Fabrication of mass spectrometry surface

Patent metadata

Field	Value
Publication number	US-11164733-B2
Application number	US-201615759192-A
Country	US
Kind code	B2
Filing date	Oct 5, 2016
Priority date	Oct 7, 2015
Publication date	Nov 2, 2021
Grant date	Nov 2, 2021

Abstract

Disclosed herein are compositions for ionizing a target and methods for making the compositions. In some embodiments, the compositions can include a structured substrate having a plurality of upright surface features, for example, microscale or nanoscale pillars, in contact with an initiator. Also disclosed herein are methods for ionizing targets.

First claim

What is claimed is:

1. A composition for ionizing a target, comprising:
a structured semiconductor substrate comprising a plurality of microscale or nanoscale conical pillars formed by etching the structured semiconductor substrate with an inductively coupled plasma, wherein all of the plurality of microscale or nanoscale pillars in the structured semiconductor substrate are upright in orientation, wherein the height of the plurality of microscale or nanoscale pillars ranges from about 50 nm to about 10 μm; and
an initiator for promoting ionization of an irradiation-ionizable target, wherein the initiator is reversibly absorbed onto the surface of the structured semiconductor substrate comprising the plurality microscale or nanoscale pillars and trapped by two or more of the plurality of microscale or nanoscale pillars, wherein the structured semiconductor substrate undergoes surface reorganization upon laser irradiation resulting in ionization of the target, whereby the height of microscale or nanoscale pillars of the plurality of microscale or nanoscale pillars decreases and/or the width of nanoscale or nanoscale pillars of the plurality of microscale or nanoscale pillars increases, thereby enhancing the ionization of the target.

2. The composition of claim 1 , wherein the structured semiconductor substrate comprises a semiconductor selected from the group consisting of Group IV semiconductors, diamond, Group I-VII semiconductors, CuF, CuCl, CuBr, CuI, AgBr, AgI, Group II-VI semiconductors, BeO, BeS, BeSe, BeTe, BePo, MgTe, ZnO, ZnS, ZnSe, ZnTe, ZnPo, CdS, CdSe, CdTe, CdPo, HgS, HgSe, HgTe, Group III-V semiconductors, BN, BP, BAs, AlN, AlP, AlAs, AlSb, GaN, GaP, GaSb, InN, InAs, InSb, sphaelerite structure semiconductors, MnS, MnSe, 3-SiC, Ga 2 Te 3 , In 2 Te 3 , MgGeP 2 , ZnSnP 2 , ZnSnAs 2 , Wurtzite Structure Compounds, NaS, MnSe, SiC, MnTe, Al 2 S 3 , Al 2 Se 3 , I-II-VI2 semiconductors, CuAlS 2 , CuAlSe 2 , CuAlTe 2 , CuGaS 2 , CuGaSe 2 , CuGaTe 2 , CuInS 2 , CuInSe 2 , CuInTe 2 , CuTiS 2 , CuTiSe 2 , CuFeS 2 , CuFeSe 2 , CuLaS 2 , AgAS 2 , AgAlSe 2 , AgAlTe 2 , AgGaS 2 , AgGaSe 2 , AgGaTe 2 , AgInS 2 , AgInSe 2 , AgInTe 2 , AgFeS 2 , and silicon.

3. The composition of claim 1 , wherein the plurality of pillars comprises two or more semiconductor pillars.

4. The composition of claim 1 , wherein the initiator is a fluorinated molecule.

5. The composition of claim 1 , wherein the initiator is selected from the group consisting of lauric acid, polysiloxanes, chlorosilanes, methoxy silanes, ethyoxy silanes, fluorous siloxanes and fluorous silanes.

6. The composition of claim 1 , wherein the structured semiconductor substrate is a black silicon substrate.

7. The composition of claim 1 , wherein the aspect ratio of the plurality of pillars ranges from about 1 to about 10.

8. The composition of claim 1 , further comprising a target in contact with the initiator.

9. The composition of claim 8 , wherein the target is a constituent of a sample selected from a biological sample, an environmental sample, a clinical sample, a forensic sample, or a combination thereof.

