Method for producing hexagonal boron nitride film using borazine oligomer as a precursor

Patent metadata

Field	Value
Publication number	US-9562287-B2
Application number	US-201314082831-A
Country	US
Kind code	B2
Filing date	Nov 18, 2013
Priority date	Sep 24, 2013
Publication date	Feb 7, 2017
Grant date	Feb 7, 2017

Abstract

Provided is a method for producing a high-quality boron nitride film grown by using a borazine oligomer as a precursor through a metal catalyst effect. The method solves the problems, such as control of a gaseous precursor and vapor pressure control, occurring in CVD (Chemical vapor deposition) according to the related art, and a high-quality hexagonal boron nitride film is obtained through a simple process at low cost. In addition, the hexagonal boron nitride film may be coated onto various structures and materials. Further, selective coating is allowed so as to carry out coating in a predetermined area and scale-up is also allowed. Therefore, the method may be useful for coating applications of composite materials and various materials.

First claim

What is claimed is:

1. A method for producing a high-quality and highly crystalline hexagonal boron nitride film for electronic materials, comprising:
mixing a borazine oligomer with an organic solvent to form a boron nitride precursor solution;
aging the precursor solution at a temperature ranging from −24° C. to −36° C. to adjust the viscosity thereof;
coating the boron nitride precursor solution onto a substrate; and
carrying out phase transfer of the borazine oligomer in the coated boron nitride precursor solution to produce a hexagonal boron nitride film on the substrate,
wherein the substrate in said coating is a metal catalyst substrate,
wherein said phase transfer is carried out by using thermal energy through heat treatment at 1000-1100° C.,
wherein the metal catalyst substrate is a metal foil, and
wherein the metal catalyst substrate has a thickness of 100 nm to 40 μm.

2. The method for producing a boron nitride film according to claim 1 , wherein the borazine oligomer is obtained by carrying out thermal oligomerization of borazine.

3. The method for producing a boron nitride film according to claim 1 , wherein the metal of the metal catalyst substrate is at least one selected from the group consisting of nickel, palladium, platinum, copper, titanium, ruthenium, chrome, iron, aluminum, and silver.

4. The method for producing a boron nitride film according to claim 1 , wherein the metal catalyst substrate is one treated by at least one process selected from the group consisting of annealing, electrochemical polishing and metal surface cleaning.

5. The method for producing a boron nitride film according to claim 1 , wherein said coating is carried out under the condition of inert gas by at least one coating process selected from the group consisting of spin coating, spray coating, drop coating and dip coating.

6. The method for producing a boron nitride film according to claim 1 , which further comprises, after said coating, baking the coated substrate to remove the organic solvent.

7. The method for producing a boron nitride film according to claim 1 , wherein said phase transfer from the borazine oligomer to hexagonal boron nitride comprises a process using at least one type of energy selected from thermal energy, plasma, laser, electron beams, ion beams and UV irradiation.

8. The method for producing a boron nitride film according to claim 7 , wherein said phase transfer is carried out under the condition of at least one gas selected from argon, nitrogen, hydrogen, ammonia and helium.

9. The method for producing a boron nitride film according to claim 7 , wherein said phase transfer is carried out by using thermal energy through heat treatment for 1-2 hours.

10. The method for producing a boron nitride film according to claim 9 , wherein the pressure in the reaction chamber during the heat treatment is within a range of 100 mtorr-760 torr.

11. The method for producing a boron nitride film according to claim 1 , which further comprises transferring the hexagonal boron nitride film to a substrate by using a polymeric protective film.

12. A method for producing a high-quality and highly crystalline boron nitride film for electronic materials comprising:
mixing a borazine oligomer with an organic solvent to form a boron nitride precursor solution; and
aging the precursor solution at a temperature raging from −24° C. to −36° C. to adjust the viscosity thereof;
coating the boron nitride precursor solution onto a substrate;
depositing a metal catalyst onto the substrate coated with the boron nitride precursor solution; and
carrying out phase transfer of the borazine oligomer in the coated boron nitride precursor solution to produce a hexagonal boron nitride film,
wherein the substrate is formed of at least one material selected from the group consisting of silicon, silicon oxide, sapphire, quartz, glass, graphite, indium oxide, polyacrylonitrile (PAN), polyethylene terephthalate (PET), polydimethylsiloxane (PDMS), polyethylene (PE), steel and carbon fibers,
wherein said phase transfer is carried out by using thermal energy through heat treatment at 1000-1100° C.

13. The method for producing a boron nitride film according to claim 12 , which further comprises treating the hexagonal boron nitride film with at least one solution selected from the group consisting of ammonium persulfate, ferric chloride (FeCl3), nitric acid, hydrochloric acid and sulfuric acid etching solutions in order to remove the metal catalyst deposited as an overlayer of the hexagonal boron nitride film.

14. The method for producing a boron nitride film according to claim 12 , wherein said deposition is carried out by at least one process selected from the group consisting of sputtering, thermal evaporation and electron beam evaporation.

15. The method for producing a boron nitride film according to claim 12 , wherein the metal catalyst is at least one selected from the group consisting of nickel, palladium, platinum, copper, titanium, ruthenium, chrome, iron, aluminum, and silver.

Assignees

• Korea Inst Sci & Tech

Inventors

• Kim Myung Jong
• Park Sungchan
• Cho Hyunjin
• Bae Sukang
• Park Jin-Hyung
• Kang Jung Ho
• Kang Sang Ook
• Lee Changhyup

Classifications

• C23C18/145

  Radiation by charged particles, e.g. electron beams or ion irradiation · CPC title

• C23C18/143

  Radiation by light, e.g. photolysis or pyrolysis · CPC title

• C23C18/1283

  Control of temperature, e.g. gradual temperature increase, modulation of temperature · CPC title

• C23C18/1241

  Metallic substrates · CPC title

• C23C18/1233

  Organic substrates · CPC title