Testing device and method for measuring adhesion force between gas hydrate and mineral particles

Patent metadata

Field	Value
Publication number	US-10775406-B2
Application number	US-201916509495-A
Country	US
Kind code	B2
Filing date	Jul 12, 2019
Priority date	Nov 30, 2018
Publication date	Sep 15, 2020
Grant date	Sep 15, 2020

Abstract

A testing device for testing adhesion force includes a thermal insulated glove box, an atomic force microscope, a cryogenic sample stage, a high pressure gas source and a circulating chiller. The atomic force microscope includes a probe for adhering mineral particles. The cryogenic sample stage is configured for preparing gas hydrate sample. The cryogenic sample stage is arranged below the probe. The atomic force microscope and the cryogenic sample stage are placed in the thermal insulated glove box. The high pressure gas source provides pressure required for synthesis of gas hydrates, the high pressure gas source comprises a high pressure chamber covered on the cryogenic sample stage and a high pressure gas cylinder connected with the high pressure chamber. The circulating chiller, an outlet of the circulating chiller is connected with the thermal insulated glove box to control humidity and temperature inside the thermal insulated glove box.

First claim

What is claimed is:

1. A testing device for testing adhesion force between gas hydrate and mineral particles comprising: a thermal insulated glove box;
an atomic force microscope for measuring adhesion force and sticking mineral particles by manipulating the probe; a cryogenic sample stage for preparing gas hydrate sample, the cryogenic sample stage is fixed on the carrier stage of the atomic force microscope, So the cryogenic sample stage can move in the horizontal plane by manipulating the carrier table, wherein the atomic force microscope and the cryogenic sample stage are placed in the thermal insulated glove box;
a high pressure gas source provides pressure required for synthesis of gas hydrates, the high pressure gas source comprises a high pressure chamber covered on the cryogenic sample stage and a high pressure gas cylinder connected with the high pressure chamber; and
a circulating chiller, an outlet of the circulating chiller is connected with the thermal insulated glove box to control humidity and temperature inside the thermal insulated glove box.

2. The testing device of claim 1 , wherein:
the testing device further comprises a pump and a liquid nitrogen tank, the pump is configured to pump low temperature nitrogen vaporized from liquid nitrogen tank to the cryogenic sample stage for refrigeration of the cryogenic sample stage.

3. The testing device of claim 1 , wherein:
the thermal insulated glove box is an airtight thermal insulated glove box, and the inner surface of the thermal insulated glove box is attached a thermal insulating layer.

4. The testing device of claim 1 , wherein:
the circulating chiller extracts the air in the thermal insulated glove box, and then pump it into the thermal insulated glove box after cooling.

5. The testing device of claim 1 , wherein:
temperature of the cryogenic sample stage is controlled in a range from minus 190° C. to 25° C.

6. The testing device of claim 1 , wherein:
the high pressure cavity is sealed connecting with the cryogenic sample stage.

7. The testing device of claim 1 , wherein:
the probe comprises a cantilever, and back of the cantilever is coated with an aluminum layer or a gold coating layer.

8. The testing device of claim 7 , wherein:
a cantilever of the probe is rectangular, and the probe has no tip.

9. A method for testing adhesion force between gas hydrate and mineral particles comprising:
providing a testing device, wherein the testing device comprises:
a thermal insulated glove box;
an atomic force microscope comprising a probe for adhering mineral particles;
a cryogenic sample stage for preparing gas hydrate sample, wherein the cryogenic sample stage is arranged on the carrier stage of the atomic force microscope, and wherein the atomic force microscope and the cryogenic sample stage are placed in the thermal insulated glove box;
a high pressure gas source provides pressure required for synthesis of gas hydrates, the high pressure gas source comprises a high pressure chamber covered on the cryogenic sample stage and a high pressure gas cylinder connected with the high pressure chamber; and
a circulating chiller, an outlet of the circulating chiller is connected with the thermal insulated glove box to control humidity and temperature inside the thermal insulated glove box;
adhering mineral particles on the end of the probe;
preparing gas hydrate sample;
adjusting temperature of air inside the insulation glove box; and
testing adhesion force between the gas hydrate and the mineral particles.

10. The method of claim 9 , wherein:
the step of adhering mineral particles using the probe comprising:
providing a plurality of mineral particles;
dispersing the mineral particles in water or anhydrous ethanol;
disposing a substrate on the cryogenic sample stage;
dripping a small amount of cloud droplets on a surface of the substrate;
dipping a small amount of glue with a fine rod, and drawing a line on the surface of the substrate using the fine rod, and the glue showing a linear shape attachment to the surface of the substrate;
using the atomic force microscope to manipulate the probe, to let the end of the probe dip the glue and adhere the mineral particles.

11. The method of claim 10 , wherein:
the step of preparing gas hydrate sample comprising:
dripping a small amount of deionized water on the substrate, and lower temperature of the deionized water below zero degrees Celsius;
covering the high pressure cavity on the cryogenic sample stage;
pumping high pressure gases into the high pressure cavity until pressure stabilizes of the high pressure cavity; and
adjusting the temperature below the phase equilibrium temperature of gas hydrate at atmospheric pressure.

12. The method of claim 11 , wherein:
the step of adjusting temperature of air inside the insulation glove box comprises:
adjusting temperature of an outlet of the circulating chiller to let temperature of air in the insulation glove box is lower than temperature of the cryogenic sample stage, and a temperature difference is ΔT, and ΔT meets the formula:

Δ
⁢

⁢
T

=

1000
⁢

kPL

λ
⁢

⁢
BD

wherein in the formula, k refers to a ratio of laser heat conversion, and k≈0.1; P refers to laser power, and P≈1 mW; λ refers to a thermal conductivity of the probe, the unit is W/° C.·m, L refers to a length of the probe, and unit of L is μm; B refers to a width of the probe, and unit of B is μm; and D refers to thickness of the probe, and unit of D is μm.

Assignees

• Univ China Geosciences Wuhan

Inventors

• Ning Fulong
• Peng Li
• Li Wei
• Wang Dongdong
• Ou Wenjia
• Liu Zhichao
• Sun Jiaxin
• Cheng Wan
• Jiang Guosheng
• Zhang Ling

Classifications

• E21B49/0875

  determining specific fluid parameters · CPC title

• E21B49/08

  Obtaining fluid samples or testing fluids, in boreholes or wells · CPC title

• G01Q30/12 Primary

  Fluid environment · CPC title

• G01Q30/10

  Thermal environment · CPC title

• G01Q10/045

  Self-actuating probes, i.e. wherein the actuating means for driving are part of the probe itself, e.g. piezoelectric means on a cantilever probe · CPC title