N-h free and si-rich per-hydridopolysilzane compositions, their synthesis, and applications

Patent metadata

Field	Value
Publication number	US-2018072571-A1
Application number	US-201715661412-A
Country	US
Kind code	A1
Filing date	Jul 27, 2017
Priority date	Dec 11, 2016
Publication date	Mar 15, 2018
Grant date	—

Abstract

Solid or liquid N—H free, C-free, and Si-rich perhydropolysilazane compositions comprising units having the following formula [—N(SiH 3 ) x (SiH 2 -) y ], wherein x=0, 1, or 2 and y=0, 1, or 2 when x+y=2; and x=0, 1 or 2 and y=1, 2, or 3 when x+y=3 are disclosed. Also disclosed are synthesis methods and applications for the same.

First claim

We claim:

1 . A N—H free, C-free, and Si-rich perhydropolysilazane composition having a molecular weight ranging from approximately 332 dalton to approximately 100,000 dalton and comprising N—H free repeating units having the formula [—N(SiH 3 ) x (SiH 2 -) y ], wherein x=0, 1, or 2 and y=0, 1, or 2 with x+y=2; and x=0, 1 or 2 and y=1, 2, or 3 with x+y=3.

2 . The N—H free, C-free, and Si-rich perhydropolysilazane composition of claim 1 , the composition having a Si:N ratio ranging from approximately 1.5:1 to approximately 2.5:1.

3 . The N—H free, C-free, and Si-rich perhydropolysilazane composition of claim 1 , the composition comprising between approximately 0 wt % and approximately 1 wt % of any N—H containing unit.

4 . The N—H free, C-free, and Si-rich perhydropolysilazane composition of claim 1 , the composition comprising between approximately 99 wt % to approximately 100 wt % of N—H free repeating units having a N atom bonded to 3 silicon atoms.

5 . The N—H free, C-free, and Si-rich perhydropolysilazane composition of claim 1 , the composition being a liquid at standard temperature and pressure.

6 . A method of synthesizing a N—H free, C-free, and Si-rich perhydropolysilazane composition, the method comprising mixing trisilylamine and a catalyst to produce the N—H free, C-free, and Si-rich perhydropolysilazane composition having a molecular weight ranging from approximately 332 dalton to approximately 100,000 dalton.

7 . The method of claim 6 , wherein the catalyst is selected from the group consisting of B(C 6 F 5 ) 3 , BPh 3 , PdCl 2 , Co 2 (CO) 8 , Ru 3 (CO) 12 , and Zeolite Y (H) Si:Al.

8 . The method of claim 6 , further comprising mixing trisilylamine and the catalyst at room temperature and atmospheric pressure.

9 . The method of claim 6 , wherein the synthesis process does not utilize a NH 3 reactant.

10 . The method of claim 6 , wherein the N—H free, C-free, and Si-rich perhydropolysilazane composition has a Si:N ratio ranging from approximately 1.5:1 to approximately 2.5:1.

11 . The method of claim 6 , wherein the catalyst is B(C 6 F 5 ) 3 , further comprising adding a quenching agent when a N—H free, C-free, and Si-rich perhydropolysilazane composition obtains the desired molecular weight.

12 . The method of claim 6 , wherein the method produces the N—H free, C-free, and Si-rich perhydropolysilazane composition without further treating the composition to remove any N—H bonds.

13 . The method of claim 6 , wherein the trisilylamine and the catalyst are mixed on a substrate

14 . The method of claim 6 , the N—H free, C-free, and Si-rich perhydropolysilazane composition comprising between approximately 0 wt % and approximately 1 wt % of any N—H containing unit.

15 . The method of claim 6 , the N—H free, C-free, and Si-rich perhydropolysilazane composition comprising between approximately 99 wt % to approximately 100 wt % of N—H free repeating units having a N atom bonded to 3 silicon atoms.

16 . A method of forming a Si-containing film on a substrate, the method comprising forming a solution comprising a N—H free, C-free, and Si-rich perhydropolysilazane composition and contacting the solution with the substrate via a spin coating, spray coating, dip coating, or slit coating technique to form the Si-containing film, the N—H free, C-free, and Si-rich perhydropolysilazane composition comprising N—H free repeating units having the formula [—N(SiH 3 ) x (SiH 2 -) y ], wherein x=0, 1, or 2 and y=0, 1, or 2 with x+y=2; and x=0, 1 or 2 and y=1, 2, or 3 with x+y=3.

17 . The method of claim 16 , further comprising curing the Si-containing film.

18 . The method of claim 16 , the Si-containing film being SiON.

19 . The method of claim 6 , the N—H free, C-free, and Si-rich perhydropolysilazane composition comprising between approximately 0 wt % and approximately 1 wt % of any N—H containing unit.

20 . The method of claim 6 , the N—H free, C-free, and Si-rich perhydropolysilazane composition comprising between approximately 99 wt % to approximately 100 wt % of N—H free repeating units having a N atom bonded to 3 silicon atoms.

Assignees

• Air Liquide Advanced Mat Inc
• Air Liquide
• Air Liquide Electronics Us Lp
• Air Liquide American
• Air Liquide Advanced Mat Llc

Inventors

• Sanchez Antonio
• Itov Gennadiy
• Khandelwal Manish
• Ritter Cole
• Zhang Peng
• Girard Jean-Marc
• Wan Zhiwen
• Kuchenbeiser Glenn
• Orban David
• Kerrigan Sean
• Pesaresi Reno
• Stephens Matthew Damien
• Wang Yang
• Husson Guillaume

Classifications

• H10P14/6927

  the material being a silicon oxynitride, e.g. SiON or SiON:H · CPC title

• H10P14/6689

  the compound being a silazane · CPC title

• C23C18/1291

  by heating of the substrate · CPC title

• C04B2235/483

  Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes · CPC title

• C04B35/571

  obtained from {Si-containing} polymer precursors {or organosilicon monomers} · CPC title