Monoalkyl tin trialkoxides and/or monoalkyl tin triamides with particulate contamination and corresponding methods

Patent metadata

Field	Value
Publication number	US-12024534-B2
Application number	US-202217966105-A
Country	US
Kind code	B2
Filing date	Oct 14, 2022
Priority date	Jan 30, 2019
Publication date	Jul 2, 2024
Grant date	Jul 2, 2024

Abstract

The purification of monoalkyl tin trialkoxides and monoalkyl tin triamides are described using fractional distillation and/or ultrafiltration. The purified compositions are useful as radiation sensitive patterning compositions or precursors thereof. The fractional distillation process has been found to be effective for the removal of metal impurities down to very low levels. The ultrafiltration processes have been found to be effective at removal of fine particulates. Commercially practical processing techniques are described.

First claim

What is claimed is:

1. A method for preparing a radiation sensitive composition comprising a solvent and an organometallic composition selected from the group consisting of monoalkyl tin trialkoxide, monoalkyl tin triamide, or a mixture thereof, the method comprising:
flowing the composition using an impeller style pump through a filter positioned in line with the flow to remove particle contaminants to form a filtered composition having a particle contamination of no more than about 100 particles per mL with a particle size of at least 70 nm as determined by light scattering, wherein the impeller style pump and the filter are connected by a flow conduit.

2. The method of claim 1 wherein the organometallic composition has a tin concentration from about 0.005M to about 1M.

3. The method of claim 1 wherein the solvent comprises an alcohol or mixture of alcohols.

4. The method of claim 1 wherein the flow is maintained with a plurality of inline impeller pumps.

5. The method of claim 1 wherein the filter is a semiconductor grade filter with a particle filtration rating of no more than 50 nm.

6. The method of claim 1 wherein the flowing comprises refiltering the filtered composition until the filtered composition has the indicated particle contamination.

7. The method of claim 1 wherein a filtration apparatus performing the flowing and refiltering is configured to recirculate the composition from a mixing container with an inlet and an outlet.

8. The method of claim 7 wherein the mixing container comprises a lid configured with an inlet port and an outlet port, respectively, providing access to the recirculating composition.

9. The method of claim 7 wherein the filtered composition is collected in a clean container, and the refiltering comprises flowing the filtered composition through a filter to further remove particle contaminants from the filtered composition.

10. The method of claim 7 wherein refiltering is repeated at least 3 times based on the filtration of a volume of composition provided.

11. The method of claim 7 wherein the refiltering of the filtered composition takes place until the filtered composition has a particle contamination of below 40 particles per mL with a size of at least 70 nm as determined by light scattering.

12. The method of claim 7 wherein the refiltering of the filtered composition takes place until the filtered composition has a particle contamination of below 5 particles per mL with a size of at least 100 nm as determined by light scattering.

13. The method of claim 1 wherein the flow conduit has a first end and a second end and wherein the flow conduit is connected to the impeller style pump at the first end and to the filter at the second end.

14. The method of claim 1 wherein the flow conduit comprises a polymer tubing.

15. The method of claim 1 wherein the filter is positioned distal to the impeller style pump.

16. The method of claim 1 wherein the flow proceeds along a flow path that passes first through the impeller style pump and then the filter.

17. The method of claim 1 wherein the flow proceeds along a flow path comprising a circular flow loop.

18. The method of claim 1 wherein the flow proceeds along a flow path comprising a closed flow loop configuration.

19. The method of claim 18 wherein the closed loop flow configuration comprises a branch directed to a collection container, wherein a valve can be opened to direct flow from the flow loop to the collection container after an in-line particle analyzer measures a sufficiently low particle concentration.

20. The method of claim 1 further comprising collecting the filtered composition in a collection container.

Assignees

• Inpria Corp

Inventors

• Clark Benjamin L
• Smiddy Dominick
• Geniza Mark
• Gates Craig M

Classifications

• G03F7/0042 Primary

  with inorganic or organometallic light-sensitive compounds not otherwise provided for, e.g. inorganic resists (G03F7/075 takes precedence) · CPC title

• G03F7/2004

  characterised by the use of a particular light source, e.g. fluorescent lamps or deep UV light · CPC title

• C07F7/2284

  Compounds with one or more Sn-N linkages · CPC title

• G03F7/0048

  characterised by the solvents or agents facilitating spreading, e.g. tensio-active agents · CPC title

• G03F7/16

  Coating processes; Apparatus therefor (applying coatings to base materials in general B05; applying photosensitive compositions to base for photographic purposes G03C1/74) · CPC title