CN103172346A - Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction - Google Patents
Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction Download PDFInfo
- Publication number
- CN103172346A CN103172346A CN2013101069014A CN201310106901A CN103172346A CN 103172346 A CN103172346 A CN 103172346A CN 2013101069014 A CN2013101069014 A CN 2013101069014A CN 201310106901 A CN201310106901 A CN 201310106901A CN 103172346 A CN103172346 A CN 103172346A
- Authority
- CN
- China
- Prior art keywords
- powder
- purity
- granularity
- electric field
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Powder Metallurgy (AREA)
Abstract
The invention relates to a method for preparing a porous nano magnesium silicon based block body thermoelectric material by a hot press method in an electric field reaction, and belongs to the technical field of thermoelectric materials and preparation methods. The method is characterized in that the method for preparing the porous nano Mg2Si-based block body thermoelectric material by the hot press method in the electric field reaction realizes reactive synthesis and compact sintering of Mg2Si in one step, so that the method is simple in step, low in cost, and high in purity of products. Various doping substances are convenient to add, and the products have porous nano-structures. Sustained pollution to the products in a multi-step preparation method can be effectively avoided. Meanwhile, reaction and compact sintering are performed at the same time, so that the temperature and time required by the preparation of products are reduced, and grain coarsening is effectively inhibited. Under the effect of protective gases, reaction byproducts are gathered in grain boundary in the form of nanoholes, so that grain growth is further inhibited and phonon scattering is enhanced. The generated products are completely reacted, the grain size is less than 70nm, the sectional hole ratio is about 5-15%, and holes and the nanocrystals coexist to the benefit of reducing the heat conductivity of the products.
Description
Technical field
Electric field reactive hot pressing of the present invention prepares the method for the silica-based block thermoelectric material of porous nano magnesium, belongs to thermoelectric material and preparation method's technical field, is specifically related to a kind of employing electric field reactive hot pressing one step and prepares porous nano Mg
2the method of Si matrix body heat electric material, utilize the method a step to realize Mg
2the reaction of Si is synthesized and densification sintering, and product is the Mg that granularity is less than the structure of 70nm and contains certain nanoporous
2the Si base thermoelectricity material.The Mg that utilizes the method to prepare
2si matrix body heat electric material has the feature of porous and nanometer, contributes to obtain higher thermo-electric conversion performance.
Background technology
Current Mg
2the preparation method that Si is traditional utilizes the Mg powder of simple substance and Si powder direct reaction to form, or utilizes other method to make Mg
2after the Si powder, then carry out densification obtain block Mg in vacuum pressure stove or plasma agglomeration stove
2the Si thermoelectric material.The subject matter existed is: because the two fusing point differs larger, cause complicated process of preparation, and length consuming time, sintering later stage grain growth is serious.Utilize MgH
2after powder replaces pure Mg powder, can effectively fall the content that reduces MgO in product, reduce temperature of reaction to 350 ℃, after the replacement(metathesis)reaction of 15-20 hour, can obtain nano level Mg
2si powder, but inevitably again introduce impurity in the densification sintering process in later stage, and sintering temperature is 650-700 ℃, causes grain growth serious, seriously reduced Mg
2the thermoelectricity transmission performance of Si thermoelectric material.
Summary of the invention
Electric field reactive hot pressing of the present invention prepares the method for the silica-based block thermoelectric material of porous nano magnesium, and purpose is: in order to overcome above-mentioned technique, prepare Mg
2the deficiency of Si thermoelectric material, the present invention has designed a kind of electric field reactive hot pressing one step and has prepared porous nano Mg
2the method of Si block thermoelectric material, the method is conducive to overcome in traditional technology due to long reaction time, high product coarse grains and the high deficiency of MgO foreign matter content of causing of sintering temperature, a step makes nanometer Mg
2si matrix body material, in addition, be conducive to determine bundle effect inhibiting grain growth by crystal boundary by introduce a small amount of nanoporous to crystal boundary, and strengthen phon scattering by quantum well effect, further reduces thermal conductivity and improve thermoelectricity capability.
