CN102925729A - Method of preparing n-type counterfeit ternary erbium-doped thermoelectric material by utilizing mechanical alloying cold pressing sintering method - Google Patents
Method of preparing n-type counterfeit ternary erbium-doped thermoelectric material by utilizing mechanical alloying cold pressing sintering method Download PDFInfo
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- CN102925729A CN102925729A CN2012103184883A CN201210318488A CN102925729A CN 102925729 A CN102925729 A CN 102925729A CN 2012103184883 A CN2012103184883 A CN 2012103184883A CN 201210318488 A CN201210318488 A CN 201210318488A CN 102925729 A CN102925729 A CN 102925729A
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Abstract
The invention discloses a method of preparing an n-type counterfeit ternary erbium-doped thermoelectric material by utilizing a mechanical alloying cold pressing sintering method, and relates to a method of preparing a thermoelectric material. The invention solves the technical problems of easiness in separation, poor mechanical property and high material cost of the conventional thermoelectric material. The method comprises the following steps of: 1, mixing a simple substance Bi, a simple substance Sb, a simple substance Te and a simple substance Se, adding a rare earth element Er, and ball-milling to obtain alloy powder; 2, cold-pressing the alloy powder to a block at room temperature; 3, placing the cold-pressing block obtained in the step 2 into a high-temperature-resistant glass tube, sintering, and cooling to room temperature along with a furnace so as to obtain the n-type counterfeit ternary erbium-doped thermoelectric material. The material, prepared by the method in the invention, has a thermoelectromotive force rate close to an oriented crystal, according to the national departmental standard, the Seebeck coefficient of the material is tested to reach 200 muVK<-1>, the conductivity is 55 omega<-1>cm<-1>, and a power factor is close to 2 muWcm<-1>K<-2>.
Description
Technical field
The present invention relates to a kind of method for preparing thermoelectric material.
Background technology
Thermoelectric material is a kind of novel refrigerating material, compares with traditional mechanical refrigeration, it has, and size is little, lightweight, friction, without significant advantage such as refrigeration agents, be applied to a lot of fields such as frigistor, temperature-sensitive device and electric heating heap.N-shaped Bi, Sb, Te alloy are thermoelectricity and the magneto-electric functional materials of excellent performance, are the important materials of the solid-state electric refrigeration device of preparation and magnetoelectricity device.Bi
2Te
3Compound and sosoloid thereof are a kind of thermoelectric materials that at room temperature has higher figure of merit, are widely used in thermoelectric (al) cooling based on thermoelectricity capability excellent under the room temperature.Its preparation method is main crystal pulling method, vacuum melting method and the Bridgman method etc. of adopting at present.These methods require raw metal purity high, and production cost is high, the production cycle is long, and the product that makes has very strong anisotropy, easily along c-axis cleavage fracture, in materials processing spillage of material serious, bad mechanical property makes the reliability reduction of thermo-electric device.
Summary of the invention
The present invention provides a kind of method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering in order to solve the existing easy splitting of thermoelectric material, bad mechanical property, technical problem that the device production cost is high.
The method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering is as follows:
One, press the Bi element, the Sb element, Te element and Se element mol ratio are 180: 2: 285: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, with simple substance Bi, simple substance Sb, simple substance Te and simple substance Se mix, then add rare earth element er, get mixture, the add-on of rare earth element er is simple substance Bi, simple substance Sb, simple substance Te, 0.1%～2.0% of simple substance Se and rare earth element er total mass, it is 1mm～10mm that mixture is crushed to particle diameter, take sherwood oil as ball-milling medium, be 410r/min at rotating speed, ratio of grinding media to material is under 10: 1 the condition, mechanical ball milling 100h obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 6mm～9mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min～2h under 350 ℃～500 ℃ condition cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
The purity of the Bi of simple substance described in the step 1 is 99.99%.The purity of the Sb of simple substance described in the step 1 is 99.99%.The purity of the Te of simple substance described in the step 1 is 99.99%.The purity of the Se of simple substance described in the step 1 is 99.99%.The purity of the Er of simple substance described in the step 1 is 99.99%.
The invention has the advantages that:
1, the inventive method can at room temperature realize the chemical combination of element, prepares alloy ultrafine powder material, and obtaining other technology can not getable weave construction.
