IP Library › Granted Patent US 12,286,355
Granted Patent B2
US 12,286,355 · App. 16/902,076 · Granted Apr 29, 2025

Additive manufacturing of microanalytical reference materials

Inventors: Kin I Sio (Walnut Creek, CA); Joshua Kuntz (Livermore, CA); Elaine Lee (Brooklyn, NY); Tashi Parsons-Davis (Antioch, CA); Andrew Pascall (Livermore, CA); Kevin E. Roberts (Brentwood, CA); Bryan B. Bandong (Pleasanton, CA); Jennifer A. Shusterman (Pleasanton, CA)
Assignee: Lawrence Livermore National Security, LLC
C01B33/12B32B18/00B33Y10/00B33Y40/20B33Y70/00C25D13/02B22F1/054B22F10/10B22F12/222C01P2004/32C04B2237/341C25D15/02
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Quick Facts
Patent No.
US 12,286,355
App. No.
16/902,076
Granted
Apr 29, 2025
Kind
B2
Abstract

A method includes acquiring particles doped with at least one analyte and forming a monolithic reference material. The method includes forming includes using the analyte-doped particles as feedstock particles in an additive manufacturing process. A product includes a monolithic reference material formed of Stöber particles doped with a trace element. A method includes acquiring particles doped with platinum group elements (PGEs). The method includes forming a monolithic reference material using the PGE-doped particles as feedstock particles in an additive manufacturing process.

Claims (22)

1. A method, comprising:

acquiring Stöber particles doped with an analyte, wherein the analyte is a minor element or a trace element;

forming a monolithic reference material, wherein the forming includes using the analyte-doped particles as feedstock particles in an additive manufacturing process; and

heating the monolithic reference material for calcining and/or densifying the monolithic reference material thereby creating a calibration standard.

2. The method of claim 1 , wherein the additive manufacturing process includes electrophoretic deposition (EPD).

3. The method of claim 1 , wherein the heating includes sintering below a melting point of the analyte-doped particles for causing the densifying.

4. The method of claim 1 , wherein the heating occurs in a reducing atmosphere.

5. The method of claim 1 , wherein the heating occurs in an oxidizing atmosphere.

6. The method of claim 1 , wherein the analyte-doped particles include platinum group elements (PGEs) selected from the group consisting of: Ru, Rh, Pd, Os, Ir and Pt.

7. The method of claim 1 , wherein forming the reference material comprises controlling a concentration of the analyte in a bulk of the reference material.

8. The method of claim 1 , wherein forming the reference material comprises controlling the additive manufacturing process to create pre-defined patterns of the analyte-doped particles in geometries configured for microanalytical analyses.

9. The method of claim 1 , wherein acquiring the particles includes forming the particles in the presence of the analyte.

10. The method of claim 1 , wherein acquiring the particles includes doping synthesized particles.

11. The method of claim 1 , wherein the monolithic reference material has a predefined gradient of the analyte.

12. The method of claim 1 , wherein acquiring the particles includes forming the particles in the presence of a precursor of the analyte.

13. The method of claim 1 , wherein the monolithic reference material has a ruler formed therein to provide a distance metric.

14. The method of claim 1 , wherein the monolithic reference material is formed on a substrate, and comprising removing the formed monolithic reference material from the substrate.

15. The method of claim 14 , wherein acquiring the Stöber particles includes forming the analyte-doped particles via a modified Stöber reaction that occurs in the presence of the analyte.

16. The method of claim 1 , wherein the monolithic reference material is formed into a structure, and comprising calcining the formed structure for transforming the analyte-doped particles in the formed structure.

17. The method of claim 16 , comprising thermally processing the formed structure, the thermal processing including sintering below a melting point of the analyte-doped particles.

18. The method of claim 16 , wherein the formed structure has a predefined gradient of the analyte.

19. The method of claim 1 , wherein the formed monolithic reference material is self-supporting.

Assignments (3)
CORRECTIVE ASSIGNMENT TO CORRECT THE FIRST ASSIGNOR'S EXECUTION DATE ON THE COVER SHEET PREVIOUSLY RECORDED AT REEL: 056676 FRAME: 0550. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jul 15, 2021
From: SIO, KIN I; KUNTZ, JOSHUA; LEE, ELAINE; PARSONS-DAVIS, TASHI; PASCALL, ANDREW; ROBERTS, KEVIN E.; BANDONG, BRYAN B.; SHUSTERMAN, JENNIFER A.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 056918/0640 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 9, 2021
From: SIO, KIN I; KUNTZ, JOSHUA; LEE, ELAINE; PARSONS-DAVIS, TASHI; PASCALL, ANDREW; ROBERTS, KEVIN E.; BANDONG, BRYAN B.; SHUSTERMAN, JENNIFER A.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 056676/0550 →
CONFIRMATORY LICENSE (SEE DOCUMENT FOR DETAILS) Recorded Jul 24, 2020
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 053309/0802 →
Continuity (2)
Provisional Application 62881830 · Aug 1, 2019
Related Publication 20210032767A1 · Feb 4, 2021
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