Low temperature process for the formation of ceramic coatings

Claim 2

A process for the formation of a ceramic or ceramic-like coating on a substrate comprising the steps of: (a) coating said substrate with a solution comprising a hydrogen silsesquioxane resin diluted in a solvent; (b) evaporating said solvent to thereby deposit a preceramic coating on said substrate; and (c) ceramifying said preceramic coating to a silicon dioxide-containing ceramic by heating said preceramic coating to a temperature of between about 40° to about 400° C. in the presence of ozone.

Claim 3

The process of claim 1 in which said ozone is generated by a source of ultraviolet light.

Claim 4

The process of claim 1 in which said ozone is generated by a source of electric discharge.

Claim 5

The process of claim 1 in which said ceramifying step is carried out in the presence of water vapor.

Claim 6

The process of claim 2 in which said source of ultraviolet light emits in the range of 185 to 200 nanometers.

Claim 7

The process of claim 1 in which said solution also contains a soluble metal oxide precursor in which the metal in said metal oxide precursor is aluminum, titanium, or zirconium and in which the metal has an alkoxide, ketonate, diketonate, silanolate, or glycolate substituent.

Claim 8

The process of claim 1 in which said solution also contains platinum.

Claim 9

The process of claim 7 in which said platinum is present in an amount of between about 15 to about 200 ppm, based on the weight of said resin.

Claim 10

The process of claim 6 in which said solution also contains platinum.

Claim 11

The process of claim 1 in which said solution containing hydrogen silsesquioxane is coated onto said substrate by spray coating, dip coating, flow coating, or spin coating.

Claim 12

The process of claim 1 in which said substrate is an electronic device.

Claim 13

The process of claim 1 in which said substrate is a silicon wafer.

Claim 14

A process for the formation of a multilayer ceramic or ceramic-like coating on a substrate comprising the steps of: (I) (a) coating said substrate with a planarizing coating comprising a solution of a hydrogen silsesquioxane resin diluted in a solvent; (b) evaporating said solvent to thereby deposit a preceramic coating on said substrate; and (c) ceramifying said preceramic coating to a silicon dioxide-containing ceramic by heating said preceramic coating to a temperature of between about 40° to about 400° C. in the presence of ozone to form said planarizing coating; (II) applying to said planarizing coating a passivating coating selected from the group consisting of (i) a silicon nitrogen-containing coating, (ii) a silicon carbon-containing coating, and (iii) a silicon carbon nitrogen-containing coating; and (III) applying to said passivating coating a silicon-containing coating selected from the group consisting of (i) a silicon coating, (ii) a silicon carbon-containing coating, (iii) a silicon nitrogen-containing coating, and (iv) a silicon carbon nitrogen-containing coating, whereby a multilayer ceramic or ceramic-like coating is obtained.

Claim 15

A process for the formation of a multilayer ceramic or ceramic-like coating on a substrate comprising the steps of: (I) (a) coating said substrate with a planarizing coating comprising a solution of a hydrogen silsesquioxane resin diluted in a solvent; (b) evaporating said solvent to thereby deposit a preceramic coating on said substrate; and (c) ceramifying said preceramic coating to a silicon dioxide-containing ceramic by heating said preceramic coating to a temperature of between about 40° to about 400° C. in the presence of ozone to form said planarizing coating; (II) applying to said planarizing coating a passivating coating selected from the group consisting of (i) a silicon nitrogen-containing coating, (ii) a silicon carbon-containing coating, and (iii) a silicon carbon nitrogen-containing coating; and (III) applying to said passivating coating a silicon-containing coating selected from the group consisting of (i) a silicon coating, (ii) a silicon carbon-containing coating, (iii) a silicon nitrogen-containing coating, and (iv) a silicon carbon nitrogen-containing coating, whereby a multilayer ceramic or ceramic-like coating is obtained.

Claim 16

The process of claim 13 wherein in said passivating coating said silicon nitrogen-containing coating is applied onto said planarizing coating by a means selected from the group consisting of (a) chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, (b) plasma enhanced chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, (c) ceramification of a silicon and nitrogen-containing polymer; and wherein said silicon carbon nitrogen-containing coating is applied onto said planarizing coating by a means selected from the group consisting of (1) chemical vapor deposition of hexamethyldisilazane, (2) plasma enhanced chemical vapor deposition of hexamethyldisilazane, (3) chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixture thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane, and further in the presence of ammonia, and (4) plasma enhanced chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixture thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane, and further in the presence of ammonia; and wherein the silicon carbon-containing coating is deposited by a means selected from the group consisting of (i) chemical vapor deposition of a silane, halosilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms, to produce said passivating coating.

Claim 17

The process of claim 13 wherein in said silicon-containing coating, the silicon coating is applied onto said passivating coating by a means selected from the group consisting of (a) chemical vapor deposition of a silane, halosilane, halopolysilane, or mixtures thereof, (b) plasma enhanced chemical vapor deposition of a silane, halosilane, halopolysilane, or mixtures thereof, or (c) metal assisted chemical vapor deposition of a silane, halosilane, halopolysilane, or mixtures thereof; and wherein the silicon carbon-containing coating is applied by a means selected from the group consisting of (1) chemical vapor deposition of a silane, alkylsilane, halosilane, halodisilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane, (2) plasma enhanced chemical vapor deposition of a silane, alkylsilane, halosilane, halodisilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane; and wherein the silicon nitrogen-containing coating is deposited by a means selected from the group consisting of (A) chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, (B) plasma enhanced chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, and (C) ceramification of a silicon and nitrogen-containing preceramic polymer; and wherein the silicon carbon nitrogen-containing coating is deposited by a means selected from the group consisting of (i) chemical vapor deposition of hexamethyldisilazane, (ii) plasma enhanced chemical vapor deposition of hexamethyldisilazane, (iii) chemical vapor deposition of a silane, alkylsilane, halosilane, halodisilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane and further in the presence of ammonia, and (iv) plasma enhanced chemical vapor deposition of a silane, alkylsilane, halosilane, halodisilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane and further in the presence of ammonia, to produce said silicon-containing coating.