2, the good counterfeit ternary thermoelectric material of mechanical property of the present invention's preparation can effectively reduce the splitting phenomenon of thermoelectric material in cutting process, thereby the one-tenth of decrease device produces cost.
3, it is favourable for the thermal conductivity that reduces material that the inventive method prepares the crystal boundary and the hole that produce in the materials process, and sintering process can make crystal boundary move, be conducive to reduce the porosity of material, increase the density of material, improve the scattering mechanism of current carrier, thereby be conducive to improve the specific conductivity of material; In addition, the doping of rare earth Er can change the energy band structure of material, increases band gap width, is conducive to improve the Seebeck coefficient of material.The material of the inventive method preparation has the thermoelectric power close with oriented crystal, tests its its Seebeck coefficient optimum value with reference to national ministerial standard and can reach 200 μ VK
-1, the specific conductivity optimum value is 55 Ω
-1Cm
-1, power factor is near 2 μ Wcm
-1K
-2
4, preparation technology's flow process of the present invention is simple, and is low to the equipment and process conditional request, and easy handling can obviously reduce the production cost of material.
5, the present invention can avoid material under molten state because the volatilization of Bi and Te element causes the problem that the material composition segregation causes material property to reduce.
Description of drawings
Fig. 1 is that the XRD figure for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering of experiment one and experiment two preparations is composed, the XRD figure for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering that A represents to test a preparation among the figure is composed, B represents to test the XRD figure for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering of two preparations and composes, ◆ expression Er
Expression Er
2Se
3
Fig. 2 is that the block magnification of colding pressing of step 2 gained in the experiment three is 20.0K SEM photo doubly;
Fig. 3 is that the block of colding pressing of step 2 gained is 20.0K SEM photo doubly through the 400 ℃ of counterfeit ternary er-doped of sintering gained N-shaped thermoelectric material magnifications in the experiment three;
Fig. 4 is that the block of colding pressing of step 2 gained is 20.0K SEM photo doubly through the 450 ℃ of counterfeit ternary er-doped of sintering gained N-shaped thermoelectric material magnifications in the experiment three;
Fig. 5 is that the block of colding pressing of step 2 gained is 20.0K SEM photo doubly through the 500 ℃ of counterfeit ternary er-doped of sintering gained N-shaped thermoelectric material magnifications in the experiment three.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment prepares the counterfeit ternary er-doped of N-shaped thermoelectric material ((Bi with the mechanical alloying cold sintering
2Te
3)
0.90(Sb
2Te
3)
0.05(Sb
2Se
3)
0.05) method as follows:
One, press the Bi element, the Sb element, Te element and Se element mol ratio are 180: 2: 285: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, with simple substance Bi, simple substance Sb, simple substance Te and simple substance Se mix, then add rare earth element er, get mixture, the add-on of rare earth element er is simple substance Bi, simple substance Sb, simple substance Te, 0.1%～2.0% of simple substance Se and rare earth element er total mass, it is 1mm～10mm that mixture is crushed to particle diameter, take sherwood oil as ball-milling medium, be 410r/min at rotating speed, ratio of grinding media to material is under 10: 1 the condition, mechanical ball milling 100h obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 6mm～9mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min～2h under 350 ℃～500 ℃ condition cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
Used ball mill is QM-1SP-CL type planetary ball mill in the present embodiment.
Embodiment two: present embodiment and embodiment one are different is that the purity of the Bi of simple substance described in the step 1 is 99.99%.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two is that the purity of the Sb of simple substance described in the step 1 is 99.99%.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three is that the purity of the Te of simple substance described in the step 1 is 99.99%.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four is that the purity of the Se of simple substance described in the step 1 is 99.99%.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five is that the purity of the Er of simple substance described in the step 1 is 99.99%.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six is that the add-on of rare earth element er described in the step 1 is 0.5% of simple substance Bi, simple substance Sb, simple substance Te, simple substance Se and rare earth element er total mass.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to six is that the add-on of rare earth element er described in the step 1 is 1.52% of simple substance Bi, simple substance Sb, simple substance Te, simple substance Se and rare earth element er total mass.Other is identical with one of embodiment one to six.
Embodiment nine: present embodiment is different from one of embodiment one to six be in the step 3 under 380 ℃～480 ℃ condition sintering.Other is identical with one of embodiment one to six.
