Additive manufacturing of microanalytical reference materials

Patent metadata

Field	Value
Publication number	US-12286355-B2
Application number	US-202016902076-A
Country	US
Kind code	B2
Filing date	Jun 15, 2020
Priority date	Aug 1, 2019
Publication date	Apr 29, 2025
Grant date	Apr 29, 2025

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.

First claim

What is claimed is:

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.

Assignees

• L Livermore Nat Security Llc

Inventors

• Sio Kin I
• Kuntz Joshua
• Lee Elaine
• Parsons-Davis Tashi
• Pascall Andrew
• Roberts Kevin E
• Bandong Bryan B
• Shusterman Jennifer A

Classifications

• B22F1/054

  Nanosized particles · CPC title

• B22F12/222

  for motion along a direction orthogonal to the plane of a layer · CPC title

• B22F10/10

  Formation of a green body · CPC title

• C25D15/02

  Combined electrolytic and electrophoretic processes {with charged materials} · CPC title

• C04B2237/341

  Silica or silicates · CPC title