Granted Patent B2

US 12,517,026 · App. 17/923,429 · Granted Jan 6, 2026

Inventors: Norman J. Wagner (Newark, DE); Richard Dombrowski (Lutherville, MD); John W. Lim (Wilmington, DE); Yu-Jiun Lin (Newark, DE)

Assignee: STF Technologies, LLC

G01N11/162G01N2011/002G01N2011/008

Abstract

Claims (56)

1 . A sample cell for simultaneous measuring of rheological properties and interrogation of microstructure in all three primary planes defined by a simple shear field, the sample cell comprising:

a) a cell geometry comprising a cylinder; a shaft; a lateral wall and a sidewall, wherein the sidewall extends both above the lateral wall to form an upper circumferential lip and below the lateral wall to form a lower circumferential lip, and wherein the shaft extends axially from the lateral wall;

b) an enclosure comprising:

(i) a base portion comprising a bottom inner surface; and a lower groove configured to receive the lower circumferential lip of the cell geometry to allow rotation of the lower circumferential lip within the lower groove;

(ii) a cover portion comprising: (A) a top inner surface; (B) a bore for receiving the shaft of the cell geometry to allow rotation of the shaft within the bore; an upper groove configured to receive the upper circumferential lip of the cell geometry to allow rotation of the upper circumferential lip within the upper groove; and

(iii) a circumferential barrier wall that extends upwardly from the bottom inner surface of the base portion to the top inner surface of the cover portion thereby forming a circular compartment outwardly concentric to the cylinder of the cell geometry, wherein the cylinder of the cell geometry and the circumferential barrier wall form a concentric space for receiving a sample material;

c) a right-angle gear drive in mechanical communication with the shaft of the cell geometry and configured for mechanical communication with a rotational rheometer shaft; and

d) a coating disposed on surfaces within the circular compartment and further disposed on the cylinder of the cell geometry;

wherein the shaft is configured to rotate within the bore of the cover portion without making contact with the cover portion, the cylinder is configured to rotate within the enclosure without making contact with the base portion or the cover portion, and the coating prevents leakage of a sample material from the concentric space.

2 . The sample cell of claim 1 , wherein the coating is a hydrophobic coating selected from the group consisting of silicone, a combination polytetrafluoroethylene/silicone lubricant, polytetrafluoroethylene, a “lotus-leaf” inspired superhydrophobic coating, a nanoparticle coating, an oleophilic polymer, rubber, oil, a hydrocarbon greases, and any combination thereof.

3 . The sample cell of claim 1 , further comprising a sample material disposed within the concentric space, wherein the cylinder applies an external stress to the sample material when the shaft is rotated by the right-angle gear drive.

4 . The sample cell of claim 1 , wherein the right-angle gear drive further comprises a first drive shaft at an angle of about 90 degrees in relation to a second drive shaft, wherein the first drive shaft and the second drive shaft are supported by one or more bearings or bushings, and wherein the first drive shaft contacts the second drive shaft through a right-angle gearing.

5 . The sample cell of claim 1 , wherein:

(a) the base portion comprises at least one sidewall, wherein the sidewall comprises a first radiation beam window for receiving a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in a visible wavelength spectrum, ultraviolet radiation, and infrared radiation and a second radiation beam window for receiving a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in the visible wavelength spectrum, ultraviolet radiation, and infrared radiation; or

(b) the cover portion comprises a third radiation beam window for receiving a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in the visible wavelength spectrum, ultraviolet radiation, and infrared radiation; or

(c) both (a) and (b).

6 . The sample cell of claim 5 , wherein the first radiation beam window, the second radiation beam window, the cover portion, or any combination thereof comprise beryllium-quartz and the beam of radiation is X-ray and/or neutron radiation.

7 . The sample cell of claim 1 , wherein the right-angle gear drive is in mechanical communication with a rheometer.

8 . The sample cell of claim 1 , wherein the base portion is disposed on a heat exchanger configured to circulate fluid for controlling a temperature of the sample cell, the temperature selected from a temperature range of about −35 degrees C. to about 150 degrees C.

9 . A 4D-rheo assembly comprising:

(a) support assembly comprising a first cell support and a second cell support;

(b) a sample cell member comprising:

(i) a cell geometry comprising a cylinder and a shaft;

(ii) an enclosure comprising:

(1) a base portion comprising a bottom inner surface;

(2) a cover portion comprising: (A) a top inner surface; and (B) a bore configured to receive the shaft of the cell geometry to allow rotation of the shaft within the bore; and

(3) a circumferential barrier wall that extends upwardly from the bottom inner surface of the base portion to the top inner surface of the cover portion thereby forming a circular compartment outwardly concentric to the cylinder of the cell geometry whereby the cylinder of the cell geometry and the circumferential barrier wall form a concentric space configured to receive a sample material; and

(iii) a coating disposed on surfaces within the circular compartment and further disposed on the cylinder of the cell geometry;

wherein the shaft is configured to rotate within the bore of the cover portion without making contact with the cover portion, wherein the cylinder is configured to rotate within the enclosure without making contact with the base portion or the cover portion, and wherein the coating prevents leakage of a sample material from the concentric space; and

wherein, when the sample cell member is disposed on the first cell support in an XY orientation, the sample cell member is configured to receive a beam of radiation in 1-3, 2-3 shear planes; and wherein, when the sample cell member is disposed on the second cell support in an XYZ orientation, the shaft of the cell geometry is in mechanical communication with a right-angle gear drive and the sample cell member is configured to receive a beam of radiation in the 1-2 shear plane.