Embodiment ten: present embodiment is different from one of embodiment one to six be in the step 3 under 400 ℃ condition sintering.Other is identical with one of embodiment one to six.
Adopt following experimental verification effect of the present invention:
Experiment one:
The method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering is as follows:
One, according to chemical formula (Bi
2Te
3)
0.90(Sb
2Te
3)
0.05(Sb
2Se
3)
0.05Be 180: 2: 285 in Bi element, Sb element, Te element and Se element mol ratio: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, simple substance Bi, simple substance Sb, simple substance Te and simple substance Se are mixed, then add rare earth element er, get mixture, the add-on of rare earth element er is 0.1% of simple substance Bi, simple substance Sb, simple substance Te, simple substance Se and rare earth element er total mass, it is 1mm that mixture is crushed to particle diameter, obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 6mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min～8h under 350 ℃ condition cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
Experiment two:
The method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering is as follows:
One, according to chemical formula (Bi
2Te
3)
0.90(Sb
2Te
3)
0.05(Sb
2Se
3)
0.05Press the Bi element, the Sb element, Te element and Se element mol ratio are 180: 2: 285: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, with simple substance Bi, simple substance Sb, simple substance Te and simple substance Se mix, then add rare earth element er, get mixture, the add-on of rare earth element er is simple substance Bi, simple substance Sb, simple substance Te, 0.1% of simple substance Se and rare earth element er total mass, it is 1mm that mixture is crushed to particle diameter, take sherwood oil as ball-milling medium, be 410r/min at rotating speed, ratio of grinding media to material is under 10: 1 the condition, mechanical ball milling 100h obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 6mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min～8h under 350 ℃ condition cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
By Fig. 1 and Fig. 2 contrast as can be known, the diffraction peak-to-peak among Fig. 2 decreases by force, and peak shape is broadening slightly also, and finds the growth along with Ball-milling Time, and the simple substance peak of Er disappears, and Er is arranged
2Se
3And Er
2Te
3Compound occurs, 331 peaks, 400 peak Er
2Se
3Compound peak value, and Er
2Te
3The variation at peak is not fairly obvious, along with Ball-milling Time increases, simple substance Er will with counterfeit ternary crystal in element chemical combination constantly occurs, and the explanation alloying needs higher energy, may enter Bi with the Er atom
2Te
3The mechanism of the inner formation of lattice dot matrix intercalation compound is relevant.
Experiment three:
The method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering is as follows:
One, according to chemical formula (Bi
2Te
3)
0.90(Sb
2Te
3)
0.05(Sb
2Se
3)
0.05Press the Bi element, the Sb element, Te element and Se element mol ratio are 180: 2: 285: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, with simple substance Bi, simple substance Sb, simple substance Te and simple substance Se mix, then add rare earth element er, get mixture, the add-on of rare earth element er is simple substance Bi, simple substance Sb, simple substance Te, 0.5% of simple substance Se and rare earth element er total mass, it is 10mm that mixture is crushed to particle diameter, take sherwood oil as ball-milling medium, be 410r/min at rotating speed, ratio of grinding media to material is under 10: 1 the condition, mechanical ball milling 100h obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 9mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min under 400 ℃, 450 ℃, 500 ℃ condition respectively cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
Can find out the block slabbing structure of colding pressing among Fig. 3, and step structure is arranged, the space is larger between particle and the particle, skewness.
Along with the rising of sintering temperature, can obviously find out more homogenizing of laminate structure among Fig. 4 and Fig. 5, along with crystal grain is grown up gradually, particle and particle are linked to be sheet, and between the space reduce, be evenly distributed.This is that adhesive surface enlarges makes granular boundary change grain boundary into, forms laminate structure because in sintering process, temperature action is so that the thermal motion of atom aggravates, and polymerization between the more atom forms adhesive surface.
