US 12,084,379 B2
Water-and-oil repellent layer-attached substrate, and method for manufacturing same
Daisuke Kobayashi, Tokyo (JP); Maemi Iwahashi, Tokyo (JP); Aichi Inoue, Tokyo (JP); Yoshihito Tokunaga, Tokyo (JP); Kenji Ishizeki, Tokyo (JP); and Yusuke Tomiyori, Tokyo (JP)
Assigned to AGC Inc., Tokyo (JP)
Filed by AGC Inc., Tokyo (JP)
Filed on Jun. 8, 2021, as Appl. No. 17/341,499.
Application 17/341,499 is a continuation of application No. PCT/JP2019/050412, filed on Dec. 23, 2019.
Claims priority of application No. 2018-242730 (JP), filed on Dec. 26, 2018.
Prior Publication US 2021/0300817 A1, Sep. 30, 2021
Int. Cl. C03C 17/42 (2006.01); C03C 21/00 (2006.01); C09D 1/00 (2006.01); C09D 5/00 (2006.01); C09D 171/02 (2006.01); C23C 14/02 (2006.01); C23C 14/10 (2006.01); C23C 14/12 (2006.01); C23C 14/24 (2006.01); G02B 1/18 (2015.01)
CPC C03C 17/42 (2013.01) [C03C 21/002 (2013.01); C09D 1/00 (2013.01); C09D 5/002 (2013.01); C09D 171/02 (2013.01); C23C 14/024 (2013.01); C23C 14/10 (2013.01); C23C 14/12 (2013.01); C23C 14/24 (2013.01); G02B 1/18 (2015.01); C03C 2217/76 (2013.01); C03C 2218/151 (2013.01); C03C 2218/32 (2013.01)] 20 Claims
 
1. A water/oil repellent layer-provided substrate, comprising:
a substrate;
an undercoat layer formed on A surface of the substrate; and
a water/oil repellent layer formed on a surface of the undercoat layer in this order,
wherein the water/oil repellent layer comprises a condensate of a fluorinated compound having a reactive silyl group, the undercoat layer contains an oxide containing silicon and contains no alkali metal nor aluminum, the substrate comprises silica glass containing an alkali metal and aluminum, and
when the following (a), (b) and (c) are specified from a depth profile (measurement interval: 2.0 nm or shorter) obtained by X-ray photoelectron spectroscopy (XPS) by C60 ion sputtering from a surface of the water/oil repellent layer, taking a total concentration of fluorine, silicon, aluminum, the alkali metal element and oxygen as 100 at %, an alkali deficiency index determined by the following (c) is higher than 0.0; provided that a depth indicated by a horizontal axis of the depth profile is a depth calculated from a sputtering rate of a thermally oxidized film having a known thickness on a silicon wafer:
(a): in the depth profile taking the total concentration of fluorine, silicon, aluminum, the alkali metal element and oxygen as 100 at %, obtained by XPS, a point at which a fluorine concentration becomes 10 at % or lower for a first time is taken as a boundary between the water/oil repellent layer and the undercoat layer;
(b): from the depth profile taking the total concentration of fluorine, silicon, aluminum, the alkali metal element and oxygen as 100 at %, obtained by XPS, a proportion of aluminum to silicon (Al/Si) and a total proportion of the alkali metal element to silicon (alkali metal element/Si) are obtained, and based on average values of values of (Al/Si) and values of (alkali metal element/Si) in a region at a depth of at least 70.0 nm and at most 80.0 nm respectively being 1, the (Al/Si) and (alkali metal element/Si) at respective positions in a depth direction are respectively normalized, and a point at which the normalized (Al/Si) value becomes 0.50 or higher for a first time is taken as a boundary between the undercoat layer and the substrate;
(c): a region from the boundary between the undercoat layer and the substrate determined by (b) as an origin up to 20 nm in the depth direction from the origin is taken as a region X, and the alkali deficiency index in the region X defined by the following formula is obtained:
alkali deficiency index=[(average value of normalized Al/Si in the region X)−(average value of normalized alkali metal element/Si in the region X)]×20.