10. A method for ionizing a target, comprising:
providing a structured semiconductor substrate having a plurality of microscale or nanoscale conical pillars formed by etching the structured semiconductor substrate with an inductively coupled plasma, wherein all of the plurality of microscale or nanoscale pillars in the structured semiconductor substrate are upright in orientation, wherein the height of the plurality of microscale or nanoscale pillars ranges from about 50 nm to about 10 μm;
applying an initiator to the structured semiconductor substrate, thereby the initiator is reversibly absorbed onto the surface of the structured semiconductor substrate having the plurality of microscale or nanoscale pillars and trapped by two or more of the plurality of microscale or nanoscale pillars;
delivering a target to the structured semiconductor substrate that the initiator is reversibly absorbed onto to form a target-loaded substrate; and
irradiating the target-loaded substrate, thereby ionizing the target, wherein upon said irradiation resulting in the ionization of the target, the target-loaded substrate undergoes surface reorganization, whereby the height of microscale or nanoscale pillars of the plurality of microscale or nanoscale pillars decreases and/or the width of microscale or nanoscale pillars of the plurality of microscale or nanoscale pillars increases, and wherein the surface reorganization enhances the ionization of the target.

11. A method for making a composition for ionizing a target, comprising:
providing a semiconductor material;
etching the semiconductor material in the presence of an inductively coupled plasma to produce a structured semiconductor substrate, wherein the structured semiconductor substrate comprises a plurality of microscale or nanoscale conical pillars and all of the plurality of microscale or nanoscale pillars in the structured semiconductor substrate are upright in orientation, wherein the height of the plurality of microscale or nanoscale pillars ranges from about 50 nm to about 10 μm; and
contacting the structured semiconductor substrate with an initiator, thereby the initiator is reversible absorbed onto the surface of the structured semiconductor substrate comprising the plurality of microscale or nanoscale pillars and trapped by two or more of the plurality of microscale or nanoscale pillars, wherein upon laser irradiation of the structured semiconductor substrate resulting in ionization of a target, the structured semiconductor substrate undergoes surface reorganization comprising the height of one or more microscale or nanoscale pillars of the plurality of microscale or nanoscale pillars decreasing and/or the width of one or more microscale or nanoscale pillars of the plurality of microscale or nanoscale pillars increasing, and wherein the surface reorganization enhances the ionization of the target.

12. The composition of claim 1 , wherein the structured semiconductor substrate is a p-type semiconductor, wherein the semiconductor is crystalline silicon, and wherein the semiconductor has a <100> orientation.

13. The composition of claim 1 , wherein the initiator is trapped by at least half of the plurality of microscale or nanoscale pillars.

14. The composition of claim 1 , wherein the initiator desorbs from the surface of the structured semiconductor substrate upon an increase and/or a decrease in temperature to form a visible film on the structured semiconductor substrate.

15. The composition of claim 1 , wherein at least one of the plurality of microscale or nanoscale pillars has a conical shape and/or a triangular sloped surface.

16. The composition of claim 1 , wherein at least one of the plurality of microscale or nanoscale pillars has a non-cylindrical shape.

17. The method of claim 10 , wherein the initiator is a fluorinated molecule.

18. The method of claim 10 , wherein the initiator is selected from the group consisting of lauric acid, polysiloxanes, chlorosilanes, methoxy silanes, ethyoxy silanes, fluorous siloxanes and fluorous silanes.

19. The method of claim 10 , wherein the average aspect ratio of the plurality of pillars is about 1 to about 10.

20. The method of claim 10 , wherein the target is a constituent of a sample selected from a biological sample, an environmental sample, a clinical sample, a forensic sample, or a combination thereof.

Assignees

• Univ California

Inventors

• Gao Jian
• Northen Trent R

Classifications

• B82Y40/00 Primary

  Manufacture or treatment of nanostructures · CPC title

• H01J49/00

  Particle spectrometers or separator tubes · CPC title

• H01J49/161

  using photoionisation, e.g. by laser · CPC title

• H01J49/0409

  Sample holders or containers (containers for retaining a material to be analyzed, B01L3/50, for DNA, C12Q1/6834, for biological materials, G01N33/543) · CPC title

• H01J49/0418 Primary

  for laser desorption, e.g. matrix-assisted laser desorption/ionisation [MALDI] plates or surface enhanced laser desorption/ionisation [SELDI] plates · CPC title