Y2Si2O7 crystal whiskers and preparation method thereof

A whisker and yttrium silicate technology, which is applied in the field of Y2Si2O7 whisker and its preparation, to achieve the effects of promoting low-temperature synthesis, lowering the synthesis temperature, and being easy to control

Active Publication Date: 2016-07-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, Y 2 Si 2 o 7 Prepar...

Method used

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  • Y2Si2O7 crystal whiskers and preparation method thereof
  • Y2Si2O7 crystal whiskers and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] a Y2 Si 2 o 7 The preparation method of whisker, comprises the following steps:

[0030] (1) Weigh analytically pure Y(NO) 3 ·6H 2 O in a beaker, in a fume hood according to Y(NO) 3 ·6H 2 The molar ratio of O:TEOS=1:1 measures certain TEOS, stirs 30min to obtain the mixed solution of the two, then adds a certain amount of dehydrated alcohol, is mixed with the solution that concentration is 0.5mol / L, heats and stirs evenly, obtains Transparent yttrium silicate precursor mixture.

[0031] (2) Place the obtained yttrium silicate precursor mixture in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 30%, then put the reaction kettle into an oven, control the temperature at 100°C, and react for 12 hours . A wet gel of yttrium silicate was obtained.

[0032] (3) The obtained yttrium silicate wet gel was dried at 100° C., and then heat-treated in a muffle furnace at 350° C. for 60 minutes to obtain yttrium silicate dry gel powder.

[...

Embodiment 2

[0036] a Y 2 Si 2 o 7 The preparation method of whisker, comprises the following steps:

[0037] (1) Weigh analytically pure Y(NO) 3 ·6H 2 O in a beaker, in a fume hood according to Y(NO) 3 ·6H 2 The molar ratio of O:TEOS=1:1 measures certain TEOS, stirs 60min to obtain the mixed solution of the two, then adds a certain amount of dehydrated alcohol, is mixed with the solution that concentration is 0.75mol / L, heats and stirs evenly, obtains Transparent yttrium silicate precursor mixture.

[0038] (2) Place the obtained yttrium silicate precursor mixture in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 50%, then put the reaction kettle into an oven, control the temperature at 110°C, and react for 24h . A wet gel of yttrium silicate was obtained.

[0039] (3) The obtained yttrium silicate wet gel was dried at 80° C., and then heat-treated in a muffle furnace at 500° C. for 30 minutes to obtain yttrium silicate dry gel powder.

[004...

Embodiment 3

[0043] a Y 2 Si 2 o 7 The preparation method of whisker, comprises the following steps:

[0044] (1) Weigh analytically pure Y(NO) 3 ·6H 2 O in a beaker, in a fume hood according to Y(NO) 3 ·6H 2 O: TEOS = 1: 1 molar ratio Take a certain amount of TEOS, stir for 50 minutes to get a mixture of the two, then add a certain amount of absolute ethanol to prepare a solution with a concentration of 1mol / L, heat and stir evenly to obtain a transparent yttrium silicate precursor mixture.

[0045] (2) Place the obtained yttrium silicate precursor mixture in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 60%, then put the reaction kettle into an oven, control the temperature at 120°C, and react for 24h . A wet gel of yttrium silicate was obtained.

[0046] (3) The obtained yttrium silicate wet gel was dried at 90° C., and then heat-treated in a muffle furnace at 400° C. for 50 minutes to obtain yttrium silicate dry gel powder.

[0047] (4) M...

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Abstract

The invention discloses a preparation method of Y2Si2O7 crystal whiskers, and belongs to the technical field of ceramic material preparation.The preparation method comprises the following steps that 1, Y(NO)3.6H2O and TEOS are taken and then stirred to be uniform, absolute ethyl alcohol is added, the materials are stirred to be uniform under the heating condition, and transparent yttrium silicate precursor mixed liquid is prepared; 2, the transparent yttrium silicate precursor mixed liquid reacts for 12-24 h at the temperature of 80 DEG C-120 DEG C, and wet yttrium silicate gel is prepared; 3, the wet yttrium silicate gel is dried and then subjected to heat treatment at the temperature of 300 DEG C-500 DEG C, and dry yttrium silicate gel powder is prepared; 4, the dry yttrium silicate gel powder and mixed complex salts are mixed to be uniform according to the ratio of 1:(1-3) and then subjected to heat treatment, wherein the mixed complex salts are formed by mixing sodium molybdate with sodium sulfate according to the mass ratio of 1:1; 5, products obtained through treatment in the step 4 are sequentially subjected to washing and acid pickling and then dried, and the Y2Si2O7 crystal whiskers are prepared.The method is simple in preparation technology and short in reaction period; the Y2Si2O7 crystal whiskers prepared through the method are controllable in morphology, uniform in crystal whisker size distribution and appropriate in length-diameter ratio.

Description

technical field [0001] The invention belongs to the technical field of preparation of ceramic materials, in particular to a Y 2 Si 2 o 7 Whiskers and methods for their preparation. Background technique [0002] Y 2 Si 2 o 7 Also known as yttrium disilicate, belongs to monoclinic p2 1 / m space group structure, formed in space by [YO 6 ] octahedral vertices are connected into a two-dimensional network structure, and the network structure layer and the interlayer gap are separated by [Si 2 o 7 ] 6- Double tetrahedral filling [Julien Parmentier, Philippe Bodart R. Phase transformations in Gel-derived and mixed-powder-derived ttrium disilicate, Y 2 Si 2 o 7 byX-raydiffractionand29SiMASNMR[J]. Journal of Solid State Chemistry, 2000, 149:16220.]. Y 2 Si 2 o 7 Crystalline phases include α-Y 2 Si 2 o 7 , β-Y 2 Si 2 o 7 , γ-Y 2 Si 2 o 7 and δ-Y 2 Si 2 o 7 (stable above 1535°C) and other crystal forms (sorted from low-temperature phase to high-temperature ph...

Claims

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Application Information

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IPC IPC(8): C30B29/34C30B29/62C30B25/00
CPCC30B25/005C30B29/34C30B29/62
Inventor 黄剑锋周磊雍翔曹丽云欧阳海波陈意声李翠艳李春光
Owner SHAANXI UNIV OF SCI & TECH
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