# US 12,371,605 B2 · Thixotropic cement slurry with graphene oxide

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- Number: US 12,371,605 B2
- Document ID: US12371605B2
- Status: Granted
- Kind: B2
- Application number: 18/511,187
- Filed: 2023-11-16
- Published: 2025-05-22
- Granted: 2025-07-29
- Earliest claimed: 2023-11-16
- Assignees: Halliburton Energy Services, Inc.
- Applicants: Halliburton Energy Services, Inc.
- Inventors: Sandip Prabhakar Patil; Sourav Ghosh; Gauri Sudhir Bhide
- Web page: https://patentgrep.com/patent/US12371605B2

## CPC

- C09K 8/5045: {containing inorganic compounds}
- C04B 14/022: {Carbon}
- C04B 14/10: Clay {(sepiolite C04B14/042; grog C04B18/025)}
- C04B 18/146: {Silica fume}
- C04B 24/38: Polysaccharides or derivatives thereof {(C04B24/243 takes precedence)}
- C04B 28/02: containing hydraulic cements other than calcium sulfates
- C04B 28/04: Portland cements
- C09K 8/467: containing additives for specific purposes
- E21B 21/003: {Means for stopping loss of drilling fluid (plastering the borehole wall E21B33/138)}
- E21B 33/138: Plastering the borehole wall; Injecting into the formation
- C04B 2111/0012: {Thixotropic mixtures}
- C04B 2201/50: for the mechanical strength
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- E21B: EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS

## Abstract

A method of servicing a wellbore penetrating a subterranean formation with a thixotropic cement composition is provided. The thixotropic cement composition includes a cementitious material, silica fume, graphene oxide, and an aqueous fluid, can have a 10-minute gel strength of from about 20 lbf/100 ft2 to about 300 lbf/100 ft2, and can be used to service a wellbore (e.g., to reduce lost circulation in the wellbore). By incorporating graphene oxide into the thixotropic cement composition, the thixotropic cement composition can have a higher 10-minute gel strength than a reference composition absent the graphene oxide.

## Claims

### Claim 1

A method of servicing a wellbore penetrating a subterranean formation, the method comprising:
preparing a thixotropic cement composition, wherein the thixotropic cement composition comprises a cementitious material, silica fume, added graphene oxide, and an aqueous fluid, wherein the silica fume comprises an amount of graphene oxide ranging from equal to or greater than 0 to equal to or less than 0.5 percent by weight, wherein the added graphene oxide is in addition to the amount of graphene oxide in the silica fume, wherein the thixotropic cement composition comprises a total amount of graphene oxide, and wherein the total amount of the graphene oxide is greater than the amount of graphene oxide in the silica fume;
wherein the preparing further comprises selecting an amount of the added graphene oxide to provide the total amount of graphene oxide such that a 10-minute gel strength of the thixotropic cement composition is greater than a 10-minute gel strength of a reference composition, wherein the 10-minute gel strengths are measured in accordance with test standard API-RP-10B-2, and wherein the reference composition does not include the added graphene oxide and is otherwise identical to the thixotropic cement composition;
and
introducing the thixotropic cement composition into the wellbore and allowing the thixotropic cement composition to set.

### Claim 2 (depends on 1)

The method of claim 1, wherein the total amount of graphene oxide is in a range of from 0.1 to 5 percent graphene oxide by weight of cement (% bwoc).

### Claim 3 (depends on 1)

The method of claim 1, wherein the amount of the graphene oxide in the silica fume is greater than zero and less than or equal to 0.5 percent by weight.

### Claim 4 (depends on 1)

The method of claim 1, wherein the amount of the graphene oxide in the silica fume is equal to or greater than 0 to less than or equal to 0.4 percent graphene oxide by weight.

### Claim 5 (depends on 1)

The method of claim 1, wherein the 10-minute gel strength of the thixotropic cement composition is from 10lbr/100 ft2 to 300 lbr/100 ft2.

### Claim 6 (depends on 5)

The method of claim 5, wherein the 10-minute gel strength of the thixotropic cement composition is from 30 lbr/100 ft2 to 300 lbr/100 ft2.

### Claim 7 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition has a 10-second gel strength of from 5 lbf/100 ft2 to about-100 lbf/100 ft2, measured in accordance with test standard API-RP-10B-2.

### Claim 8 (depends on 1)

The method of claim 1, wherein the set thixotropic cement composition reduces lost circulation by reducing or preventing flow of a drilling fluid from the wellbore through a lost circulation zone and into an adjacent subterranean formation.

### Claim 9 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition comprises polysaccharide, and wherein the polysaccharide is present in an amount of from 0.001 to 10, from 0.01 to 5, or from 0.1 to 2 weight percent by weight of cement (% bwoc).

### Claim 10 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition comprises polysaccharide, and wherein the polysaccharide comprises diutan gum, welan gum, xanthan gum, guar gum or a combination thereof.

### Claim 11 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition comprises clay, and wherein the clay is present in an amount of from 0.01 to 50, from 0.01 to 25, or from 0.01 to 15 percent by weight of cement (% bwoc).

### Claim 12 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition comprises clay, and wherein the clay comprises sepiolite, montmorillonite, beidellite, nontronite, samonite, smectite, kaolinite, serpentine, illite, chlorite, saponite, fuller's earth, attapulgite, or a combination thereof.

### Claim 13 (depends on 1)

The method of claim 1, wherein the 10-minute gel strength of the thixotropic cement composition is greater than or equal to 30% of the 10-minute gel strength of the reference composition.

### Claim 14 (depends on 1)

The method of claim 1, wherein at atmospheric pressure and 3 rpm, the thixotropic cement composition has a rheology dial reading in a range of from 3 to 50 measured in accordance with test standard API-RP-10B-2.

### Claim 15 (depends on 1)

The method of claim 1, wherein the thixotropic cement composition has a thickening time to 70 Bearden units of Consistency (Bc) in a range of from 2 hours to 15 hours at 3,000 psi, measured in accordance with test standard API-RP-10B-2.
