Diamond rotors for MAS-NMR

Patent metadata

Field	Value
Publication number	US-11999006-B2
Application number	US-202017098359-A
Country	US
Kind code	B2
Filing date	Nov 14, 2020
Priority date	Nov 14, 2019
Publication date	Jun 4, 2024
Grant date	Jun 4, 2024

Abstract

A method for fabricating MAS NMR rotors and drive caps made of diamond to increase the maximum achievable spinning frequency and enhance MAS NMR sensitivity and resolution. Diamond is an excellent choice for making MAS NMR rotors due to its high tensile and flexural strength, however, micromachining diamond is difficult due to its hardness. Although laser cutting is often employed to cut diamond sheets, this process cannot be used to create the high aspect ratio and small features required for MAS NMR rotors. In the present invention, a laser micromachining process is used to create the desired high aspect ratio while maintaining the small lateral features. In this process, the laser is used to first convert the diamond into graphite followed by a conversion to carbon dioxide in the presence of oxygen. To create a rotor, a rectangular log has a center hole drilled by the laser, and is then micromachined into a hollow cylinder.

First claim

We claim:

1. A method for micromachining a diamond rotor comprising:
cutting a rectangular log of diamond using a diamond cutting process;
drilling a hole lengthwise through the log using a pulsed laser with wavelength, pulse duration and pulse power sufficient to convert diamond to graphite and subsequently convert the graphite to carbon dioxide or carbon monoxide in ambient air;
rotating the log in a laser beam to micromachine the log into a cylinder.

2. The method of claim 1 wherein the rotor has a final outside diameter between 0.1 mm and 4 mm and an inside diameter is between 10% to 90% of the outside diameter.

3. The method of claim 1 wherein the log has dimensions greater than the diamond rotor being machined.

4. The method of claim 1 wherein the wavelength is approximately 532 nm.

5. The method of claim 1 wherein the laser has a penetration depth of approximately 1.1 mm.

6. The method of claim 1 further comprising drilling the hole in steps, wherein each step creates a pocket of predetermined depth z mm.

7. The method of claim 6 further comprising increasing an optical focal point of the laser downward z mm as each pocket is completed until the hole totally penetrates the log.

8. The method of claim 1 wherein the diamond log is a chemical vapor deposition (CVD) diamond.

9. A method of micromachining a diamond rotor comprising:
obtaining a sheet of chemical vapor deposition (CVD) grown diamond;
measuring transmission and absorption of the diamond to determine optimum laser wavelength, pulse duration and pulse power;
cutting from the sheet a rectangular log of diamond using a laser cutting process;
mounting the rectangular log, and using a top-down pulsed laser with adjustable optical focal length, cutting a circular hole longitudinally through the log from a top end to a bottom end using the following steps:
(a) Cutting a pocket of predetermined depth z with the laser by converting diamond material in the cut to graphite with the laser, and then oxidizing it to carbon dioxide by heat from the laser using oxygen from ambient air;
(b) Moving focal length downward a distance z and repeating step (a) until a final pocket penetrates the bottom of the log to produce a drilled log;
rotating the drilled log, micromachining the log into a cylinder using the laser to shave material from the log as it rotates.

10. The method of claim 9 wherein the rotor has a final outside diameter between 0.1 mm and 4 mm and the inside diameter is between 10% to 90% of the outside diameter.

11. The method of claim 9 wherein the log has dimensions greater than the diamond rotor being machined.

12. The method of claim 9 wherein the wavelength is approximately 532 nm.

13. The method of claim 9 wherein the laser has a penetration depth of approximately 1.1 mm.

14. The method of claim 9 wherein the diamond log is a chemical vapor deposition (CVD) diamond.

15. A method of laser drilling of diamond comprising:
measuring a light transmission and absorption spectrum for a chosen diamond material;
using the light transmission and absorption spectrum, choosing a laser wavelength, pulse duration and pulse power sufficient to convert the diamond to graphite;
drilling a hole with the laser by converting diamond material in the hole to graphite and subsequently oxidizing it to carbon dioxide using oxygen from ambient air.

16. The method of claim 15 wherein the wavelength is approximately 532 nm.

17. The method of claim 15 wherein the laser has a penetration depth of approximately 1.1 mm.

18. The method of claim 15 further comprising drilling the hole in steps, wherein each step creates a pocket of predetermined depth z mm.

19. The method of claim 18 further comprising increasing an optical focal point of the laser downward z mm as each pocket is completed until the hole is completed.

Assignees

• Massachusetts Inst Technology

Inventors

• Patil Prashant
• Banks Daniel
• Bahri Salima
• Langford William
• Blackburn Camron
• Fredin Zachary
• Griffin Robert
• Gershenfeld Neil

Classifications

• B23K26/0006 Primary

  taking account of the properties of the material involved (B23K26/32, B23K26/40 take precedence) · CPC title

• B23K26/55

  for creating voids inside the workpiece, e.g. for forming flow passages or flow patterns · CPC title

• B28D5/0058

  Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material (B28D5/0005, B28D5/024 take precedence) · CPC title

• B28D5/0082

  for supporting, holding, feeding, conveying or discharging work · CPC title

• G01R33/307

  specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer · CPC title