# US 12,595,410 B2 · Luminescent diamond > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 12,595,410 B2 - Document ID: US12595410B2 - Status: Granted - Kind: B2 - Application number: 18/005,115 - Filed: 2021-07-14 - Published: 2023-08-17 - Granted: 2026-04-07 - Earliest claimed: 2020-07-14 - Assignees: Schlumberger Technology Corporation - Applicants: Schlumberger Technology Corporation - Inventors: Yahua Bao; J. Daniel Belnap - Web page: https://patentgrep.com/patent/US12595410B2 ## CPC - C01B 32/25: Diamond - C09K 11/65: containing carbon (in organic compounds C09K11/06) - C01B 32/28: After-treatment, e.g. purification, irradiation, separation or recovery - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE ## Abstract Luminescent diamond is made by subjecting a volume of diamond grains to high-pressure/high-temperature conditions with or without a catalyst or pressure transfer media to cause the grains to undergo plastic deformation to produce nitrogen vacancy defects, increasing the luminescent activity/intensity of the resulting diamond material. The consolidated diamond material may be further treated to further increase luminescent activity/intensity including reducing the consolidated diamond material to diamond particles, heat treatment in vacuum, and/or air heat treatment. The resulting luminescent diamond particles display a level of luminescence intensity greater than that of conventional luminescent nanodiamond, and may be functionalized for use in biological applications. ## Claims ### Claim 1 A luminescent diamond material comprising diamond particles that are mechanically interlocked together and combined with a pressure transfer media, wherein the luminescent diamond material is made by a high-pressure/high-temperature process, wherein a temperature of the high-pressure/high-temperature process is from about 1300° C. to about 2500° C. and a pressure of the high-pressure/high-temperature process is from about 3.0 GPa to about 10 GPa, wherein the diamond particles include diamond grains that have undergone plastic deformation, wherein the luminescent diamond material displays a level of luminescence intensity in one or more combinations of blue, violet-blue, red, or green wavelength spectrums that is greater than that of a precursor diamond material used to form the luminescent diamond material, wherein the diamond particles are free of intercrystalline bonded diamond, wherein the luminescent diamond material comprises greater than about 20 percent by volume diamond and greater than about 5 percent by volume pressure transfer media based on the total volume of the luminescent diamond material, and wherein the pressure transfer media comprises a non-catalyst material that does not promote intercrystalline diamond bonding during the high-pressure/high-temperature process. ### Claim 2 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the pressure transfer media is selected from the group consisting of carbonates, nitrates, sulfates, phosphates, chlorates, perchlorates, acetates, chromates, oxalates, sulfides, ammonium compounds, hydroxides, oxides, cyanides, cyanates, dichromates, halides, and combinations or mixtures thereof. ### Claim 3 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the pressure transfer media is selected from the group consisting of water soluble, acid soluble, and base soluble materials. ### Claim 4 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the pressure transfer media is a chloride. ### Claim 5 (depends on 1) The luminescent diamond material as recited in claim 1, comprising greater than about 50 percent by volume diamond and greater than about 10 percent by volume pressure transfer media based on the total volume of the luminescent diamond material. ### Claim 6 (depends on 1) The luminescent diamond material as recited in claim 1 comprising a total graphite content of less than about 5 percent by weight after being made by the high-pressure/high-temperature process without further treatment. ### Claim 7 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the luminescent diamond material displays a luminescence intensity in the green spectrum that is greater than in the red spectrum. ### Claim 8 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the luminescent diamond material displays a luminescence intensity in the red spectrum that is greater than that in the green spectrum. ### Claim 9 (depends on 1) The luminescent diamond material as recited in claim 1, wherein the luminescent diamond material displays a luminescence intensity in the red spectrum that is approximately the same as that in the green spectrum. ### Claim 10 A method for making luminescent diamond comprising subjecting a volume of precursor diamond grains in the presence of a pressure transfer media to a