Dense layered double hydroxide, and method for producing same

Patent metadata

Field	Value
Publication number	US-9708194-B2
Application number	US-201514696731-A
Country	US
Kind code	B2
Filing date	Apr 27, 2015
Priority date	Mar 25, 2013
Publication date	Jul 18, 2017
Grant date	Jul 18, 2017

Abstract

The present invention provides and produces a high-grade layered double hydroxide (LDH) dense body having a relative density of 88% or greater in a simple and stable manner. The present invention provides a LDH dense body including a layered double hydroxide as a main phase and having a relative density of 88% or greater, the LDH being represented by general formula: M 2+ 1-x M 3+ x (OH) 2 A n− x/n .mH 2 O wherein M 2+ is a divalent cation, M 3+ is a trivalent cation, A n− is an n-valent anion, n is an integer of 1 or greater, and x is 0.1 to 0.4. This LDH dense body can be produced by compacting and firing a raw material powder of a LDH to obtain an oxide fired body, retaining this oxide fired body in or immediately above an aqueous solution comprising an n-valent anion to reproduce the LDH, and removing excessive water from the resulting water-rich LDH solidified body.

First claim

What is claimed is:

1. A layered double hydroxide dense body comprising a layered double hydroxide as a main phase and having a relative density of 88% or greater, the layered double hydroxide being represented by the general formula:
M 2+ 1-x M 3+ x (OH) 2 A n− x/n .m H 2 O
wherein M 2+ is a divalent cation, M 3+ is a trivalent cation, A n− is an anion having a valency of n, n is an integer of 1 or greater, x is 0.1 to 0.4, and m is any integer greater than 0, wherein the relative density of the body is determined by dividing the density of the body calculated from the size and weight of the body by the theoretical density of the body,
wherein the body has an anisotropic conductivity characterized in that conductivity in a specific direction is greater than conductivity in a direction perpendicular to the specific direction, and
wherein the main phase is composed of layered double hydroxide grains from which a clear endothermic peak is not observed at a temperature of 300° C. or less in a different thermal analysis.

2. The layered double hydroxide dense body according to claim 1 , wherein the relative density is 90% or greater.

3. The layered double hydroxide dense body according to claim 1 , consisting essentially of the layered double hydroxide.

4. The layered double hydroxide dense body according to claim 1 , wherein in the general formula, at least M 2+ comprises Mg 2+ , M 3+ comprises Al 3+ , and A n− comprises OH − and/or CO 3 2− .

5. The layered double hydroxide dense body according to claim 1 , which has a transparency as indicated by a linear transmittance of 20% or greater at 600 nm when both sides of the dense body are polished with a coated abrasive having a particle size of #8000 defined in JIS R 6001 (1998) such that the dense body has a thickness of 1 mm.

6. The layered double hydroxide dense body according to claim 1 , which is free from cracks.

7. The layered double hydroxide dense body according to claim 1 , wherein the conductivity in the specific direction is 0.1 mS/cm or greater when measured by a four-terminal method at a temperature of 30° C. and a relative humidity of 90%.

8. A method for producing a layered double hydroxide dense body, comprising the steps of:
providing a raw material powder of a layered double hydroxide represented by the general formula:
M 2+ 1-x M 3+ x (OH) 2 A n− x/n .m H 2 O

wherein M 2+ is a divalent cation, M 3+ is a trivalent cation, A n− is an anion having a valency of n, n is an integer of 1 or greater, and x is 0.1 to 0.4 and m is any integer greater than 0;
compacting the raw material powder to obtain a compact, wherein the compaction is performed such that the compact has a relative density of 43 to 65%;
firing the compact to obtain an oxide fired body;
retaining the oxide fired body in or immediately above an aqueous solution comprising an anion having a valency of n to reproduce the layered double hydroxide, thereby obtaining a water-rich layered double hydroxide solidified body; and
removing excessive water from the water-rich layered double hydroxide solidified body, wherein the dense body comprises the layered double hydroxide as a main phase and having a relative density of 88% or greater, and the relative density is determined by dividing the density of the body calculated from the size and weight of the body by the theoretical density of the body,
wherein the body has an anisotropic conductivity characterized in that conductivity in a specific direction is greater than the conductivity in a direction perpendicular to the specific direction, and
wherein the main phase is composed of layered double hydroxide grains from which a clear endothermic peak is not observed at a temperature of 300° C. or less in a different thermal analysis.

9. The method according to claim 8 , wherein the compaction is performed at a pressure of 100 kgf/cm 2 or greater and less than 1000 kgf/cm 2 .

10. The method according to claim 8 , wherein the firing is performed such that the oxide fired body has a weight that is 57 to 65% of the weight of the compact and/or a volume that is 70 to 76% of the volume of the compact.

11. The method according to claim 8 , wherein the firing is performed such that the oxide fired body has a relative density of 20 to 40% in terms of oxide.

12. The method according to claim 8 , wherein the firing is performed at a temperature of 700 to 800° C.

13. The method according to claim 8 , wherein the reproduction of the layered double hydroxide is performed by retaining the oxide fired body at a temperature of 20° C. or greater and less than 200° C. in a state in which at least one surface of the oxide fired body is in contact with the aqueous solution.

14. The method according to claim 8 , wherein the step of removing excessive water is performed in an environment having a temperature of 300° C. or less and a relative humidity of 25% or greater.

15. The method according to claim 8 , further comprising the step of calcining the raw material powder at a temperature of 500° C. or less to obtain an oxide powder before the compaction.

Assignees

• Ngk Insulators Ltd

Inventors

• Saito Naomi
• FUJISAKI Megumi
• Matsuda Kazuyuki

Classifications

• C04B35/64

  Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F}) · CPC title

• C04B35/44 Primary

  based on aluminates · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01P2006/40

  Electric properties · CPC title

• C01G1/02

  Oxides · CPC title