Preprocessing method for solid material, and solid material product filled with solid material manufactured using said solid material preprocessing method

Patent metadata

Field	Value
Publication number	US-11806677-B2
Application number	US-201816772234-A
Country	US
Kind code	B2
Filing date	Dec 6, 2018
Priority date	Dec 14, 2017
Publication date	Nov 7, 2023
Grant date	Nov 7, 2023

Abstract

A preprocessing method comprises a sintering step of heating a solid material container filled with a solid material using a temperature which is lower than either the melting point or sublimation of the solid material, whichever is lower, and crystallizing at least part of the solid material, and an impurity removal step of heating the solid material container filled with the solid material using a temperature which is lower than either the melting point or sublimation of the solid material, whichever is lower, and removing at least part of the impurities included in the solid material.

First claim

The invention claimed is:

1. A method for preprocessing a solid material, the method comprising an impurity removal step of:
heating a solid material which fills a solid material container at a temperature lower than the melting point of the solid material,
removing at least part of the impurities contained in the solid material,
heating the solid material which fills a solid material container at a temperature less than a phase transition point of the solid material, and
sintering at least part or all of the solid material,
wherein in the impurity removal step, a carrier gas having a predetermined flow rate is introduced into the solid material container, and in the sintering step no carrier gas is introduced into the solid material container,
wherein the solid material container has a carrier gas introduction pipe which introduces the carrier gas into the solid material container, a first filling unit which is disposed inside the solid material container and is filled with the solid material, a second filling unit which is disposed on at least part of an outer circumference of the first filling unit and is filled with the solid material, at least one tray-shaped third filling unit which is disposed on a ceiling-side of the interior of the solid material container, a solid material discharge pipe which discharges the carrier gas with the accompanying solid material from the solid material container, and a heating unit which heats the solid material container, a carrier gas outlet of the carrier gas introduction pipe is provided to the first filling unit, an inlet of the solid material discharge pipe is provided to the third filling unit, and the carrier gas passes through the first filling unit, the second filling unit, and the third filling unit, in this order.

2. The method of claim 1 , wherein the impurity removal step is a step of heating the solid material so as to reach a temperature less than a phase transition point thereof.

3. The method of claim 1 , wherein the solid material includes a compound selected from the group consisting of WCl 5 , WCl 6 , WOCl 4 , WO 2 Cl 2 , SiI 4 , TiI 4 , GeI 4 , GeI 2 , TiBr 4 , Si 2 I 6 , BI 3 , PI 3 , TiF 4 , TaF 5 , MoO 2 Cl 2 , MoOCl 4 , ZrCl 4 , NbCl 5 , NbOCl 3 , TaCl 5 , VCl 5 , Y(CH 3 C 5 H 4 ) 3 , Sc(CH 3 C 5 H 4 ) 3 , MoCl 5 , AlCl 3 , HfCl 4 , (CH 3 ) 3 In, (C 5 H 5 ) 2 Mg, NbF 5 , XeF 2 , VF 5 , and carboxylic acid anhydride.

4. The method of claim 3 , wherein a solid material product is filled in the solid material container.

Assignees

• Air Liquide
• Air Liquide American

Inventors

• Tarutani Kohei
• Girard Jean-Marc
• Blasco Nicolas
• Wiese Stefan
• Husson Guillaume

Classifications

• H10P14/00 Primary

  Formation of materials, e.g. in the shape of layers or pillars · CPC title

• B01D7/02 Primary

  Crystallisation directly from the vapour phase (into single crystals C30B23/00) · CPC title

• C01G41/04

  Halides · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2006/80

  Compositional purity · CPC title