high-pressure/high-temperature condition at an elevated temperature greater than about 900° C. and a pressure greater than about 3.0 GPa to cause the diamond grains to undergo plastic deformation to produce nitrogen vacancy defects in the diamond grains, wherein the pressure transfer media is placed adjacent the volume of diamond grains before the high-pressure/high-temperature condition, wherein the pressure transfer media is selected from the group consisting of chlorides, carbonates, nitrates, sulfates, phosphates, chlorates, perchlorates, acetates, chromates, oxalates, sulfides, ammonium compounds, hydroxides, oxides, cyanides, cyanates, dichromates, halides, and combinations thereof, wherein a resulting diamond material displays a level of luminescence intensity in one or combinations of violet-blue, blue, red, and green wavelength spectrums that is greater than that of the precursor diamond grains, and wherein the resulting diamond material is free of intercrystalline bonded diamond. ### Claim 11 (depends on 10) The method as recited in claim 10, wherein the pressure transfer media does not promote intercrystalline diamond bonding during the high-pressure/high-temperature condition. ### Claim 12 (depends on 10) The method as recited in claim 10, wherein the pressure transfer media is a chloride. ### Claim 13 (depends on 10) The method as recited in claim 10, wherein the pressure transfer media melts and fills the interstitial pores within the volume of diamond grains during the high-pressure/high-temperature condition at the elevated temperature. ### Claim 14 (depends on 10) The method as recited in claim 10, wherein after the high-pressure/high-temperature condition, the resulting diamond material comprises diamond particles that are mechanically interlocked together. ### Claim 15 (depends on 10) The method as recited in claim 10, wherein after the high-pressure/high-temperature condition, the resulting diamond material comprises greater than about 20 percent by volume diamond and greater than about 5 percent by volume pressure transfer media based on the total volume of the diamond material. ### Claim 16 (depends on 10) The method as recited in claim 10, wherein after the high-pressure/high-temperature condition, the resulting diamond material comprises greater than about 50 percent by volume diamond and greater than about 10 percent by volume pressure transfer media based on the total volume of the diamond material. ### Claim 17 (depends on 10) The method as recited in claim 10, wherein the pressure transfer media is soluble in acid, water, or base. ### Claim 18 (depends on 10) The method as recited in claim 10, comprising, after the high-pressure/high-temperature condition, washing the resulting diamond material to remove all or a portion of the pressure transfer media therefrom. ### Claim 19 (depends on 10) The method as recited in claim 10, wherein during the high-pressure/high-temperature condition, includes an oxidizing pressure transfer media to remove graphite formed during the high-pressure/high-temperature condition. ### Claim 20 (depends on 10) The method as recited in claim 10, wherein the resulting diamond material has a total graphite content of less than about 5 percent by weight based on the total weight of the diamond material. ### Claim 21 A luminescent diamond material comprising diamond particles that are mechanically interlocked together and combined with a pressure transfer media, wherein the luminescent diamond material is made by a high-pressure/high-temperature process, wherein a temperature of the high-pressure/high-temperature process is about 2200° C. and a pressure of the high-pressure/high-temperature process is from about 7.3 GPa to about 7.7 GPa, wherein the diamond particles include diamond grains that have undergone plastic deformation, wherein the luminescent diamond material displays a level of luminescence intensity in one or more combinations of blue, violet-blue, red, or green wavelength spectrums that is greater than that of a precursor diamond material used to form the luminescent diamond material, wherein the diamond particles are free of intercrystalline bonded diamond, wherein the luminescent diamond material comprises greater than about 20 percent by volume diamond and greater than about 5 percent by volume pressure transfer media based on the total volume of the luminescent diamond material, wherein the pressure transfer media comprises a non-catalyst material that does not promote intercrystalline diamond bonding during the high-pressure/high-temperature process, and wherein the non-catalyst material is a chloride, wherein the luminescent diamond material comprises approximately 8 percent by weight magnesium carbonate, and wherein the diamond grains have an average grain size of about 2 μm.