Graphene-based electro-microfluidic devices and methods for protein structural analysis

Patent metadata

Field	Value
Publication number	US-11175244-B2
Application number	US-201916444240-A
Country	US
Kind code	B2
Filing date	Jun 18, 2019
Priority date	Jun 19, 2018
Publication date	Nov 16, 2021
Grant date	Nov 16, 2021

Abstract

The invention provides a novel microfluidic platform for use in electro-crystallization and electro-crystallography experiments. The manufacturing and use of graphene as X-ray compatible electrodes allows the application of electric fields on-chip, during X-ray analysis. The presence of such electric fields can be used to modulate the structure of protein (or other) molecules in crystalline (for X-ray diffraction) or solution form (for X-ray scattering). Additionally, the presence of an electric field can be used to extend the lifetime of fragile samples by expediting the removal of reactive secondary radiation damage species.

First claim

What is claimed is:

1. An electro-microfluidic device, comprising:
a top layer comprising a top support layer and one or more top layers of graphene, wherein each top layer of the one or more top layers of graphene comprises an optically-clear top window area;
a bottom layer comprising a bottom support layer and one or more bottom layers of graphene, wherein each bottom layer of the one or more bottom layers of graphene comprises an optically-clear bottom window area;
a middle layer sandwiched between the one or more top layers of graphene and the one or more bottom layers of graphene having a patterned cavity defining a sample holding chamber;
a cathode electrically connected to a proximal portion of the one or more top layers of graphene or the one or more bottom layers of graphene; and
an anode electrically connected to a distal portion of the one or more top layers of graphene or the one or more bottom layers of graphene configured to allow an application of an electric field within or across the sample holding chamber;

wherein the optically-clear top window area comprises at least a portion of the one or more top layers of graphene, and the optically-clear bottom window area comprises at least a portion of the one or more bottom layers of graphene.

2. The electro-microfluidic device of claim 1 , further comprising:
an inlet port in a fluidic communication with the sample holding chamber; and
an outlet port in a fluidic communication with the sample holding chamber.

3. The electro-microfluidic device of claim 1 , wherein the top support layer comprises a UV curable plastic material, a glass, silicon, a silicon nitride material, or a thermal plastic material.

4. The electro-microfluidic device of claim 1 , wherein the bottom support layer comprises a UV curable plastic material, a glass, silicon, a silicon nitride material, or a thermal plastic material.

5. The electro-microfluidic device of claim 1 , further comprising:
an adhesive layer,

wherein the top layer and the middle layer are joined together by the adhesive layer therebetween.

6. The electro-microfluidic device of claim 5 , further comprising:
an adhesive layer,

wherein the bottom layer and the middle layer are joined together by the adhesive layer therebetween.

7. The electro-microfluidic device of claim 1 , wherein the sample holding chamber is from 10 pL to 10 μL in volume.

8. The electro-microfluidic device of claim 1 , wherein an overall thickness between the top layer and the bottom layer is from 10 μm to 1 mm.

9. The electro-microfluidic device of claim 1 , wherein each of the top layer and the bottom layer comprises a single graphene film having a size from 2 mm 2 to 60 cm 2 .

10. The electro-microfluidic device of claim 9 , wherein the single graphene film is patterned.

11. The electro-microfluidic device of claim 1 , wherein each of the top layer and the bottom layer comprises a single graphene film having a thickness from one atomic layer to 10 atomic layers.

12. The electro-microfluidic device of claim 11 , wherein each of the top layer and the bottom layer comprises a graphene film of one atomic layer.

13. The electro-microfluidic device of claim 1 , wherein each of the optically-clear top window area and the optically-clear bottom window area is from 100 μm 2 to 1 cm 2 in size.

14. The electro-microfluidic device of claim 1 , wherein the one or more top layers of graphene and the one or more bottom layers of graphene serve as a vapor diffusion barrier.

15. The electro-microfluidic device of claim 1 , wherein the one or more top layers of graphene and the one or more bottom layers of graphene serve as a diffusion barrier to one or more of water vapor, O 2 , CO, CO 2 , water, and Xe.

16. An array device comprising:
two or more electro-microfluidic devices according to claim 1 .

17. A method for growing crystalline or non-crystalline materials, comprising: growing one or more crystalline or non-crystalline materials in a sample holding chamber of an electro-microfluidic device of claim 1 under a controlled application of an electric field.

18. A method of electro-crystallization and X-ray scattering analysis or X-ray diffraction analysis, comprising:
growing one or more crystalline or non-crystalline materials in a sample holding chamber of an electro-microfluidic device of claim 1 , optionally under a controlled application of an electric field;
directing an X-ray beam to the one or more crystalline or non-crystalline materials via an optically-clear top window area or an optically-clear bottom window area of the electro-microfluidic device; and
measuring X-ray scattering or X-ray diffraction of the one or more crystalline or non-crystalline materials via the optically-clear bottom window area or the optically-clear top window area of the electro-microfluidic device.

19. A method for fabricating an electro-microfluidic device, comprising:
providing a first graphene film comprising one or more layers of graphene and a second graphene film comprising one or more layers of graphene;
transferring the first graphene film to a support layer forming a top layer with a window area defined by the first graphene film;
transferring the second graphene film to a support layer forming a bottom layer with a window area defined by the second graphene film;
forming an electro-microfluidic device by bonding a middle layer having a pattern to and between the top layer and the bottom layer to form a sandwiched construct having:
a cavity for holding a sample defined by the top layer and bottom layer and the pattern of the middle layer, and
a first channel and a second channel connecting to the second graphene film at a proximal location and a distal location; and

providing a conductive material to the first channel and second channel so as to form an electric connectivity to the second graphene film.

20. A device comprising:
an electro-microfluidic device fabricated by the method of claim 19 .

Assignees

• Univ Massachusetts

Inventors

• Perry Sarah L
• Sui Shou

Classifications

• G01N23/2076

  for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS · CPC title

• G01N23/201

  by measuring small-angle scattering · CPC title

• G01N23/20066

  Measuring inelastic scatter of gamma rays, e.g. Compton effect · CPC title

• G01N23/2204

  Specimen supports therefor; Sample conveying means therefore · CPC title

• B01D9/0063

  Control or regulation (control per se G05) · CPC title