Electric field reactive hot pressing of the present invention prepares the method for the silica-based block thermoelectric material of porous nano magnesium, it is characterized in that a kind of employing electric field reactive hot pressing one step prepares porous nano Mg
2the method of Si matrix body heat electric material, the method is to carry out in the auxiliary synthetic furnace of electric field-activate pressure, additional industrial frequency AC electric field and uniaxial pressure are by promoting MgH
2interface close contact and the transport of substances of powder, nanometer Si powder, a small amount of Y powder and Bi powder, synchronously complete the sintering densification of chemical reaction and product powder, prepares the starting material MgH of this material
2the granularity of powder≤45 μ m, purity>=99.5%, granularity≤the 50nm of nanometer Si powder, purity>=99.90%, the granularity of rare earth metal y powder≤45 μ m, purity>=99.5%, the granularity of heavy metal Bi powder≤45 μ m, purity>=99.5%, the mole mixture ratio example is (2-x): (1-y): x:y(x≤0.01, y≤0.01), reactional equation is: (2-x) MgH
2si+yBi=the Mg of+xY+(1-y)
2-xy
xsi
1-ybi
y+ (2-x) H
2(1) (x≤0.01, y≤0.01), under the effect of additional inert protective gas, the by product H of generation
2slowly overflow, by reducing oxidation potential, prevent magnesian further formation, in the later stage sintering process, remaining hydrogen is gathered in crystal boundary gradually simultaneously, crystal boundary is played to pinning effect, main manifestations has changed pore surface curvature radius for the crystal boundary displacement produced when diffusing atom flows to pore by crystal boundary, and the chemical potential gradient that this radius-of-curvature the causes motivating force of grain growing just, when atom flows to crystal boundary by hole, just be presented as on inferior macroscopic view that grain growing is obstructed, concrete grammar and processing step are:
1) at first by the reactant MgH of granularity≤45 μ m and purity>=99.5%
2the heavy metal Bi powder of the rare earth metal y powder of the nanometer Si powder of powder, granularity≤50nm and purity>=99.90%, granularity≤45 μ m and purity>=99.5%, granularity≤45 μ m and purity>=99.5%, with (2-x): (1-y): the molar ratio of x:y mixes (x≤0.01, y≤0.01), assurance in ball milling 1-3 hour mixes, and forms mixed powder 9;
2) then mixed powder 9 is placed between the seaming chuck 6 and push-down head 7 of graphite jig 4; the graphite jig assembled is placed in to reaction cavity 3; with top electrode 2, with lower electrode 5, contact; be evacuated to below 10Pa; then pass into inert protective gas 11 by gas cylinder 12 in cavity, until in cavity, pressure reaches 10
5pa also keeps;
3) connect power frequency AC 10 unidirectional pressurization 1, realize synchronous reaction and sintering densification, it is 30-40 ℃/min that the powder heat-up rate is set, when temperature reaches 350 ℃, insulation 10-15 minute, to guarantee that powder fully reacts and carries out sintering, applies the pressure of 30MPa, after then continuing to be warming up to 450-550 ℃ in this process, apply the uniaxial pressure of 70-100MPa, insulation 5-10min, eventually sever power supply, sample furnace cooling after unloading.The preparation process technical process as shown in Figure 2.
The present invention is that a kind of beneficial effect for preparing the method for the silica-based block thermoelectric material of porous nano magnesium is: the method operation is simple, and cost is low, and resultant purity is high, the various dopants of convenient interpolation, and resultant has porous nanometer structure.The codope of transition metal Y and heavy metal Bi can improve the concentration of donor element, and then increases the quantity of current carrier, reaches the purpose of improving electrical property.Effectively avoided in multistep preparation method the chronic pollution to product.Simultaneously, reaction and sintering densification synchronously carry out, and have reduced product and have prepared needed temperature and time, effectively suppress grain coarsening.Under the shielding gas effect, byproduct of reaction is gathered in crystal boundary with the form of nano aperture, and further inhibiting grain growth also strengthens phon scattering.The product generated reacts completely, and grain-size is about 40nm, and the section hole ratio is about 5-15%, and co-existing in of hole and nanocrystal is conducive to reduce the product thermal conductivity.
