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Flame spray pyrolysis method for forming nanoscale lithium metal phosphate powders

A nanoscale, flame technology, applied in the field of forming ceramic powder, can solve the problems of large particle size, difficulty in applying highly volatile components, and retention of volatile components

Inactive Publication Date: 2015-09-02
CORNING INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the co-precipitation method often results in particle sizes that are too large for the membrane to be durable for seawater applications
[0007] Flame spray pyrolysis (FSP) can be used to form powdered materials from chemical precursors, but the FSP method can be difficult to apply to precursors containing highly volatile components such as lithium due to the high temperature conditions in the flame and the accompanying Difficulty retaining volatile components in the final product

Method used

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  • Flame spray pyrolysis method for forming nanoscale lithium metal phosphate powders
  • Flame spray pyrolysis method for forming nanoscale lithium metal phosphate powders
  • Flame spray pyrolysis method for forming nanoscale lithium metal phosphate powders

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Embodiment 1, comparative example

[0049] Precursor solutions were prepared by dissolving lithium tert-butoxide, aluminum tri-sec-butoxide, titanium isopropoxide and trimethylphosphate in 2-methoxyethanol. The total concentration of chemical precursors in solution was 1.4M. Relative to the phosphorus content in the precursor solution, the amount of lithium tert-butoxide was sufficient to form LiTi 2 (PO 4 ) 3 A 34% excess of the stoichiometric amount.

[0050] For the flame spray pyrolysis process, the precursor solution was entrained in an oxygen flow at a flow rate of 20 slpm such that the flow rate of the precursor solution was 10 mL / min. Use CH 4 and O 2 The co-flow produces a pilot flame. CH that ignites the flame 4 and O 2 The flow rates were 5.2 slpm and 5.0 slpm, respectively. figure 2 shows that the resulting powder product (which is essentially pure TiP 2 o 7 ) XRD scan pattern.

[0051] Although the precursor solution contained excess Li, the f...

Embodiment 2

[0052] Embodiment 2, comparative example

[0053] In a second comparative example, a nanoscale powder was produced using a precursor solution comprising lithium tert-butoxide, aluminum tri-sec-butoxide, titanium isopropoxide, and trimethylphosphate in 2-methoxyethanol. The lithium (lithium tert-butoxide) content in the precursor solution was in a stoichiometric excess of approximately 19% relative to the phosphorus content in the precursor solution. The total concentration of all chemical precursors in the precursor solution was 5.7M.

[0054] During the FSP, the flow rate of the precursor solution was 10 mL / min. The precursor solution was entrained in an oxygen flow at a flow rate of 20 slpm. Use CH 4 and O 2 The co-flow produces a pilot flame. CH that ignites the flame 4 and O 2 The flow rates were 5.2 slpm and 5.0 slpm, respectively.

[0055]Although the amount of lithium tert-butoxide was reduced to a 19% excess in this comparative example, the resulting nanoscale ...

Embodiment 3

[0057] Powder 3 was produced from a 2.8 M precursor solution of lithium tert-butoxide, aluminum tri-sec-butoxide, titanium isopropoxide and trimethylphosphate dissolved in 2-methoxyethanol, in which lithium tert-butoxide The amount of precursor was equal to a stoichiometric excess of 13%. The precursor solution was delivered to the FSP nozzle by entraining it in an oxygen flow of 20 slpm at a flow rate of 12.5 mL / min. With CH supplied at 5.2slpm and 5.0slpm respectively 4 and O 2 The co-flow produces a pilot flame. The differential pressure of the spray is about 1 bar.

[0058] see Figure 4 It can be seen that the nanoscale ceramic powder of Example 3 contains LiTi 2 (PO 4 ) 3 as the dominant product phase.

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Abstract

A flame spray pyrolysis method for making nanoscale, lithium ion-conductive ceramic powders comprises providing a precursor solution comprising chemical precursors dissolved in an organic solvent, and spraying the precursor solution into an oxidizing flame to form a nanoscale, lithium ion-conductive ceramic powder, wherein a concentration of the chemical precursors in the solvent ranges from 1 to 20 M. The precursor solution can comprise 1-20% excess lithium with respect to a stoichiometric composition of the ceramic powder. Nominal compositions of the nanoscale, ceramic powders are Li1.4Al0.4M1.6(PO4)3 where M is Ti or Ge.

Description

[0001] Related Application Cross Reference [0002] This application claims priority under 35 U.S.C. §120 to U.S. Application Serial No. 13 / 627,384, filed September 26, 2012, which application is based upon and is hereby incorporated by reference in its entirety. Background technique [0003] The present invention relates generally to methods for forming ceramic powders and, more particularly, to flame spray pyrolysis for forming lithium metal phosphate ceramic powders. Such powders can have nanoscale particle sizes and can be used to form lithium ion conductive ceramic membranes. For example, as disclosed herein, effective Li-ion-conducting ceramics include lithium aluminum titanium phosphate (LATP), which can include 1.4 al 0.4 Ti 1.6 (PO 4 ) 3 materials of nominal composition, and lithium aluminum germanium phosphate (LAGP), which may include Li 1.4 al 0.4 Ge 1.6 (PO 4 ) 3 Nominal composition of materials. [0004] Powders of suitable ceramic composition can be c...

Claims

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Application Information

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IPC IPC(8): C04B35/447C04B35/626B82Y40/00H01M10/0562C01B25/37C01B25/45
CPCH01M10/0562C01B25/45C04B35/6264C04B2235/3287C04B2235/5454B82Y40/00C04B2235/3232C04B2235/80C04B35/62665B82Y30/00C04B2235/3203C04B2235/6025C04B35/447H01M10/052C04B2235/3217Y02E60/10
Inventor M·E·拜丁J·L·布朗C·R·费克特宋真
Owner CORNING INC
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