Fluorescent detection of curing difference between surfaces
View Patent ↗Pyrene can be used as a fluorescent probe for various industrial purposes. For example, it can be included in photocurable or thermally curable compositions and monitoring the fluorescence emission spectra before and after some curing will provide an indication of how much curing has occurred. Such monitoring can be carried out multiple times during a manufacturing process. Monitoring can also be done at different locations of a composition such as at inner and outer surfaces of a photocured or thermally cured layer.
1. A method for determining the extent of curing in a layer of a photocurable or thermally curable composition, the method comprising:
providing a dried layer of a photocurable or thermally curable composition over a supporting side of a transparent polymeric substrate, the dried layer having an outermost surface and an innermost surface, and the photocurable or thermally curable composition comprising a photocurable or thermally curable component and pyrene,
exposing the photocurable or thermally curable composition to form an at least partially photocured or thermally cured composition in an at least partially photocured or thermally cured dried layer having an innermost surface and an outermost surface,
determining a first fluorescence emission spectrum emitted by the pyrene at the innermost surface of the at least partially photocured or thermally cured dried layer,
determining a second fluorescence emission spectrum emitted by the pyrene at the outermost surface of the at least partially photocured or thermally cured dried layer,
comparing the first fluorescence emission spectrum and the second fluorescence emission spectrum to determine any difference in curing between the outermost surface and the innermost surface of the at least partially photocured or thermally cured dried layer.
2. The method of claim 1 , comprising providing the photocurable or thermally curable composition on a supporting side of a transparent polymeric substrate in a patternwise manner, the transparent polymeric substrate also comprising an opposing second supporting side.
3. The method of claim 2 comprising providing the photocurable or thermally curable composition as multiple patterns on the supporting side of the transparent polymeric substrate that is a transparent polymeric web.
4. The method of claim 2 comprising providing the photocurable or thermally curable composition as multiple patterns on the supporting side of the transparent polymeric substrate in a roll-to-roll fashion.
5. The method of claim 1 , wherein the photocurable component is a photopolymerizable epoxy material.
6. The method of claim 1 , wherein the exposing is sufficient to photocure at least 10 weight % of the photocurable component.
7. The method of claim 1 , wherein the photocurable or thermally curable composition further comprises metal particles that have a particle size of at least 0.01 μm and up to and including 25 μm.
8. The method of claim 7 , wherein the photocurable or thermally curable composition further comprises metal particles that are carbon-coated silver particles or carbon-coated copper particles.
9. The method of claim 5 , wherein the photocurable composition further comprises a photoacid generator that is an iodonium or sulfonium salt.
10. The method of claim 1 , wherein the pyrene is present in the photocurable or thermally curable composition in an amount of at least 0.0001 weight % and up to and including 10 weight % based on the total solids in the photocurable or thermally curable composition.
11. The method of claim 1 , wherein the photocurable composition comprises one or more free radically polymerizable compounds as the photocurable component, and further comprises one or more free radical photoinitiators.
12. The method of claim 1 , wherein comparing the first fluorescence emission spectrum and the second fluorescence emission spectrum is carried out by comparing first and second predetermined emission peaks in the first fluorescence emission spectrum and the second fluorescence emission spectrum.
13. The method of claim 1 , wherein the dried layer has an average dry thickness of at least 0.1 μm and up to and including 10,000 μm.