The accompanying drawing explanation
Fig. 1 reaction unit fundamental diagram
1-impressed pressure 2-top electrode 3-reaction cavity 4-graphite jig 5-lower electrode 6-seaming chuck 7-push-down head 8-thermopair 9-reaction powder 10-power frequency AC 11-inert protective gas 12-gas cylinder
Fig. 2 preparation process process flow sheet
embodiment:
embodiment 1
By reactant MgH
2powder (granularity≤45 μ m, purity>=99.5%), nanometer Si powder (granularity≤50nm, purity>=99.90%), rare earth metal y powder (granularity≤45 μ m, purity>=99.5%) and heavy metal Bi powder (granularity≤45 μ m, purity>=99.5%) mole mixture ratio example is 1.995:0.995:0.005:0.005 (x=0.005, y=0.005), assurance in ball milling 1-3 hour mixes, form mixed powder 9, then mixed powder 9 is placed between the seaming chuck 6 and push-down head 7 of graphite jig 4, the graphite jig assembled is placed in to reaction cavity 3, with top electrode 2, with lower electrode 5, contact, be evacuated to below 10Pa, then pass into Ar shielding gas 11 by gas cylinder 12 in cavity, until in cavity, pressure reaches 10
5pa also keeps.Connect power frequency AC 10 unidirectional pressurization 1, realize synchronous reaction and sintering densification.It is 35 ℃/min that the powder heat-up rate is set, and when temperature reaches 350 ℃, is incubated 10 minutes, to guarantee that powder fully reacts and carries out sintering, applies the pressure of 30MPa, after then continuing to be warming up to 450 ℃ in this process, apply the uniaxial pressure of 70MPa, insulation 15min.The eventually sever power supply, sample furnace cooling after unloading.The product generated reacts completely, and dense structure's degree is 75.3%, the about 40nm of grain-size.
By reactant MgH
2powder (granularity≤45 μ m, purity>=99.5%), nanometer Si powder (granularity≤50nm, purity>=99.90%), rare earth metal y powder (granularity≤45 μ m, purity>=99.5%) and heavy metal Bi powder (granularity≤45 μ m, purity>=99.5%) mole mixture ratio example is 1.995:0.099:0.005:0.01 (x=0.005, y=0.01), assurance in ball milling 1-3 hour mixes, form mixed powder 9, then mixed powder 9 is placed between the seaming chuck 6 and push-down head 7 of graphite jig 4, the graphite jig assembled is placed in to reaction cavity 3, with top electrode 2, with lower electrode 5, contact, be evacuated to below 10Pa, then pass into He shielding gas 11 by gas cylinder 12 in cavity, until in cavity, pressure reaches 10
5pa also keeps.Connect power frequency AC 10 unidirectional pressurization 1, realize synchronous reaction and sintering densification.It is 40 ℃/min that the powder heat-up rate is set, and when temperature reaches 350 ℃, is incubated 15 minutes, to guarantee that powder fully reacts and carries out sintering, applies the pressure of 30MPa, after then continuing to be warming up to 550 ℃ in this process, apply the uniaxial pressure of 70MPa, insulation 15min.The eventually sever power supply, sample furnace cooling after unloading.The product generated reacts completely, and dense structure's degree is 91.5%, the about 53nm of grain-size.
By reactant MgH
2powder (granularity≤45 μ m, purity>=99.5%), nanometer Si powder (granularity≤50nm, purity>=99.90%), rare earth metal y powder (granularity≤45 μ m, purity>=99.5%) and heavy metal Bi powder (granularity≤45 μ m, purity>=99.5%) mole mixture ratio example is 1.99:0.99:0.01:0.01 (x=0.01, y=0.01), assurance in ball milling 1-3 hour mixes, form mixed powder 9, then mixed powder 9 is placed between the seaming chuck 6 and push-down head 7 of graphite jig 4, the graphite jig assembled is placed in to reaction cavity 3, with top electrode 2, with lower electrode 5, contact, be evacuated to below 10Pa, then pass into 50%Ar+50%He shielding gas 11 by gas cylinder 12 in cavity, until in cavity, pressure reaches 10
5pa also keeps.Connect power frequency AC 10 unidirectional pressurization 1, realize synchronous reaction and sintering densification.It is 40 ℃/min that the powder heat-up rate is set, and when temperature reaches 350 ℃, is incubated 15 minutes, to guarantee that powder fully reacts and carries out sintering, applies the pressure of 30MPa, after then continuing to be warming up to 550 ℃ in this process, apply the uniaxial pressure of 100MPa, insulation 10min.The eventually sever power supply, sample furnace cooling after unloading.The product generated reacts completely, and dense structure's degree is 99.2%, the about 67nm of grain-size.