10 . The 4D-rheo assembly of claim 9 , wherein:

the cylinder of the cell geometry further comprises a lateral wall and a sidewall, wherein the sidewall extends both above the lateral wall to form an upper circumferential lip and below the lateral wall to form a lower circumferential lip, and wherein the shaft extends axially from the lateral wall;

the bottom inner surface further comprises a lower groove configured to receive the lower circumferential lip of the cell geometry to allow rotation of the lower circumferential lip within the lower groove; and

the top inner surface further comprises an upper groove configured to receive the upper circumferential lip of the cell geometry to allow rotation of the upper circumferential lip within the upper groove.

11 . The 4D-rheo assembly of claim 9 , wherein the coating is a hydrophobic coating or a hydrophilic coating.

12 . The 4D-rheo assembly of claim 11 , wherein the coating is a hydrophobic coating selected from the group consisting of silicone, a combination polytetrafluoroethylene/silicone lubricant, polytetrafluoroethylene, a “lotus-leaf” inspired superhydrophobic coating, a nanoparticle coating, an oleophilic polymer, rubber, oil, a hydrocarbon greases, and any combination thereof.

13 . The 4D-rheo assembly of claim 11 , wherein the coating is a hydrophilic coating selected from the group consisting of polyethyleneoxide, an amide, a polyimide, polyvinylpyrrolidone, polyvinyl alcohol, a polyurethane, polyacrylic acid, a polysaccharide, a Pluronic block copolymer, a biopolymer, and any combination thereof.

14 . The 4D-rheo assembly of claim 9 , wherein the base portion, cover portion, cylinder, circumferential barrier wall, or any combination thereof comprise a material selected from the group consisting of stainless steel, titanium, beryllium-quartz, and aluminum.

15 . The 4D-rheo assembly of claim 9 , wherein:

(a) the sample cell member is disposed on the first cell support in the XY orientation and the shaft of the cell geometry is configured for mechanical communication with a rheometer shaft; or

(b) wherein the sample cell member is disposed on the second cell support in the XYZ orientation and the shaft of the cell geometry is in mechanical communication with a right-angle gear drive, wherein the right-angle gear drive is configured for mechanical communication with a rheometer shaft.

16 . The 4D-rheo assembly of claim 15 , wherein the sample cell member is disposed on the second cell support in the XYZ orientation and the shaft of the cell geometry is in mechanical communication with a right-angle gear drive, wherein the right-angle gear drive further comprises a first drive shaft at an angle of about 90 degrees in relation to a drive second shaft, wherein the first drive shaft and the second drive shaft are supported by one or more bearings or bushings, and wherein the first drive shaft contacts the second drive shaft through a right-angle gearing.

17 . The 4D-rheo assembly of claim 9 , wherein:

(a) the base portion of the sample cell member comprises at least one sidewall, wherein the sidewall comprises a first radiation beam window configured to receive a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in a visible wavelength spectrum, ultraviolet radiation, and infrared radiation and a second radiation beam window configured to receive a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in the visible wavelength spectrum, ultraviolet radiation, and infrared radiation; or

(b) the cover portion of the sample cell member comprises a third radiation beam window configured to receive a beam of radiation selected from the group consisting of neutron radiation, X-ray radiation, photon radiation in the visible wavelength spectrum, ultraviolet radiation, and infrared radiation; or

(c) both (a) and (b).

18 . The 4D-rheo assembly of claim 17 , wherein the first radiation beam window, the second radiation beam window, the cover portion, or any combination thereof comprise beryllium-quartz and the beam of radiation is X-ray radiation or neutron radiation.

19 . The 4D-rheo assembly of claim 9 , wherein the shaft of the cell geometry is in mechanical communication with a rheometer.

20 . A method of analyzing a sample material, comprising:

(a) providing the 4D-rheo assembly of claim 9 ;

(b) disposing the sample material within the concentric space;

(c) rotating the shaft of the cell geometry whereby an external rotational stress is applied to the material;

(d) applying a beam of neutron radiation to the sample cell member; and

(e) detecting a scattering plane image.

21 . The method of claim 20 , wherein the sample material is a non-Newtonian sample material.

22 . The method of claim 20 , wherein the sample cell member is disposed on the second cell support in the XYZ orientation and the shaft of the cell geometry is in mechanical communication with a right-angle gear drive, wherein the right-angle gear drive is configured for mechanical communication with a rheometer shaft.

Assignments (2)

Continuity (2)

References Cited (24)