foot face diffusion impervious layer after the absolute ethyl alcohol cleaning, puts into then and CoSb
3The Mo-Cu alloy electrode that the base thermoelectricity material thermal coefficient of expansion is complementary, utilize the discharge plasma sintering to carry out rapid welding, parameters of welding is vacuum degree 5-15Pa, sintering pressure is 10-25MPa, heating rate is 200-250 ℃/min, be incubated 30-60 second at 550 ℃, slowly cooling then, rate of temperature fall is controlled at 80-150 ℃/min;
E) at the CoSb of P type and N type
3The low-temperature end of base thermoelectric semiconductor is electroplated on the barrier layer or the Ni layer of the about 30 μ m of vacuum sputtering one layer thickness, adopts the Sn-Pb scolder that Cu sheet on low-temperature end and the ceramic substrate is carried out soldering then and is connected, and is prepared into π type CoSb
3Based thermoelectric converting device.
10. by the described π type of claim 9 CoSb
3The preparation method of based thermoelectric converting device, it is characterized in that the Mo-Cu alloy electrode before the discharge plasma sintering in advance through blasting treatment, and ultrasonic removal surface impurity.
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| CN108461619A (en) * | 2018-06-01 | 2018-08-28 | 济南大学 | A kind of preparation method of Se doping skutterudite thermoelectric material |
| CN108461619B (en) * | 2018-06-01 | 2021-07-23 | 济南大学 | Preparation method of Se-doped skutterudite thermoelectric material |
| CN111211214A (en) * | 2020-01-09 | 2020-05-29 | 中国科学院上海硅酸盐研究所 | Interface barrier layer for half-heusler alloy thermoelectric material |
| CN113020736A (en) * | 2021-03-25 | 2021-06-25 | 哈尔滨工业大学 | Brazing connection method for skutterudite thermoelectric material and copper electrode |
| CN113020736B (en) * | 2021-03-25 | 2022-08-30 | 哈尔滨工业大学 | Brazing connection method for skutterudite thermoelectric material and copper electrode |
| CN113369623A (en) * | 2021-06-30 | 2021-09-10 | 哈尔滨工业大学（深圳） | Brazing connection method of half-heusler thermoelectric material with high service temperature |
| CN113369623B (en) * | 2021-06-30 | 2022-06-03 | 哈尔滨工业大学（深圳） | Brazing connection method of half-heusler thermoelectric material with high service temperature |
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