Claims (1)
1. the electric field reactive hot pressing prepares the method for the silica-based block thermoelectric material of porous nano magnesium, it is characterized in that a kind of employing electric field reactive hot pressing one step prepares porous nano Mg
2the method of Si matrix body heat electric material, the method is to carry out in the auxiliary synthetic furnace of electric field-activate pressure, additional industrial frequency AC electric field and uniaxial pressure are by promoting MgH
2interface close contact and the transport of substances of powder, nanometer Si powder, a small amount of Y powder and Bi powder, synchronously complete the sintering densification of chemical reaction and product powder, prepares the starting material MgH of this material
2the granularity of powder≤45 μ m, purity>=99.5%, granularity≤the 50nm of nanometer Si powder, purity>=99.90%, the granularity of rare earth metal y powder≤45 μ m, purity>=99.5%, the granularity of heavy metal Bi powder≤45 μ m, purity>=99.5%, the mole mixture ratio example is (2-x): (1-y): x:y(x≤0.01, y≤0.01), reactional equation is: (2-x) MgH
2si+yBi=the Mg of+xY+(1-y)
2-xy
xsi
1-ybi
y+ (2-x) H
2(1) (x≤0.01, y≤0.01), under the effect of additional inert protective gas, the by product H of generation
2slowly overflow, by reducing oxidation potential, prevent magnesian further formation, in the later stage sintering process, remaining hydrogen is gathered in crystal boundary gradually simultaneously, and crystal boundary is played to pinning effect, and the crystal boundary displacement produced when diffusing atom flows to pore by crystal boundary has changed pore surface curvature radius, and the chemical potential gradient that this radius-of-curvature the causes motivating force of grain growing just, when atom flows to crystal boundary by hole, just be presented as on inferior macroscopic view that grain growing is obstructed, concrete grammar and processing step are:
1) at first by the reactant MgH of granularity≤45 μ m and purity>=99.5%
2the heavy metal Bi powder of the rare earth metal y powder of the nanometer Si powder of powder, granularity≤50nm and purity>=99.90%, granularity≤45 μ m and purity>=99.5%, granularity≤45 μ m and purity>=99.5%, with (2-x): (1-y): the molar ratio of x:y mixes (x≤0.01, y≤0.01), assurance in ball milling 1-3 hour mixes, and forms mixed powder 9;
2) then mixed powder (9) is placed between the seaming chuck (6) and push-down head (7) of graphite jig (4); the graphite jig assembled is placed in to reaction cavity (3); with top electrode (2), with lower electrode (5), contact; be evacuated to below 10Pa; then pass into inert protective gas (11) by gas cylinder (12) in cavity, until in cavity, pressure reaches 10
5pa also keeps;
3) connect power frequency AC (10) unidirectional pressurization (1), realize synchronous reaction and sintering densification, powder is set and heats up, speed is 30-40 ℃/min, when temperature reaches 350 ℃, insulation 10-15 minute, fully react and carry out sintering to guarantee powder, apply the pressure of 30MPa in this process, then after continuing to be warming up to 450-550 ℃, apply the uniaxial pressure of 70-100MPa, insulation 5-10min, the eventually sever power supply, sample furnace cooling after unloading.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310106901.4A CN103172346B (en) | 2013-03-29 | 2013-03-29 | Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310106901.4A CN103172346B (en) | 2013-03-29 | 2013-03-29 | Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103172346A true CN103172346A (en) | 2013-06-26 |
| CN103172346B CN103172346B (en) | 2014-06-11 |
Family
ID=48632624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310106901.4A Expired - Fee Related CN103172346B (en) | 2013-03-29 | 2013-03-29 | Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103172346B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109770A (en) * | 2014-07-18 | 2014-10-22 | 太原理工大学 | Method for preparing Mg2SixSn[1-x]Biy-base thermoelectric material by microwave-assisted MgH2 solid reaction process |
