Continuous nanosynthesis apparatus and process

Patent metadata

Field	Value
Publication number	US-10112836-B2
Application number	US-201314090816-A
Country	US
Kind code	B2
Filing date	Nov 26, 2013
Priority date	Nov 26, 2012
Publication date	Oct 30, 2018
Grant date	Oct 30, 2018

Abstract

A nanosynthesis apparatus includes an outer tube and an inner tube with surfaces that oppose each other across a gap as part of a reaction chamber. A deposition fluid flows along the reaction chamber to grow nanostructures such as graphene or carbon nanotubes on a substrate in the reaction chamber. The reaction chamber may have an annular cross-section, and the growth substrate may wrap around the inner tube in a helical manner. This configuration can allow a flexible film substrate to travel through the reaction chamber along a path that is significantly longer than the length of the reaction chamber while maintaining a uniform gap between the substrate and the reaction chamber wall, which can facilitate a uniform temperature distribution and fluid composition across the width of the substrate.

First claim

The invention claimed is:

1. A nanosynthesis apparatus, comprising:
an outer tube having an internal surface;
an inner tube at least partially disposed within the outer tube, the inner tube having an external surface that opposes the internal surface of the outer tube across a gap having opposite first and second ends arranged along a longitudinal axis;
a feed system arranged to provide a growth substrate in the gap, wherein the growth substrate enters the gap at the first end of the gap, wraps at least partly around the inner tube in the gap, and exits the gap at the second end of the gap;
a deposition fluid source in fluid communication with the gap via an aperture formed through one of the tubes and located between the first and second ends of the gap, wherein an annealing zone is defined between the aperture and the first end of the gap and a growth zone is defined between the aperture and the second end of the gap;
a second fluid source coupled with the gap at the first end of the gap such that, in the presence of a pressure differential between the first and second ends of the gap, a second fluid from the second fluid source flows along the gap in an axial direction from the first end of the gap to the second end of the gap, the second fluid being confined to the gap while between the first and second ends of the gap;
a heater arranged to heat and control the temperature in at least a portion of the gap during operation of the apparatus,
wherein, in the presence of a pressure differential between the deposition fluid source and the second end of the gap, a deposition fluid flows from the deposition fluid source, into the gap through the aperture, and toward the second end of the gap, and
wherein, when both fluids are flowing along the gap, the gap is substantially free from the deposition fluid in the annealing zone and contains a mixture of both fluids in the growth zone.

2. A nanosynthesis apparatus as defined in claim 1 , wherein the outer and inner tubes are concentric.

3. A nanosynthesis apparatus as defined in claim 1 , wherein said internal and external surfaces are cylindrical.

4. A nanosynthesis apparatus as defined in claim 1 , wherein the outer and inner tubes are quartz tubes.

5. A nanosynthesis apparatus as defined in claim 1 , wherein the deposition fluid source is sealingly coupled with the inside of the inner tube at a first end of the inner tube and the aperture is formed through the inner tube and fluidly connects the inside of the inner tube with the gap, thereby fluidly connecting the deposition fluid source with the gap, the apparatus further comprising a partition located inside the inner tube between the aperture and the second end of the gap so that, in the presence of a pressure differential between the first end of the inner tube and the second end of the gap, the deposition fluid flows from the deposition fluid source, along the inside of the inner tube, through the aperture, into the gap, toward the second end of the gap, and away from the first end of the gap.

6. A nanosynthesis apparatus as defined in claim 1 , wherein the second fluid is a second deposition fluid.

7. A nanosynthesis apparatus as defined in claim 1 , wherein the second fluid is a conditioning fluid.

8. A nanosynthesis apparatus as defined in claim 1 , wherein the heater is a tube furnace adapted to circumscribe the outer tube along at least a portion the gap.

9. A nanosynthesis apparatus as defined in claim 1 , wherein the inner tube is adapted to rotate within the outer tube.

10. A nanosynthesis apparatus as defined in claim 1 , wherein the feed system is adapted to move the growth substrate through the gap along a helical path.

11. A nanosynthesis apparatus, comprising:
an outer tube having an internal surface and a longitudinal axis;
a substrate support surface at least partially disposed within the outer tube and opposing the internal surface of the outer tube across a gap having opposite ends and circumscribing the substrate support surface;
a deposition fluid source in fluid communication with the gap and operable to provide a deposition fluid to the gap such that the deposition fluid flows along the gap in a direction from one of the opposite ends toward the other of the opposite ends, wherein the deposition fluid comprises a constituent to be deposited on a growth substrate in the gap;
a heater arranged to heat at least a portion of the gap;
a feed system arranged to provide the growth substrate in the gap and onto the substrate support surface at an angle with respect to the longitudinal axis of the outer tube such that a length of the growth substrate wraps around and is in physical contact with the substrate support surface and extends between the ends of the gap, whereby the growth substrate is exposed to the deposition fluid flowing along the gap;
an inner tube that includes the substrate support surface, the deposition fluid source being in fluid communication with the inside of the inner tube; and
an aperture extending through the inner tube at a location between the ends of the gap, wherein the deposition fluid source is in fluid communication with the gap via the inner tube and the aperture such that the deposition fluid flows along only a portion of the gap.

12. A nanosynthesis apparatus as defined in claim 11 , wherein the feed system is configured to move the growth substrate through the gap in a direction from one end to the other end and in a first rotational direction about the longitudinal axis, and wherein the substrate support surface is configured to rotate about the longitudinal axis in a second rotational direction opposite from the first rotational direction.

13. A nanosynthesis apparatus as defined in claim 11 , wherein the gap has an annular cross-section.

14. A method of nanosynthesis, comprising the steps of:
(a) placing the growth substrate in a reaction chamber defined along the gap of the nanosynthesis apparatus of claim 11 ; and
(b) flowing the deposition fluid through at least a portion of the reaction chamber in the axial direction, whereby said constituent of the deposition fluid is deposited along the growth substrate as part of a nanostructure.

15. The method of claim 14 , wherein the growth substrate is arranged along a helical path while in the reaction chamber.

16. The method of claim 14 , further comprising the step of:
moving the growth substrate through the reaction chamber in the axial direction.

17. The method of claim 16 , further comprising the step of:
moving the growth substrate through the reaction chamber in an opposite axial direction.

18. The method of claim 14 , wherein the growth substrate is a metal foil.

19. The method of claim 14 , wherein nanoparticles are present along a surface of the growth substrate.

20. The method of claim 14 , wherein step (b) comprises flowing the deposition fluid into the reaction chamber at a location between the opposite ends of the gap.

21. The method of claim 20 , further comprising the step of flowing a second fluid through the reaction chamber so that the deposition fluid and the second fluid flow together along a portion of the reaction chamber.

22. The method of claim 21 , wherein the second fluid is a second deposition fluid.

23. The method of claim 21 , wherein the second fluid is a conditioning fluid.

24. The method of claim 21 , wherein at least one of the fluids is a gas.

25. The method of claim

Assignees

• Univ Michigan Regents

Inventors

• Hart Anastasios John
• Polsen Erik

Classifications

• C23C16/545

  for coating elongated substrates · CPC title

• C23C16/46

  characterised by the method used for heating the substrate (C23C16/48, C23C16/50 take precedence) · CPC title

• B05C3/005

  incorporating means for heating or cooling the liquid or other fluent material (B05C11/1042 takes precedence) · CPC title

• C30B25/08

  Reaction chambers; Selection of materials therefor · CPC title

• C01B33/021

  Preparation (chemical coating from the vapour phase C23C16/00) · CPC title