Heat reflecting pane and a method of producing it

• US 4,216,259 A
• Filed: 01/02/1979
• Issued: 08/05/1980
• Est. Priority Date: 01/02/1979
• Status: Expired due to Term

• Current Assignee: Bfg Glassgroup
• Original Assignee: Bfg Glassgroup
• Inventors: Groth, Rolf
• Primary Examiner(s): Hoffman, James R.
• Application Number:
  US06/000,104
• Time in Patent Office: 581 Days
• Field of Search: 427/160, 427/166, 428/216, 428/432
• US Class Current: 428/216
• CPC Class Codes: C03C 17/27 by oxidation of a coating previously applied
• CPC Class Codes: C03C 2217/212 TiO2
• CPC Class Codes: C03C 2218/151 by vacuum evaporation
• CPC Class Codes: C03C 2218/322 Oxidation
• CPC Class Codes: C23C 14/16 on metallic substrates or on substrates of boron or silicon
• CPC Class Codes: C23C 14/58 After-treatment
• CPC Class Codes: C23C 14/5806 Thermal treatment
• CPC Class Codes: C23C 14/5853 Oxidation
• CPC Class Codes: Y10T 428/24975 No layer or component greater than 5 mils thick

Abstract

A heat-reflecting pane consists of a substantially transparent glass substrate with two layers of titanium oxide, the outside layer being in the rutile form with the intermediate layer being in the anatase form. The pane is formed by double coating the glass substrate with layers of titanium applied by vacuum deposition. A weaker vacuum is used to obtain the anatase form with a stronger vacuum used to obtain the rutile form. Both layers are then oxidized at temperatures of at least 550° C. to form TiO₂. The intermediate layer of TiO₂ in the anatase form prevents the rutile layer from becoming opaque when the pane is heated to the temperature necessary for heat treatment of the glass substrate. The treatment may be effected either during the heating step in which the titanium is oxidized or in a subsequent additional heating step.

Claims

1. A heat-reflecting pane comprising:

a substantially transparent glass substrate; and

two adjacent layers of TiO₂ on said glass substrate comprising;

an intermediate layer of TiO₂ on said glass substrate;

said intermediate layer of TiO₂ being in the anatase form; and

an outside layer of TiO₂ on said glass substrate;

said outside layer of TiO₂ being in the rutile form;

said adjacent layers having been formed by first depositing an intermediate Ti layer to said glass substrate by vapor deposition in vacuo followed by depositing an outside Ti layer to said intermediate layer of Ti by vapor deposition in vacuo and subsequently oxidizing said intermediate and outside Ti layers at a temperature of at least 400°

C.

2. A heat-reflecting pane as defined in claim 1 wherein said adjacent layers of TiO₂ have a combined thickness of between 300 and 600 A.

3. A heat-reflecting pane as defined in claim 2 wherein said intermediate layer of TiO₂ has a thickness of at least 30 A.

4. A heat-reflecting pane as defined in claim 3 wherein said outside layer of TiO₂ has a thickness of no greater than 300 A.

5. A heat-reflecting pane as defined in claim 4 wherein said outside layer of TiO₂ has a thickness of at least 80 A.

6. A heat-reflecting pane as defined in claim 5 wherein said outside layer of TiO₂ has a thickness of between 220 and 250 A.

7. A heat-reflecting pane as defined in claim 1 wherein said glass substrate has been toughened by being heated to a temperature of at least 550°

C., preferably 570°

to 620°

C., followed by chilling.

8. A method of manufacturing a heat-reflecting pane comprising:

providing a substantially transparent glass substrate;

applying an intermediate Ti layer to the side of said glass substrate by vapor deposition in vacuo, using a pressure of approximately 10^-4 Torr in order to obtain the anatase form of TiO₂ ;

applying an outside Ti layer to the previously formed Ti layer by vapor deposition in vacuo, using a pressure of at least 10^-5 Torr in order to obtain the rutile form of TiO₂ ;

subsequently heating the pane in air to a temperature of at least 550°

C. in order to oxidize both Ti layers to form two layers of TiO₂, the outside Ti layer being in the rutile form with the intermediate layer being in the anatese form; and

subsequently cooling the pane.

9. A manufacturing method as defined in claim 8 wherein said intermediate Ti layer is deposited in more than 60 seconds at a pressure of between 1×

10^-4 and 2×

10^-4 Torr and said outside Ti layer is deposited in less than 30 seconds at a pressure of between 1×

10^-5 and 6×

10^-5 Torr.

10. A manufacturing method as defined in claim 8 wherein the application steps occur in a vapor-coating device and comprise:

applying said intermediate Ti layer;

lowering the pressure; and

applying said outside Ti layer, whereby the two Ti layers are vapor-deposited in succession using the same vapor-coating device.

11. A manufacturing method as defined in claim 8 wherein the heating step consists of heating the pane to a temperature of between 570°

and 620°

C. in order to oxidize the Ti films.

12. A manufacturing method as defined in claim 11 wherein the cooling step is effected rapidly to chill the glass substrate and toughen the same.

13. A manufacturing method as defined in claim 8 wherein after cooling of the pane subsequent to said step of heating the pane to at least 550°

C. to oxidize the Ti layers, the pane is again heated to at least 550°

C., preferably 570°

to 620°

C., and is then rapidly cooled to chill the glass substrate and toughen the same.