| CN106694891A (en) * | 2016-11-15 | 2017-05-24 | 上海电机学院 | Ball milling electric field pressure-assisted sintering remanufacturing method and device of titanium chips |
| CN106825585A (en) * | 2016-11-15 | 2017-06-13 | 上海电机学院 | Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured |
| CN106913582A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院上海硅酸盐研究所 | A kind of magnesium silicide nano material and its preparation method and application |
| CN108695429A (en) * | 2017-03-31 | 2018-10-23 | 丰田自动车株式会社 | Thermo-electric converting material and its manufacturing method |
| CN108963064A (en) * | 2017-12-28 | 2018-12-07 | 中国科学院物理研究所 | Hot pressed sintering device, the block thermoelectric material of micro-nano porous structure and its preparation method |
| CN109534385A (en) * | 2018-11-06 | 2019-03-29 | 武汉理工大学 | A kind of Fu Nakong silver sulfide and its fast preparation method |
| CN110116206A (en) * | 2019-04-22 | 2019-08-13 | 武汉科技大学 | A kind of dedicated AC power frequency discharge sintering equipment of thermoelectric material and sintering method |
| CN110892537A (en) * | 2017-08-15 | 2020-03-17 | 三菱综合材料株式会社 | Magnesium-based thermoelectric conversion material, magnesium-based thermoelectric conversion element, and method for producing magnesium-based thermoelectric conversion material |
| CN112614929A (en) * | 2021-01-05 | 2021-04-06 | 哈尔滨工业大学 | Method for constructing grain boundary holes to improve SnTe thermoelectric performance |
| CN117645301A (en) * | 2024-01-30 | 2024-03-05 | 山东硅纳新材料科技有限公司 | High-purity submicron-order Mg 2 Si preparation method and continuous vacuum rotary kiln |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530957A (en) * | 2011-12-14 | 2012-07-04 | 太原理工大学 | Method for preparing nano Mg2-xSiREx thermoelectric material |
-
2013
- 2013-03-29 CN CN201310106901.4A patent/CN103172346B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530957A (en) * | 2011-12-14 | 2012-07-04 | 太原理工大学 | Method for preparing nano Mg2-xSiREx thermoelectric material |
Non-Patent Citations (1)
| Title |
|---|
| 周琦等: "《高能球磨过程中Mg2Si的形成及其影响因素的研究》", 《兰州理工大学学报》 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109770B (en) * | 2014-07-18 | 2016-05-11 | 太原理工大学 | Microwave is assisted MgH2Solid reaction process is prepared Mg2SixSn1-xBiyThe method of base thermoelectricity material |
| CN104109770A (en) * | 2014-07-18 | 2014-10-22 | 太原理工大学 | Method for preparing Mg2SixSn[1-x]Biy-base thermoelectric material by microwave-assisted MgH2 solid reaction process |
| CN106913582A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院上海硅酸盐研究所 | A kind of magnesium silicide nano material and its preparation method and application |
| CN106694891A (en) * | 2016-11-15 | 2017-05-24 | 上海电机学院 | Ball milling electric field pressure-assisted sintering remanufacturing method and device of titanium chips |
| CN106825585A (en) * | 2016-11-15 | 2017-06-13 | 上海电机学院 | Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured |
| CN108695429A (en) * | 2017-03-31 | 2018-10-23 | 丰田自动车株式会社 | Thermo-electric converting material and its manufacturing method |
| CN108695429B (en) * | 2017-03-31 | 2022-06-03 | 丰田自动车株式会社 | Thermoelectric conversion material and method for producing same |
| CN110892537A (en) * | 2017-08-15 | 2020-03-17 | 三菱综合材料株式会社 | Magnesium-based thermoelectric conversion material, magnesium-based thermoelectric conversion element, and method for producing magnesium-based thermoelectric conversion material |
| CN110892537B (en) * | 2017-08-15 | 2023-11-07 | 三菱综合材料株式会社 | Magnesium thermoelectric conversion material, magnesium thermoelectric conversion element, and method for producing magnesium thermoelectric conversion material |
| CN108963064A (en) * | 2017-12-28 | 2018-12-07 | 中国科学院物理研究所 | Hot pressed sintering device, the block thermoelectric material of micro-nano porous structure and its preparation method |
