Method for making semimetal compound of Pt

Patent metadata

Field	Value
Publication number	US-10280529-B2
Application number	US-201715642412-A
Country	US
Kind code	B2
Filing date	Jul 6, 2017
Priority date	Sep 28, 2016
Publication date	May 7, 2019
Grant date	May 7, 2019

Abstract

The disclosure relates to a method for making semimetal compound of Pt. The semimetal compound is a single crystal material of PtSe 2 . The method comprises: placing pure Pt and pure Se in a reacting chamber as reacting materials; evacuating the reacting chamber to be vacuum less than 10 Pa; heating the reacting chamber to a first temperature of 600 degrees Celsius to 800 degrees Celsius and keeping for 24 hours to 100 hours; cooling the reacting chamber to a second temperature of 400 degrees Celsius to 500 degrees Celsius and keeping for 24 hours to 100 hours at a cooling rate of 1 degrees Celsius per hour to 10 degrees Celsius per hour to obtain a crystal material of PtSe 2 ; and separating the excessive reacting materials from the crystal material of PtSe 2 .

First claim

What is claimed is:

1. A method for making semimetal compound of Pt, the method comprising:
providing a quartz tube having an open end and a sealed end opposite to the open end;
filling quartz slag in the quartz tube so that the quartz slag to form a support at the sealed end;
filling quartz wool in the quartz tube so that the quartz wool to form a filter on the quartz slag;
placing Pt and Se in the quartz tube as reacting materials, wherein a first purity of the Pt is greater than 99.9%, and a second purity of the Se is greater than 99.99%;
evacuating the quartz tube to be vacuum with a pressure lower than 10 Pa;
sealing the open end;
vertically accommodating the quartz tube in a steel sleeve so that the reacting materials is located at a bottom of the quartz tube and the quartz slag and the quartz wool are located at a top of the quartz tube;
heating the steel sleeve to a first temperature of 600 degrees Celsius to 800 degrees Celsius and keeping the first temperature for a first period of 24 hours to 100 hours;
cooling the steel sleeve to a second temperature of 400 degrees Celsius to 500 degrees Celsius and keeping the second temperature for a second period of 24 hours to 100 hours at a cooling rate of 1 degrees Celsius per hour to 10 degrees Celsius per hour to obtain a reaction product comprising a crystal material of PtSe 2 ; and
separating the crystal material of PtSe 2 from the reaction product by reversing the steel sleeve.

2. The method of claim 1 , wherein a molar ratio of Pt element and Se element is from 2:80 to 2:120.

3. The method of claim 2 , wherein the molar ratio of Pt element and Se element is 2:98.

4. The method of claim 1 , wherein the pressure is lower than 1 Pa.

5. The method of claim 1 , wherein the sealing the open end comprises fast heating the open end by a flame.

6. The method of claim 1 , wherein the vertically accommodating the quartz tube in the steel sleeve comprises filling fire-resistant cotton between the quartz tube and the steel sleeve.

7. The method of claim 1 , wherein the separating the crystal material of PtSe 2 from the reaction product further comprises centrifuging the reaction product.

8. The method of claim 7 , wherein a period of the centrifuging the reaction product is in a range from a minute to 5 minutes, and a speed of the centrifuging the reaction product is in a range of 2000 rpm to 3000 rpm.

Assignees

• Univ Tsinghua
• Hon Hai Prec Ind Co Ltd

Inventors

• Zhang Ke-Nan
• Yan Ming-Zhe
• Zhou shu-yun
• Wu Yang
• Fan Shou-Shan

Classifications

• C01P2004/60

  Particles characterised by their size · CPC title

• C30B25/00

  Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2004/01

  depicted by an image · CPC title

• C01B19/007 Primary

  Tellurides or selenides of metals (C01B19/002 takes precedence) · CPC title