Integrated monolithic microfabricated dispensing nozzle and liquid chromatography-electrospray system and method

• US 6,787,766 B2
• Filed: 04/30/2003
• Issued: 09/07/2004
• Est. Priority Date: 03/02/1999
• Status: Expired due to Term

• Current Assignee: Advion, Inc. (Beijing Bohui Innovation Biotechnology Group Co., Ltd.)
• Original Assignee: Advion BioSciences Incorporated
• Inventors: Schultz, Gary A., Corso, Thomas N.
• Primary Examiner(s): Wells, Nikita
• Application Number:
  US10/427,145
• Publication Number:
  US 20030189167A1
• Time in Patent Office: 496 Days
• Field of Search: 250/288, 250/281, 250/282, 250/423.R, 210/198.2, 210/243, 210/656
• US Class Current: 250/288
• CPC Class Codes: G01N 30/6095 Micromachined or nanomachined, e.g. micro- or nanosize
• CPC Class Codes: G01N 30/7266 by electric field, e.g. electrospray
• CPC Class Codes: H01J 49/0018 Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS]
• CPC Class Codes: H01J 49/167 Capillaries and nozzles specially adapted therefor; electrostatic spraying per se B05B5/00

Abstract

A droplet/electrospray device and a liquid chromatography-electrospray system are disclosed. The droplet/electrospray device comprises a substrate defining a channel between an entrance orifice on an injection surface and an exit orifice on an ejection surface, a nozzle defined by a portion recessed from the ejection surface surrounding the exit orifice, and an electrode for application of an electric potential to the substrate to optimize and generate droplets or an electrospray. A plurality of these electrospray devices can be used in the form of an array of miniaturized nozzles. The liquid chromatography-electrospray device comprises a separation substrate defining an introduction channel between an entrance orifice and a reservoir and a separation channel between the reservoir and an exit orifice, the separation channel being populated with separation posts perpendicular to the fluid flow. A cover substrate is bonded to the separation substrate to enclose the reservoir and the separation channel adjacent the cover substrate. The exit orifice of the liquid chromatography device is homogeneously interfaced with the entrance orifice of the electrospray device to form an integrated single system. Procedures for fabrication of the electrospray devices of the present invention are also disclosed.

Claims

1. An electrospray device comprising:

a substrate having an injection surface and an ejection surface opposing the injection surface, wherein the substrate is an integral monolith comprising;

an entrance orifice on the injection surface;

an exit orifice on the ejection surface;

a channel extending between the entrance orifice and the exit orifice;

a recess extending into the ejection surface and surrounding the exit orifice, thereby defining a nozzle on the ejection surface; and

a voltage application system comprising;

a first electrode attached to said substrate to impart a first potential to said substrate and

a second electrode to impart a second potential, wherein the first and the second electrodes are positioned to define an electric field surrounding the exit orifice,

wherein said substrate has a plurality of entrance orifices on the injection surface, a plurality of exit orifices on the ejection surface with each of the plurality of exit orifices corresponding to a respective one of the plurality entrance orifices, and a plurality of channels extending between one of the plurality of exit orifices and the corresponding one of the plurality of entrance orifices.

2. An electrospray device according to claim 1, wherein the exit orifices are present on the ejection surface of the substrate at a density of up to about 15,625 exit orifices/cm².

3. An electrospray device according to claim 2, wherein said density is about 15,625 exit orifices/cm².

4. An electrospray device according to claim 1, wherein the exit orifices are present on the ejection surface of the substrate at a density of up to about 27,778 exit orifices/cm².

5. An electrospray device according to claim 4, wherein said density is about 27,778 exit orifices/cm².

6. An electrospray device according to claim 1, wherein the exit orifices are present on the ejection surface of the substrate at a density of up to about 40,000 exit orifices/cm².