Claims (10)
1. the method for preparing the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the method that it is characterized in that preparing with the mechanical alloying cold sintering the counterfeit ternary er-doped of N-shaped thermoelectric material is as follows:
One, press the Bi element, the Sb element, Te element and Se element mol ratio are 180: 2: 285: 15 ratio takes by weighing simple substance Bi, simple substance Sb, simple substance Te and simple substance Se, with simple substance Bi, simple substance Sb, simple substance Te and simple substance Se mix, then add rare earth element er, get mixture, the add-on of rare earth element er is simple substance Bi, simple substance Sb, simple substance Te, 0.1%～2.0% of simple substance Se and rare earth element er total mass, it is 1mm～10mm that mixture is crushed to particle diameter, take sherwood oil as ball-milling medium, be 410r/min at rotating speed, ratio of grinding media to material is under 10: 1 the condition, mechanical ball milling 100h obtains alloy powder;
Two, be that the condition of 170MPa, room temperature depresses to diameter and is 10mm, highly is the cylindrical cold briquetting body of 6mm～9mm with alloy powder at pressure;
Three, the block of colding pressing that step 2 is obtained is put into high-temperature resistant glass tube, is evacuated to 10
-3Pa, sealing, then sintering 30min～2h under 350 ℃～500 ℃ condition cools to room temperature with the furnace, namely gets the counterfeit ternary er-doped of N-shaped thermoelectric material.
2. describedly according to claim 1 prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the purity that it is characterized in that the Bi of simple substance described in the step 1 is 99.99%.
3. describedly according to claim 1 prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the purity that it is characterized in that the Sb of simple substance described in the step 1 is 99.99%.
4. describedly according to claim 1 prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the purity that it is characterized in that the Te of simple substance described in the step 1 is 99.99%.
5. describedly according to claim 1 prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the purity that it is characterized in that the Se of simple substance described in the step 1 is 99.99%.
6. describedly according to claim 1 prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the purity that it is characterized in that the Er of simple substance described in the step 1 is 99.99%.
7. according to claim 1,2,3,4,5 or 6 describedly prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the add-on that it is characterized in that rare earth element er described in the step 1 is 0.5% of simple substance Bi, simple substance Sb, simple substance Te, simple substance Se and rare earth element er total mass.
8. according to claim 1,2,3,4,5 or 6 describedly prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, the add-on that it is characterized in that rare earth element er described in the step 1 is 1.52% of simple substance Bi, simple substance Sb, simple substance Te, simple substance Se and rare earth element er total mass.
9. according to claim 1,2,3,4,5 or 6 describedly prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, it is characterized in that in the step 3 sintering under 380 ℃～480 ℃ condition.
10. according to claim 1,2,3,4,5 or 6 describedly prepare the method for the counterfeit ternary er-doped of N-shaped thermoelectric material with the mechanical alloying cold sintering, it is characterized in that in the step 3 sintering under 400 ℃ condition.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167486A (en) * | 2014-07-23 | 2014-11-26 | 宁波工程学院 | N-type medium-high-temperature pseudo binary thermoelectric alloy and preparation technology thereof |
| CN111848165A (en) * | 2020-08-03 | 2020-10-30 | 深圳见炬科技有限公司 | P-type bismuth telluride thermoelectric material and preparation method thereof |
| CN113285010A (en) * | 2021-04-20 | 2021-08-20 | 哈尔滨石油学院 | High-pressure preparation method of Er-doped bismuth telluride-based pseudo ternary thermoelectric material |
-
2012
- 2012-08-31 CN CN2012103184883A patent/CN102925729A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 曹显莹: "赝三元机械合金化掺Er热电材料的制备与性能研究", 《中国优秀硕士学位论文全文数据库 基础科学辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167486A (en) * | 2014-07-23 | 2014-11-26 | 宁波工程学院 | N-type medium-high-temperature pseudo binary thermoelectric alloy and preparation technology thereof |
| CN104167486B (en) * | 2014-07-23 | 2016-08-24 | 宁波工程学院 | High temperature pseudo-binary electrothermal alloy and preparation technology thereof in a kind of n-type |
| CN111848165A (en) * | 2020-08-03 | 2020-10-30 | 深圳见炬科技有限公司 | P-type bismuth telluride thermoelectric material and preparation method thereof |
| CN113285010A (en) * | 2021-04-20 | 2021-08-20 | 哈尔滨石油学院 | High-pressure preparation method of Er-doped bismuth telluride-based pseudo ternary thermoelectric material |
| CN113285010B (en) * | 2021-04-20 | 2023-04-18 | 哈尔滨石油学院 | High-pressure preparation method of Er-doped bismuth telluride-based pseudo-ternary thermoelectric material |
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Application publication date: 20130213 |