# US 10,767,259 B2 · Components with an atomic layer deposition coating and methods of producing the same > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,767,259 B2 - Document ID: US10767259B2 - Status: Granted - Kind: B2 - Application number: 14/597,159 - Filed: 2015-01-14 - Published: 2015-05-07 - Granted: 2020-09-08 - Earliest claimed: 2013-07-19 - Assignees: Agilent Technologies, Inc. - Applicants: Agilent Technologies, Inc. - Inventors: Elizabeth Carr; Kevin P. Killeen - Web page: https://patentgrep.com/patent/US10767259B2 ## CPC - C23C 16/44: characterised by the method of coating (C23C16/04 takes precedence) - B01D 15/206: {Packing or coating} - B01D 15/22: relating to the construction of the column - C23C 16/045: {Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates} - C23C 16/45555: {applied in non-semiconductor technology} - G01N 30/6073: {in open tubular form} - G01N 2030/567: {coating} - C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q) ## Abstract Liquid chromatography and gas chromatography components with a conformal protective coating on internal surfaces thereof and methods for producing the same are provided. The conformal protective coating is formed via an atomic layer deposition (ALD) process. The components and methods of the present disclosure find use in providing protective coatings for liquid chromatography and gas chromatography components that are compatible with bioanalytical separations and sensitive trace analyses. ## Claims ### Claim 1 A component having a lumen with an interior surface covered with a conformal protective coating, wherein the conformal protective coating is formed via an atomic layer deposition process comprising: contacting the interior surface of the component with a first molecular precursor in a gas phase for a period of time such that the first molecular precursor reacts to form a deposit on the interior surface of the component, wherein the component is a tube or channel, and the component is a liquid chromatography device, a gas chromatography device, or a micro fluidic device; removing unreacted first molecular precursor and reaction byproducts, if any, from the component; and contacting the interior surface of the component with a second molecular precursor in a gas phase for a period of time such that the second molecular precursor reacts with the deposit to form a conformal protective coating on the interior surface of the component. ### Claim 2 (depends on 1) The component of claim 1, wherein the component is a liquid chromatography device or a gas chromatography device. ### Claim 3 (depends on 1) The component of claim 1, wherein the component is composed of stainless steel, titanium, titanium alloy or a polymer. ### Claim 4 (depends on 1) The component of claim 1, wherein the lumen is characterized by an inner diameter of 10 mm or less and a length of 20 mm or more. ### Claim 5 (depends on 1) The component of claim 1, wherein the conformal protective coating has a substantially uniform thickness. ### Claim 6 (depends on 5) The component of claim 5, wherein the conformal protective ng has a substantially uniform thickness of 1 nm to 500 nm. ### Claim 7 (depends on 1) The component of claim 1, wherein the conformal protective coating comprises an inorganic compound selected from Si, Pt and Ru, or combinations thereof. ### Claim 8 (depends on 1) The component of claim 1, wherein the conformal protective coating comprises a material selected from Sift, SiC, Si3N4, SiOxCy (wherein 2x+4y=4), SiOxNy (wherein 2x+3y=4), SiCxHy (wherein 4x+y=4), TiO2, ZrO2, Al2O3, Y2O3, Ta2O5, and HfO2, or combinations thereof. ### Claim 9 (depends on 1) The component of claim 1, wherein the conformal protective coating comprises two or more layers each comprising a different material. ### Claim 10 An atomic layer deposition method for coating with a conformal protective coating an interior surface of a component having a lumen, the method comprising: contacting the interior surface of the component with a first molecular precursor in a gas phase for a period of time such that the first molecular precursor reacts to form a deposit on the interior surface of the component, wherein the component is a tube or channel, and the component is a liquid chromatography device, a gas chromatography device, or a micro fluidic device; removing unreacted first molecular precursor and reaction byproducts, if any, from the component; and contacting the interior surface of the component with a second molecular precursor in a gas phase for a period of time such that the second molecular precursor reacts with the deposit to form a conformal protective coating on the interior surface of the component. ### Claim 11 (depends on 10) The method of claim 10, further comprising removing unreacted second molecular precursor and reaction byproducts, if any, from the component. ### Claim 12 (depends on 11) The method of claim 11, wherein removing unreacted first molecular precursor and reaction byproducts comprises purging the component with an inert gas. ### Claim 13 (depends on 10) The method of claim 10, further comprising repeating the method to produce a desired thickness and/or composition of the conformal protective coating. ### Claim 14 (depends on 10) The method of claim 10, wherein the component is a liquid chromatography device or a gas chromatography device. ### Claim 15 (depends on 10) The method of claim 10 wherein the conformal protective coating has a substantially uniform thickness of 1 nm to 500 nm. ### Claim 16 (depends on 10) The method of claim 10, further comprising repeating the method using different molecular precursors to produce two or more layers each comprising a different protective material. ### Claim 17 (depends on 1) The component of claim 1, wherein the lumen has an inner diameter of 1 mm or less. ### Claim 18 (depends on 17) The component of claim 17, wherein the lumen has a length of 50 mm or more. ### Claim 19 (depends on 1) The component of claim 1, wherein the component is a liquid chromatography column or a gas chromatography column. ### Claim 20 (depends on 1) The component of claim 1, wherein the component is a microfluidic device that is a component of a gas chromatograph or a liquid chromatograph.