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Mercury-tellurium compound containing transition metal complex ions and hydrazine-aided preparation method thereof

A tellurium compound and transition metal technology, applied in the field of mercury-tellurium compound and hydrazine-assisted preparation, can solve the problem of no mercury-tellurium compound and the like, and achieve the effects of simple synthesis method, convenient product separation and purification, and lower reaction temperature

Active Publication Date: 2017-06-16
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no research reports on the synthesis of mercury tellurium compounds using hydrazine as a reaction medium and reducing agent at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment one: [Mn(trien)(N 2 h 4 ) 2 ]Hg 2 Te 4

[0048] MnCl 2 (0.031 g, 0.25 mmol), HgCl 2 (0.136 g, 0.50 mmol) and Te (0.255 g, 2 mmol) were added to 2.0 ml of hydrazine (N 2 h 4 ) and 1.0 ml of triethylenetetramine (trien) mixed solution, stirred for 10 minutes, put the mixture into a polytetrafluoroethylene-lined stainless steel reactor, and reacted at 100° C. for 5 days. After cooling to room temperature, black crystals were precipitated, filtered, washed with 5 ml of ethanol and acetone, and dried in vacuo to obtain 0.182 g of crystals with a yield of 62%. Elemental analysis: C 5.93, H 2.15, N 9.38%; theoretical value: C 6.12, H 2.23, N 9.52%. Infrared absorption spectrum data (KBr, cm -1 ): 3455(s), 3250(m), 2943(m), 2867(m), 1719(w), 1635(w), 1564(w), 1458(m), 1383(m), 1315(m ),1173(w),1135(w),1080(s),1004(s),946(s),883(s),816(s),706(w),592(s),483(s ), 429(m), 410(w). Solid State Absorption Spectrometry: Semiconductor Energy Gap E g = 0.84eV.

Embodiment 2

[0049] Embodiment two: [Zn(trien)(N 2 h 4 ) 2 ]Hg 2 Te 4

[0050] ZnCl 2 (0.035 g, 0.25 mmol), HgCl 2 (0.136 g, 0.50 mmol) and Te (0.255 g, 2 mmol) were added to 2.0 ml of hydrazine (N 2 h 4 ) and 1.0 ml of triethylenetetramine (trien) mixed solution, stirred for 10 minutes, put the mixture into a polytetrafluoroethylene-lined stainless steel reactor, and reacted at 100° C. for 5 days. After cooling to room temperature, black crystals were precipitated, filtered, washed with 5 ml of ethanol and acetone, and dried in vacuo to obtain 0.199 g of crystals with a yield of 67%. Elemental analysis: C 5.94, H 2.12, N 9.31%; theoretical value: C 6.07, H 2.21, N 9.44%. Infrared absorption spectrum data (KBr, cm -1 ): 3460(s), 3270(m), 3106(w), 2922(w), 2064(m), 1656(s), 1589(s), 1526(w), 1463(m), 1379(s ),1274(w),1118(s),1072(w),996(s),950(s),861(w),786(m),673(w),618(s),542(m ), 479(s), 424(m), 408(w). Solid State Absorption Spectrometry: Semiconductor Energy Gap E g = 0.8...

Embodiment 3

[0051] Embodiment three: [Fe(trien)(N 2 h 4 ) 2 ]Hg 2 Te 4

[0052] FeCl 2 (0.032 g, 0.25 mmol), HgCl 2 (0.136 g, 0.50 mmol) and Te (0.255 g, 2 mmol) were added to 2.0 ml of hydrazine (N 2 h 4 ) and 1.0 ml of triethylenetetramine (trien) mixed solution, stirred for 10 minutes, put the mixture into a polytetrafluoroethylene-lined stainless steel reactor, and reacted at 100° C. for 5 days. After cooling to room temperature, black crystals were precipitated, filtered, washed with 5 ml of ethanol and acetone, and dried in vacuum to obtain 0.191 g of crystals, with a yield of 65%. Elemental analysis: C 5.99, H 2.17, N 9.45%; theoretical value: C 6.12, H 2.23, N 9.51%. Infrared absorption spectrum data (KBr, cm -1 ): 3455(w), 3305(w), 3252(m), 3200(m), 2999(w), 2367(w), 1565(s), 1485(s), 1452(m), 1378(s ), 1207(w), 1109(w), 1024(s), 877(w), 744(w), 650(w), 510(m), 418(w). Solid State Absorption Spectrometry: Semiconductor Energy Gap E g = 0.87eV.

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Abstract

The invention discloses a mercury-tellurium compound containing transition metal complex ions and a hydrazine-aided preparation method thereof. The mercury-tellurium compound has a general formula of [TM(trien)(N2H4)2]Hg2Te4 or [TM(tepa)(N2H4)]2Hg4Te12, or [TM(trien){Hg2Te4}], or [TM(tepa)]2Hg5Te12, wherein TM is selected from a group consisting of Fe, Co, Ni, Mn and Zn, trien is triethylene tetramine, and tepa is tetraethylenepentamine. The invention also provides the hydrazine-aided preparation method for the compound. The hydrazine-aided preparation method is simple in synthesis, employs elemental tellurium powder as the single tellurium source, needs no intermediate step, substantially reduces reaction temperature in synthesis of the mercury-tellurium compound and does not need protection gas; the prepared compound is convenient to separate and purify; and the structure of mercury-tellurium anions and coordination between the mercury-tellurium anions and transition metal ions can be regulated by using different reaction temperatures and different organic amine ligands.

Description

technical field [0001] The invention relates to a mercury tellurium compound containing transition metal complex ions and a hydrazine-assisted preparation method thereof. Background technique [0002] Transition metals have an unfilled (n-1)d electron layer structure, which exhibits good magnetic and luminescent properties, and metal chalcogenides have good semiconductor properties. Therefore, mercury tellurium compounds containing transition metal complex ions are excellent properties Multifunctional composite materials have broad application prospects in the fields of magnetic materials, semiconductor materials, luminescence and photocatalysis. In the research field of metal chalcogenides containing transition metal complex ions, metal sulfides and metal selenides have been extensively studied. People have synthesized a series of transition metal complex ions by using solvothermal method with organic polyamines as ligands. metal sulfides and metal selenides [1-5] . Due ...

Claims

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Application Information

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IPC IPC(8): C07F13/00C07F3/06C07F15/02C07F15/06C07F15/04
CPCC07F3/06C07F13/00C07F15/02C07F15/04C07F15/06
Inventor 贾定先孙佩佩刘淑真韩静瑜李淑芬张立梅
Owner SUZHOU UNIV
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