7. An electrospray device according to claim 6, wherein said density is about 40,000 exit orifices/cm².

8. An electrospray device according to claim 6, wherein the exit orifices are present on the ejection surface of the substrate at a density of up to about 62,500 exit orifices/cm².

9. An electrospray device according to claim 8, wherein said density is about 62,500 exit orifices/cm².

10. An electrospray device according to claim 1, wherein the exit orifices are present on the ejection surface of the substrate at a density of up to about 160,000 exit orifices/cm².

11. An electrospray device according to claim 10, wherein said density is about 160,000 exit orifices/cm².

12. An electrospray device comprising:

a) a substrate comprising;

an entrance orifice on an injection surface;

an exit orifice defining a nozzle on an ejection surface;

a channel extending between the entrance orifice and the exit orifice, thereby defining a fluid passage, wherein at least all fluid contacting surfaces of the device are coated with a moisture barrier; and

b) a voltage application system comprising;

a first electrode positioned to impart a first potential to said substrate and

a second electrode electrically isolated from said first electrode and positioned to impart a second potential to fluid passing though the device, wherein said first and second electrodes are positioned to define an electric field surrounding the nozzle.

13. An electrospray device according to claim 12, wherein said moisture barrier comprises a layer up to about 2 μ

m in thickness.

14. An electrospray device according to claim 12, wherein said moisture barrier comprises a layer of silicon nitride.

15. An electrospray device according to claim 12, wherein at least all fluid contacting surfaces of the device are coated with an insulating layer.

16. An electrospray device according to claim 15, wherein said insulating layer comprises silicon dioxide, silicon nitride, or combinations thereof.

17. An electrospray device according to claim 12, wherein said channel is a through-substrate channel.

18. An electrospray device according to claim 12, wherein said nozzle is defined by a recess surrounding the exit orifice and extending into the ejection surface.

19. An electrospray device according to claim 12, wherein said substrate injection surface opposes said ejection surface.

20. An electrospray device according to claim 12, wherein said nozzle has a cross-sectional area of less than about 3000 μ

m².

21. An electrospray device according to claim 12, wherein application of potentials to said first and second electrodes causes fluid passing through said electrospray device to discharge from the exit orifice in the form of a spray.

22. An electrospray device according to claim 12, wherein application of potentials to said first and second electrodes causes fluid passing through said electrospray device to discharge from the exit orifice in the form of droplets.

23. An electrospray device according to claim 12, wherein said substrate is silicon.

24. An electrospray device according to claim 12, wherein said substrate is polymeric.

25. An electro spray device according to claim 12, wherein said substrate is glass.

26. An electrospray device according to claim 12, wherein said substrate has a plurality of entrance orifices on the injection surface, a plurality of exit orifices on the ejection surface with each of the plurality of exit orifices corresponding to a respective one of the plurality entrance orifices, and a plurality of channels extending between one of the plurality of exit orifices and the corresponding one of the plurality of entrance orifices.

27. An electrospray device according to claim 12, further comprising:

a conduit positioned to provide fluid to the entrance orifice.

28. A system for processing droplets/sprays of fluid comprising:

an electrospray device according to claim 12 and

a device to receive droplets/sprays of fluid from the exit orifice of said electrospray device.

29. A system according to claim 28, wherein said substrate has a plurality of entrance orifices on the injection surface, a plurality of exit orifices on the ejection surface with each of the plurality of exit orifices corresponding to a respective one of the plurality entrance orifices, and a plurality of channels extending between one of the plurality of exit orifices and the corresponding one of the plurality of entrance orifices, said device to receive fluid droplets/sprays comprising:

a daughter plate have a plurality of fluid receiving wells each positioned to receive fluid ejected from a respective one of the exit orifices.

30. A system according to claim 28, wherein said device to receive droplets/sprays of fluid is a mass spectrometry device.

31. A system for processing droplets/sprays of fluid comprising:

an electrospray device according to claim 12 and

a device to provide fluid to the entrance orifice of said electrospray device.