Composition for forming silica layer, method for manufacturing silica layer, and silica layer

Patent metadata

Field	Value
Publication number	US-9957418-B2
Application number	US-201514967102-A
Country	US
Kind code	B2
Filing date	Dec 11, 2015
Priority date	May 15, 2015
Publication date	May 1, 2018
Grant date	May 1, 2018

Abstract

A composition for forming a silica layer includes a silicon-containing polymer and a solvent, wherein the silicon-containing polymer has a total sum of Si—H integral values in a 1 H-NMR spectrum of less than or equal to about 12.
The sum of the Si—H integral values is calculated under conditions described in the specification.

First claim

What is claimed is:

1. A composition for forming a silica layer, the composition comprising
a silicon-containing polymer including a SiH 3 moiety, and
a solvent,
wherein the silicon-containing polymer has a total sum of Si—H integral values in a 1 H-NMR spectrum of less than or equal to about 12,
the total sum of Si—H integral values is calculated through the following acts S1 and S2 provided in Condition 1:
[Condition 1]
S1) a Sample 1 having a solid content of about 15±0.1 wt % is prepared by adding the silicon-containing polymer to dibutylether (DBE) and then diluting it by 20% by volume with a CDCl 3 (Chloroform-d) solvent, thereby preparing a Sample 2, and
S2) 1 H-NMR spectrum of the Sample 2 is measured at 300 MHz to calculate integral values of Si—H 1 , Si—H 2 , and Si—H 3 according to the following method, the calculation is repeated three times, these three measurements are averaged, and this average is regarded as a total sum of the Si—H integral values,
wherein a method of calculating the sum of the integral values of the Si—H 1 , Si—H 2 , and Si—H 3 is as follows:
assuming that the dibutylether has an integral value of 40, integral values of a peak (peak B) corresponding to Si—H 1 and Si—H 2 present in the silicon-containing polymer and a peak (peak C) corresponding to Si—H 3 are respectively calculated, and
the peaks B and C are summed, and the sum is regarded as the sum of the integral values of Si—H 1 , Si—H 2 , and Si—H 3 ; and
the SiH 3 moiety is included in an amount of about 15 to about 35 wt % based on a total amount of Si—H.

2. The composition of claim 1 , wherein the total sum of the Si—H integral values is in a range of about 5 to about 12.

3. The composition of claim 2 , wherein the total sum of the Si—H integral values is in a range of about 8 to about 11.5.

4. The composition of claim 1 , wherein the silicon-containing polymer comprises polysilazane, polysiloxazane, or a combination thereof.

5. The composition of claim 1 , wherein the solvent comprises at least one selected from benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, triethylbenzene, cyclohexane, cyclohexene, decahydro naphthalene, dipentene, pentane, hexane, heptane, octane, nonane, decane, ethylcyclohexane, methylcyclohexane, cyclohexene, p-menthane, dipropylether, dibutylether (DBE), anisole, butyl acetate, amyl acetate, methyl isobutyl ketone, and a combination thereof.

6. The composition of claim 1 , wherein the silicon-containing polymer comprises a moiety represented by Chemical Formula 1:

wherein, in Chemical Formula 1, R 1 to R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C30 alkyl group, a substituted or unsubstituted C3 to C30 cycloalkyl group, a substituted or unsubstituted C6 to C30 aryl group, a substituted or unsubstituted C7 to C30 arylalkyl group, a substituted or unsubstituted C1 to C30 heteroalkyl group, a substituted or unsubstituted C2 to C30 heterocycloalkyl group, a substituted or unsubstituted C2 to C30 alkenyl group, a substituted or unsubstituted alkoxy group, a carboxyl group, an aldehyde group, a hydroxy group, or a combination thereof, and
“*” indicates a linking point.

7. The composition of claim 6 , wherein the silicon-containing polymer further comprises a moiety represented by Chemical Formula 2:

R 4 to R 7 of Chemical Formula 2 are each independently hydrogen, a substituted or unsubstituted C1 to C30 alkyl group, a substituted or unsubstituted C3 to C30 cycloalkyl group, a substituted or unsubstituted C6 to C30 aryl group, a substituted or unsubstituted C7 to C30 arylalkyl group, a substituted or unsubstituted C1 to C30 heteroalkyl group, a substituted or unsubstituted C2 to C30 heterocycloalkyl group, a substituted or unsubstituted C2 to C30 alkenyl group, a substituted or unsubstituted alkoxy group, a carboxyl group, an aldehyde group, a hydroxy group, or a combination thereof, and
“*” indicates a linking point.

8. The composition of claim 1 , wherein the silicon-containing polymer is included in an amount of about 0.1 to about 30 wt % based on the total amount of the composition for forming a silica layer.

9. A method for manufacturing a silica layer, the method comprising:
coating the composition of claim 1 on a substrate;
drying the substrate coated with the composition to produce a resultant; and
curing the resultant under an inert atmosphere at a temperature of greater than or equal to about 150° C. to manufacture a silica layer.

10. The method of claim 9 , wherein the composition for forming a silica layer is coated utilizing a spin-coating method.

11. The method of claim 9 , wherein the total sum of the Si—H integral values is in a range of about 5 to about 12.

12. The method of claim 11 , wherein the total sum of the Si—H integral values is in a range of about 8 to about 11.5.

13. The method of claim 9 , wherein the silicon-containing polymer comprises polysilazane, polysiloxazane, or a combination thereof.

14. The method of claim 9 , wherein the solvent comprises at least one selected from benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, triethylbenzene, cyclohexane, cyclohexene, decahydro naphthalene, dipentene, pentane, hexane, heptane, octane, nonane, decane, ethylcyclohexane, methylcyclohexane, cyclohexene, p-menthane, dipropylether, dibutylether, anisole, butyl acetate, amyl acetate, methyl isobutyl ketone, and a combination thereof.

15. The method of claim 9 , wherein the silicon-containing polymer comprises a moiety represented by Chemical Formula 1:

wherein, in Chemical Formula 1, R 1 to R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C30 alkyl group, a substituted or unsubstituted C3 to C30 cycloalkyl group, a substituted or unsubstituted C6 to C30 aryl group, a substituted or unsubstituted C7 to C30 arylalkyl group, a substituted or unsubstituted C1 to C30 heteroalkyl group, a substituted or unsubstituted C2 to C30 heterocycloalkyl group, a substituted or unsubstituted C2 to C30 alkenyl group, a substituted or unsubstituted alkoxy group, a carboxyl group, an aldehyde group, a hydroxy group, or a combination thereof, and
“*” indicates a linking point.

16. A silica layer manufactured according to the method of claim 9 .

17. An electronic device comprising a silica layer, the silica layer being a derivation of the composition of claim 1 .

Assignees

• Samsung Sdi Co Ltd

Inventors

• Lee Eun-Seon
• Kim Woo-Han
• Yun Hui-Chan
• Bae Jin-Hee
• Hwang Byeong-Gyu

Classifications

• C08G77/62

  Nitrogen atoms · CPC title

• C09D1/00

  Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances · CPC title

• C09D183/16 Primary

  in which all the silicon atoms are connected by linkages other than oxygen atoms · CPC title

• H01B3/46

  silicones · CPC title

• H10P14/60

  of insulating materials · CPC title