Claim 18

The process of claim 13 in which said ozone is generated by a source of ultraviolet light.

Claim 19

The process of claim 13 in which said ozone is generated by a source of electric discharge.

Claim 20

The process of claim 13 in which said ceramifying step is carried out in the presence of water vapor.

Claim 21

The process of claim 16 in which said source of ultraviolet light emits in the range of 185 to 200 nanometers.

Claim 22

The process of claim 13 in which said solution also contains a soluble metal oxide precursor in which the metal in said metal oxide precursor is aluminum, titanium, or zirconium and in which the metal has an alkoxide, ketonate, diketonate, silanolate, or glycolate substituent.

Claim 23

The process of claim 13 in which said solution also contains platinum.

Claim 24

The process of claim 21 in which said platinum is present in an amount of between about 15 to about 200 ppm, based on the weight of said resin.

Claim 25

The process of claim 20 in which said solution also contains platinum.

Claim 26

The process of claim 13 in which said solution containing hydrogen silsesquioxane resin is coated onto said substrate by spray coating, dip coating, flow coating, or spin coating.

Claim 27

The process of claim 13 in which said substrate is an electronic device.

Claim 28

The process of claim 13 in which said substrate is a silicon wafer.

Claim 29

A process for the formation of a dual layer ceramic or ceramic-like coating on a substrate comprising the steps of: (I) (a) coating said substrate with a planarizing coating comprising a solution of a hydrogen silsesquioxane resin diluted in a solvent; (b) evaporating said solvent to thereby deposit a preceramic coating on said substrate; and (c) ceramifying said preceramic coating to a silicon dioxide-containing ceramic by heating said preceramic coating to a temperature of between about 40° to about 400° C. in the presence of ozone to form said planarizing coating; and (II) applying to said planarizing coating a passivating coating selected from the group consisting of (i) a silicon nitrogen-containing coating, (ii) a silicon carbon-containing coating, and (iii) a silicon carbon nitrogen-containing coating, whereby a dual layer ceramic or ceramic-like coating is obtained.

Claim 30

A process for the formation of a dual layer ceramic or ceramic-like coating on a substrate comprising the steps of: (I) (a) coating said substrate with a planarizing coating comprising a solution of a hydrogen silsesquioxane resin diluted in a solvent; (b) evaporating said solvent to thereby deposit a preceramic coating on said substrate; and (c) ceramifying said preceramic coating to a silicon dioxide-containing ceramic by heating said preceramic coating to a temperature of between about 40° to about 400° C. in the presence of ozone to form said planarizing coating; and (II) applying to said planarizing coating a passivating coating selected from the group consisting of (i) a silicon nitrogen-containing coating, (ii) a silicon carbon-containing coating, and (iii) a silicon carbon nitrogen-containing coating, whereby a dual layer ceramic or ceramic-like coating is obtained.

Claim 31

The process of claim 27 wherein in said passivating coating said silicon nitrogen-containing coating is applied onto said planarizing coating by a means selected from the group consisting of (a) chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, (b) plasma enhanced chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixtures thereof in the presence of ammonia, (c) ceramification of a silicon and nitrogen-containing polymer; and wherein said silicon carbon nitrogen-containing coating is applied onto said planarizing coating by a means selected from the group consisting of (1) chemical vapor deposition of hexamethyldisilazane, (2) plasma enhanced chemical vapor deposition of hexamethyldisilazane, (3) chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixture thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane, and further in the presence of ammonia, and (4) plasma enhanced chemical vapor deposition of a silane, halosilane, halodisilane, halopolysilane or mixture thereof in the presence of an alkane of one to six carbon atoms or an alkylsilane, and further in the presence of ammonia; and wherein the silicon carbon-containing coating is deposited by a means selected from the group consisting of (i) chemical vapor deposition of a silane, halosilane, halopolysilane, or mixtures thereof in the presence of an alkane of one to six carbon atoms, to produce said passivating coating.

Claim 32

The process of claim 27 in which said ozone is generated by a source of ultraviolet light.

Claim 33

The process of claim 27 in which said ozone is generated by a source of electric discharge.

Claim 34

The process of claim 27 in which said ceramifying step is carried out in the presence of water vapor.

Claim 35

The process of claim 29 in which said source of ultraviolet light emits in the range of 185 to 200 nanometers.

Claim 36

The process of claim 25 in which said solution also contains a soluble metal oxide precursor in which the metal in said metal oxide precursor is aluminum, titanium, or zirconium and in which the metal has an alkoxide, ketonate, diketonate, silanolate, or glycolate substituent.

Claim 37

The process of claim 25 in which said solution also contains platinum.

Claim 38

The process of claim 34 in which said platinum is present in an amount of between about 15 to about 200 ppm, based on the weight of said resin.

Claim 39

The process of claim 33 in which said solution also contains platinum.

Claim 40

The process of claim 27 in which said solution containing hydrogen silsesquioxane resin is coated onto said substrate by spray coating, dip coating, flow coating, or spin coating.

Claim 41

The process of claim 27 in which said substrate is an electronic device.

Claim 42

The process of claim 27 in which said substrate is a silicon wafer.