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Production method of Zintl phase monocrystal

A technology of Zinter phase and single crystal, applied in the field of Zinter phase single crystal thermoelectric material and its preparation, can solve the problems of uneconomical, high energy consumption and high reaction temperature, and achieve the effect of low energy consumption and cost

Inactive Publication Date: 2009-05-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature required by this method is high (1327°C), the requirements for the reaction vessel are high, and the energy consumption is also large, so it is uneconomical

Method used

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  • Production method of Zintl phase monocrystal
  • Production method of Zintl phase monocrystal
  • Production method of Zintl phase monocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 0.7g of high-purity elemental barium, 0.56g of manganese, 1.241g of antimony and 8.672g of tin in an argon-protected glove box according to Ba:Mn:Sb:Sn=1:2:2:14.3 (molar ratio). After weighing, put it in a corundum crucible with a volume of 5ml, cover a small amount of quartz wool, cover the above crucible with the same corundum crucible, then place it in a quartz tube, seal it with plastic wrap, remove it from the glove box, and vacuum it And wash several times with argon. The quartz tube was sealed under 1 / 5 atm argon protection. Finally, place the quartz tube in a muffle furnace, heat up to 1100 °C at a rate of 600 °C / h, and slowly cool down (2 °C / h) to 750 °C after 1 hour of heat preservation, then quickly take out the quartz tube and use a centrifuge (4000r / min speed) centrifugation. After the temperature dropped to room temperature, the quartz tube was put into an argon glove box and crushed, and the obtained product was washed with 0.1M hydrochloric acid...

Embodiment 2

[0035] Weigh 0.538g of high-purity elemental barium, 0.114g of strontium, 0.574g of manganese, 0.574g of manganese, and 1.273g and tin 8.873g. After weighing, put it in a corundum crucible with a volume of 5ml, cover a small amount of quartz wool, cover the above crucible with the same corundum crucible, then place it in a quartz tube, seal it with plastic wrap, remove it from the glove box, and vacuum it And wash several times with argon. The quartz tube was sealed under 1 / 5 atm argon protection. Finally, place the quartz tube in a muffle furnace, heat up to 1100 °C at a rate of 600 °C / h, and slowly cool down (2 °C / h) to 750 °C after 1 hour of heat preservation, then quickly take out the quartz tube and use a centrifuge (4000r / min speed) centrifugation. After the temperature dropped to room temperature, the quartz tube was put into an argon glove box and crushed, and the obtained product was washed with 0.1M hydrochloric acid to remove remaining tin to obtain Ba 0.75 Sr ...

Embodiment 3

[0039] Weigh high-purity elemental barium 0.479g, yttrium 0.259g, manganese 0.548g, antimony 1.214g and tin 8.463g. After weighing, put it in a corundum crucible with a volume of 5ml, cover a small amount of quartz wool, cover the above crucible with the same corundum crucible, then place it in a quartz tube, seal it with plastic wrap, remove it from the glove box, and vacuum it And wash several times with argon. The quartz tube was sealed under 1 / 5 atm argon protection. Finally, place the quartz tube in a muffle furnace, heat up to 1100 °C at a rate of 600 °C / h, and slowly cool down (2 °C / h) to 750 °C after 1 hour of heat preservation, then quickly take out the quartz tube and use a centrifuge (4000r / min speed) centrifugation. After the temperature dropped to room temperature, the quartz tube was put into an argon glove box and crushed, and the obtained product was washed with 0.1M hydrochloric acid to remove remaining tin to obtain Ba 0.7 Yb 0.3 mn 2 Sb 2 single crys...

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Abstract

The invention relates to a Zintl phase single crystal thermoelectric material and a preparation method thereof. The single crystal thermoelectric material comprises the following components: BaMn2Sb2, Ba1-xSrxMn2Sb2, Ba1-xYbxMn2Sb2, BaMn2-yZnySb2 and BaMn2Sb2-zGez (x is more than or equal to 0 and less than or equal to 1,y is more than or equal to 0 and less than or equal to 2, and z is more than or equal to 0 and less than or equal to 0.5) Ba0.75Sr0.25Mn2Sb2, Ba0.7Yb0.3Mn2Sb2, BaMn1.5Zn0.5Sb2 and BaMn2Sb1.5Ge0.5. The preparation method adopts a flux method. The method comprises the following steps: firstly weighing tin, manganese, antimony, barium and strontium, Yttrium, zinc or germanium for doping in a glove box, and adding the raw materials into a corundum crucible; then putting an inverted corundum crucible onto the corundum crucible containing the raw materials, filling a small amount of quartz wool between the two corundum crucibles, and putting the two corundum crucibles into a quartz tube; sealing the quartz tube through a preservative film and taking the quartz tube out of the glove box; carrying out vacuum pumping and repeatedly flushing the quartz tube with argon gas; and then sealing and welding the quartz tube and finally adopting a program temperature control furnace to prepare the single crystal. As the reaction temperature of the method is lower than that of a simple substance fusion method, the method is simpler and has less power consumption and lower cost.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a Zinter phase single crystal thermoelectric material and a preparation method thereof. Background technique [0002] Zintl compounds are narrow-band semiconductors with complex crystal structures. It usually refers to the positively charged alkaline earth metal (Ca, Sr, Ba) or divalent rare earth metal (such as Eu, Yb) atoms, transition metal (such as Mn, Zn, Nb) atoms or IIIA group metals (Al, Compounds composed of Ga, In) atoms and phosphorus (P, As, Sb, or Bi) atoms [S.M.KlauzLarich (Ed.). Chemistry, structure, and bonding of Zintl phase and ions. VCH publishers, Inc., New York , NY, 1996]. With the change of constituent atoms, the physical properties of Zintl compounds can change from semiconductor properties to large magnetoresistance, giant magnetoresistance, and ferromagnetism, so they have been extensively studied in the past ten years [J.Y.Chen, M.E.Wang, A.Rehr, S.M....

Claims

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Application Information

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IPC IPC(8): C30B11/00C30B29/10
Inventor 蔡克峰汪慧峰
Owner TONGJI UNIV
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