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Oxide of transition metalin treble valence state, and preparation method

A technology for transition metals and oxides, applied in the field of triple valence transition metal oxides and their preparation, to achieve the effects of large and uniform product crystal particles, mild synthesis conditions, and good repeatability

Inactive Publication Date: 2008-02-13
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, the case of a single metal ion exhibiting more than two stable oxidation states has not been reported

Method used

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  • Oxide of transition metalin treble valence state, and preparation method

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Experimental program
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Effect test

Embodiment 1

[0024] Dissolve the reaction raw materials with high-purity water and prepare a solution for later use, which are La(NO 3 ) 3 Solution 0.4M, Ca(NO 3 ) 2 Solution 0.4M, KMnO 4 Solution 0.12M, MnCl 2 Solution 0.56M. Take 5mlLa(NO 3 ) 3 The solution was placed in a beaker, and under stirring, 5ml Ca(NO 3 ) 2 solution, 10ml KMnO 4 Solution, at this time, the solution presents a dark purple color unique to potassium permanganate. Under vigorous stirring, KOH was added to make the solution in a suspension state, showing a deep black color and a metallic luster under light. Finally add MnCl 2 The solution was stirred evenly and put into a reaction kettle with a filling degree of about 75%. After tightening, it was placed in an oven at 240°C for 2 days of crystallization. The resulting product is La 0.66 Ca 0.29 K 0.05 MnO 3 .

[0025] If KOH is added too fast, dark green will appear when the solution temperature is too high, which may be due to the high alkalinity en...

Embodiment 2

[0034] The reaction raw materials are Re(NO 3 ) 3 (Re=La, Y) solution 0.4M, M 11 (NO 3 ) 2 (M 11 =Ca, Sr, Ba) solution 0.4M, KMnO 4 Solution 0.12M, MnCl 2 Solution 0.56M. According to Re(NO 3 ) 3 : M 11 (NO 3 ) 2 : MnCl 2 4H 2 O: KMnO 4 The molar ratio is 1:4~0.1:3.2~0.8:2.4~1.8, put it in a beaker, and add M 1 OH(M 1 = Li, Na, K). At this time, the solution is in the state of a suspension. Stir evenly and put it into the reaction kettle with a filling degree of about 75%. After tightening it, put it in an oven at 240°C for two days to crystallize. A series of corresponding products Re can be obtained within the range of reactant ratio. 1-x-y m 11 x m 1 y MnO 3 .

Embodiment 3

[0036] The reaction raw materials are Re(NO 3 ) 3 (Re=La, Y) solution 0.4M, M 11 (NO 3 ) 2 (M 11 =Ca, Sr, Ba) solution 0.4M, VCl 3 solution 0.56M, and V 2 o 5 . According to Re(NO 3 ) 3 : M 11 (NO 3 ) 2 : VCl 3 :V 2 o 5 The molar ratio is 1:4~0.1:3.2~0.8:1.2~0.9, put it in a beaker, and add M 1 OH(M 1 = Li, Na.K). At this time, the solution is in the state of a suspension. Stir evenly and put it into the reaction kettle with a filling degree of about 75%. After tightening it, put it in an oven at 180-240°C to crystallize for 2 days, and a series of corresponding products can be obtained within the range of reactant ratio. 1-x-y m 11 x m 1 y VO 3 .

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Abstract

An oxide of triplet-valence transition metal with perovskite-like structure and semiconductor nature has a formula Re1-x-yMaxMbyMeO3, where Re=La or Y Ma=Li, Na, or K, x=0-1, y=0-1 and Me=Mn, V, Cr, Mo or W. It is prepared through mixing, stirring, regulating basicity and hydrothermal redox reaction at 180-300 deg.C for 1-5 days.

Description

technical field [0001] The invention belongs to the field of inorganic synthetic chemistry and relates to a perovskite-like structure (ABO 3 ) triple valence state transition metal oxide and preparation method thereof. Background technique [0002] In natural and synthetic crystalline metal oxides, a single metal ion can exhibit two oxidation states, and such crystalline metal oxides with two oxidation states are called mixed valence metal oxides. Known mixed valence metal oxides are Fe 3 o 4 , Na x WO 3 , La 1-x Ca x MnO 3 and many other transition metal oxides. At present, the most influential mixed valence crystal is the manganate giant magnetoresistance material (CMR) Re 1-x m 11 x MnO 3 . La 1-x Ca x MnO 3 It is a kind of perovskite manganate (ABO 3 , A is a 12-coordination ion, B is a 6-coordination ion), and Mn has a +3 and +4 mixed valence state due to Ca doping (see C.N.R.Rao et al., Chem.Mater.1996, 8, 2421.). Because there are complex electron-el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/00C01D15/00C01D13/00C01F17/00C01F11/00C01G41/00C01G39/00C01G37/00C01G31/00
Inventor 冯守华袁宏明施展
Owner JILIN UNIV
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