| CN108963064B (en) * | 2017-12-28 | 2019-11-29 | 中国科学院物理研究所 | Hot pressed sintering device, the block thermoelectric material of micro-nano porous structure and its preparation method |
| CN109534385B (en) * | 2018-11-06 | 2020-11-06 | 武汉理工大学 | Nano-pore-rich silver sulfide and rapid preparation method thereof |
| CN109534385A (en) * | 2018-11-06 | 2019-03-29 | 武汉理工大学 | A kind of Fu Nakong silver sulfide and its fast preparation method |
| CN110116206A (en) * | 2019-04-22 | 2019-08-13 | 武汉科技大学 | A kind of dedicated AC power frequency discharge sintering equipment of thermoelectric material and sintering method |
| CN112614929A (en) * | 2021-01-05 | 2021-04-06 | 哈尔滨工业大学 | Method for constructing grain boundary holes to improve SnTe thermoelectric performance |
| CN117645301A (en) * | 2024-01-30 | 2024-03-05 | 山东硅纳新材料科技有限公司 | High-purity submicron-order Mg 2 Si preparation method and continuous vacuum rotary kiln |
| CN117645301B (en) * | 2024-01-30 | 2024-04-02 | 山东硅纳新材料科技有限公司 | High-purity submicron-order Mg 2 Si preparation method and continuous vacuum rotary kiln |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103172346B (en) | 2014-06-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103172346B (en) | Method for preparing porous nano magnesium silicon based block body thermoelectric material by hot press method in electric field reaction | |
| CN101973532B (en) | Method for preparing nano aluminum nitride powder | |
| CN102674270A (en) | Method for preparing Cu2Se thermoelectric material by low-temperature solid-phase reaction | |
| CN103588182B (en) | A kind of preparation method of spherical aluminum nitride powder | |
| WO2014097963A1 (en) | Zinc oxide-based transparent conductive film | |
| JP2009541193A (en) | Apparatus and method for producing semiconductor grade silicon | |
| CN109796209A (en) | One kind (Ti, Zr, Hf, Ta, Nb) B2High entropy ceramic powder and preparation method thereof | |
| CN102502539A (en) | Method for preparing yttrium-doped nano aluminum nitride powder | |
| Wieg et al. | Visible photoluminescence in polycrystalline terbium doped aluminum nitride (Tb: AlN) ceramics with high thermal conductivity | |
| CN101786165B (en) | Method for synthesizing Nb/Nb5Si3 composite materials at high temperature through microwave induced self propagating | |
| CN110204341A (en) | One kind (Hf, Ta, Nb, Ti) B2High entropy ceramic powder and preparation method thereof | |
| JP5881066B2 (en) | Thermoelectric conversion element and thermoelectric conversion module | |
| Zhao et al. | Transformation of waste crystalline silicon into submicro β-SiC by multimode microwave sintering with low carbon emissions | |
| Zhang et al. | Enhanced thermoelectric performance of 3D-printed Bi2Te3-based materials via adding Te/Se | |
| CN106672988A (en) | Preparation method of high purity rare earth boride | |
| CN103320636B (en) | Novel method for quickly preparing high-performance Mg2Si0.3Sn0.7-based thermoelectric material | |
| Ebadzadeh et al. | Microwave hybrid synthesis of silicon carbide nanopowders | |
| CN107353012A (en) | A kind of composite thermoelectric material and preparation method thereof | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| JP2014019584A (en) | Lanthanum hexaboride sintered body, production method thereof, lanthanum hexaboride film and organic semiconductor device | |
| CN104404284A (en) | Method for rapid preparation of high performance AgBiSe2 block thermoelectric material | |
| CN107399972A (en) | A kind of method that transparent aluminium nitride ceramic is prepared based on SPS methods | |
| JP2011116575A (en) | Method for producing magnesium silicide, magnesium silicide, electrode member and thermoelectric element | |
| Kim et al. | Fabrication of silicide-based thermoelectric nanocomposites: a review | |
| CN102530957B (en) | Method for preparing nano Mg2-xSiREx thermoelectric material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140611 |