Millimeter-sized sp3 amorphous carbon block material and method for preparing the same

Patent metadata

Field	Value
Publication number	US-2023096646-A1
Application number	US-202117535899-A
Country	US
Kind code	A1
Filing date	Nov 26, 2021
Priority date	Sep 26, 2021
Publication date	Mar 30, 2023
Grant date	—

Abstract

The invention relates to a millimeter-sized bulk spa amorphous carbon material and a method of preparing the same, and the method comprises a step of performing a high-temperature and high-pressure (HTHP) treatment on C60 powder at a temperature of 450-1100° C., preferably 700-1000° C., more preferably 900-1000° C., and most preferably 1000° C., and a pressure of 20-37 GPa, preferably 20-30 GPa, and most preferably 27 GPa, so as to obtain the millimeter-sized bulk sp3 amorphous carbon material. The sp3 carbon content in the amorphous carbon material is adjustable by changing the temperature and pressure conditions, so that the sp3 content is greater than 80%, and the sp3 content of high-quality samples is close to 100%. The optical band gap and thermal conductivity of the series of amorphous carbon materials can be effectively adjusted. The obtained series of amorphous carbon materials have ultra-high hardnesses, high thermal conductivities, adjustable band gaps (1.90-2.79 eV) which exceed the ranges of the band gaps of amorphous silicon and germanium. As a result, a new space is opened up for the application of amorphous materials.

First claim

1 . A method for preparing a millimeter-sized bulk sp 3 amorphous carbon material, comprising a step of
performing a high-temperature and high-pressure (HTHP) treatment on a sample of C 60 powder at a temperature of 450-1100° C., preferably 700-1000° C., more preferably 900-1000° C., and most preferably 1000° C., and a pressure of 20-37 GPa, preferably 20-30 GPa, and most preferably 27 GPa, so as to obtain the millimeter-sized bulk sp 3 amorphous carbon material.

2 . The method of claim 1 , wherein the HTHP treatment is carried out in a large-volume press, and preferably, the C 60 powder is encapsulated into a sample chamber made of metal Re to undergo the HTHP treatment.

3 . The method of claim 1 , further comprising a step of heat-treating the C 60 powder, preferably at a temperature from 80° C. to 150° C. for 2 to 4 hours, to obtain dried C 60 powder before the HTHP treatment.

4 . The method of claim 1 , wherein the HTHP treatment comprises pressurizing the C 60 powder to said pressure within 7-10 hours, and heating the C 60 powder to said temperature using a rhenium tube.

5 . The method of claim 1 , further comprising a step of heat and pressure preservation of the treated sample after the HTHP treatment, and preferably, the heat and pressure preservation lasts for 1-2 hours.

6 . The method of claim 1 , further comprising a step of cooling and depressurizing the treated sample after the HTHP treatment, and preferably, the treated sample is cooled to room temperature by quenching immediately and is depressurized to ambient pressure within 14-20 hours.

7 . The method of claim 1 , further comprising ultrasonically cleaning the treated sample in acetone and polishing the treated sample with a diamond grinding disc to obtain a pure bulk amorphous carbon material.

8 . The method of claim 1 , wherein the mass purity of the C 60 powder is greater than or equal to 99.9%.

9 . The method of claim 1 , wherein the sp 3 content of the bulk sp 3 amorphous carbon material is greater than 80%, preferably in the range of 83.3% to 95.1%.

10 . The method of claim 1 , wherein the optical band gap of the bulk sp 3 amorphous carbon material is in the range of 1.90-2.79 eV.

11 . The method of claim 1 , wherein the thermal conductivity of the bulk sp 3 amorphous carbon material is in the range of 18-26 W/mK.

12 . The method of claim 1 , wherein the Vickers hardness of the bulk sp 3 amorphous carbon material is in the range of 95-102 GPa.

13 . The method of claim 1 , comprising:
step 1: heating C 60 powder at a temperature in the range of 80-150° C. for 2-4 hours to obtain dried C 60 powder; step 2: encapsulating the C 60 powder heated in step 1 into a sample chamber made of metal Re, which is then placed in an HTHP apparatus of a large-volume press to undergo the HTHP treatment at a temperature in the range of 700-1000° C. and a pressure in the range of 20-37 GPa, followed by heat and pressure preservation for 1-2 hours, subsequent immediate quenching to room temperature and slowly depressurizing to ambient pressure, and taking out the sample; and step 3: ultrasonically cleaning the sample in acetone, and then polishing it with a diamond grinding disc to obtain a pure bulk sp 3 amorphous carbon material.

14 . A millimeter-sized bulk sp 3 amorphous carbon material, wherein the sp 3 content of the bulk sp 3 amorphous carbon material is greater than 80%, preferably in the range of 83.3-95.1%.

15 . The millimeter-sized bulk sp 3 amorphous carbon material of claim 14 , wherein the bulk sp 3 amorphous carbon material is translucent or transparent.

16 . The millimeter-sized bulk sp 3 amorphous carbon material of claim 14 , wherein the optical band gap of the bulk sp 3 amorphous carbon material is in the range of 1.90-2.79 eV.

17 . The millimeter-sized bulk sp 3 amorphous carbon material of claim 14 , wherein the thermal conductivity of the bulk sp 3 amorphous carbon material is in the range of 18-26 W/mK.

18 . The millimeter-sized bulk sp 3 amorphous carbon material of claim 14 , wherein the Vickers hardness of the bulk sp 3 amorphous carbon material is in the range of 95-102 GPa.

19 . A millimeter-sized bulk sp 3 amorphous carbon material, wherein the millimeter-sized bulk sp 3 amorphous carbon material is prepared by the method of claim 1 .

Assignees

• Univ Jilin

Inventors

• Liu Bingbing
• Yao Mingguang
• Shang Yuchen
• Liu Zhaodong
• Dong Jiajun

Classifications

• C01B32/156 Primary

  After-treatment · CPC title

• C01P2006/90

  Other properties not specified above · CPC title

• C01P2006/60

  Optical properties, e.g. expressed in CIELAB-values · CPC title

• C04B35/528 Primary

  obtained from carbonaceous particles with or without other non-organic components · CPC title

• C01P2006/40

  Electric properties · CPC title