US2021101839A1PendingUtilityA1

Ceramic oxide composites reinforced with 2d mx-enes

Assignee: UNIV DREXELPriority: Jun 20, 2018Filed: Jun 14, 2019Published: Apr 8, 2021
Est. expiryJun 20, 2038(~11.9 yrs left)· nominal 20-yr term from priority
C04B 35/645C04B 2235/80C04B 35/62655C04B 2235/3843C04B 2235/3284C04B 2235/786C04B 35/56C04B 2235/3224C04B 35/01C04B 2235/604C01C 3/08C04B 2235/3852C01B 32/90C04B 35/5618C04B 2235/768C04B 35/453C04B 2235/85C04B 2235/656C04B 2235/785C04B 2235/3817C01B 32/907C04B 35/58C04B 2235/77C04B 2235/5292H01L 35/34H01L 35/26H10N 10/01H10N 10/857
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Claims

Abstract

The present disclosure is directed to nanocomposites comprising a co-sintered composition of a MXene crystal form composition and an inorganic oxide, or oxide-type ceramic and methods of making and using the same.

Claims

exact text as granted — not AI-modified
1 . A nanocomposite comprising a co-sintered composition of a MXene composition and an inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride. 
     
     
         2 . The nanocomposite of  claim 1 , comprising a co-sintered composition of the MXene composition and an inorganic binary, ternary, or quaternary oxide. 
     
     
         3 . The nanocomposite of  claim 1 , wherein the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride comprises one or more alkali metal (Group 1 of the Periodic Table; e.g., including oxides of lithium, sodium, potassium, rubidium, and/or cesium), alkaline earth metal (Group 2 of the Periodic Table; e.g., including oxides of Be, Mg, Ca, Sr, and Ba), transition metal (comprising elements of Groups 3-12 of the Periodic Table), lanthanide and actinide metal, and/or metalloid (comprising elements of Groups 13-16 of the Periodic Table; e.g., including oxides of Al, Ga, In, Sn, Bi, Sb, P, or Pb), the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride optionally comprising Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Ge, Sn, Pb, Bi, or a combination thereof. 
     
     
         4 . The nanocomposite of  claim 1 , comprising one or more oxide of In, Ti, Sn, Zn, Zr, or a combination thereof. 
     
     
         5 . The nanocomposite of  claim 1 , comprising one or more oxide of Co, Mn, Nb, Pb, Ta, Ti, W, Zn, and Zr. 
     
     
         6 . The nanocomposite of  claim 1 , wherein the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride is or comprises a ferrite, a nickelate, a niobate, a ruthenate, a tantalate, a titanate, a tungstate, a vanadate, a zirconate, or a combination or mixture thereof. 
     
     
         7 . The nanocomposite of  claim 1 , comprising ZnO. 
     
     
         8 . The nanocomposite of  claim 1 , further comprising one or more lanthanide or actinide metal oxide. 
     
     
         9 . The nanocomposite of  claim 1 , having a perovskite structure. 
     
     
         10 . The nanocomposite of  claim 1 , wherein the MXene composition comprises at least one layer having first and second surfaces, each layer described by a formula M n+1 X n  and comprising:
 a substantially two-dimensional array of crystal cells, each crystal cell having an empirical formula of M n+1 X n , such that each X is positioned within an octahedral array of M,   wherein M is at least one Group IIIB, IVB, VB, or VIB metal,   wherein each X is C, N, or a combination thereof;   n=1, 2, or 3.   
     
     
         11 . The nanocomposite of  claim 10 , wherein the empirical formula of the M n+1 X n  MXene composition comprises Sc 2 C, Ti 2 C, V 2 C, Cr 2 C, Cr 2 N, Zr 2 C, Nb 2 C, Hf 2 C, Ti 3 C 2 , V 3 C 2 , Ta 3 C 2 , Ti 4 C 3 , V 4 C 3 , Ta 4 C 3 , Sc 2 N, Ti 2 N, V 2 N, Cr 2 N, Cr 2 N, Zr 2 N, Nb 2 N, Hf 2 C, Ti 3 N 2 , V 3 C 2 , Ta 3 C 2 , Ti 4 N 3 , V 4 C 3 , Ta 4 N 3  or a combination or mixture thereof, preferably Ti 3 C 2  or Ti 2 C. 
     
     
         12 . The nanocomposite of  claim 1 , wherein the MXene composition comprises a substantially two-dimensional array of crystal cells having an empirical formula of Ti 3 C 2 . 
     
     
         13 . The nanocomposite of  claim 1 , wherein the MXene composition at least one layer having first and second surfaces, each layer described by a formula M′ 2 M″ n X n+1  and comprising:
 a substantially two-dimensional array of crystal cells, each crystal cell having an empirical formula of M′ 2 M″ n X n+1 , such that each X is positioned within an octahedral array of M′ and M″, and where M″ n  are present as individual two-dimensional array of atoms intercalated (sandwiched) between a pair of two-dimensional arrays of M′ atoms, 
 wherein M′ and M″ are different Group IBB, IVB, VB, or VIB metals (especially where M′ and M″ are Ti, V, Nb, Ta, Cr, Mo, or a combination thereof), 
 wherein each X is C, N, or a combination thereof; and 
 n=1 or 2. 
 
     
     
         14 . The nanocomposite of  claim 13 , wherein the empirical formula of the MXene composition comprises Mo 2 TiC 2 , Mo 2 VC 2 , Mo 2 TaC 2 , Mo 2 NbC 2 , Mo 2 Ti 2 C 3 , Cr 2 TiC 2 , Cr 2 VC 2 , Cr 2 TaC 2 , Cr 2 NbC 2 , Ti 2 NbC 2 , Ti 2 TaC 2 , V 2 TaC 2 , or V 2 TiC 2 , preferably Mo 2 TiC 2 , Mo 2 VC 2 , Mo 2 TaC 2 , or Mo 2 NbC 2 , or their nitride or carbonitride analogs or Mo 2 Ti 2 C 3 , Mo 2 V 2 C 3 , Mo 2 Nb 2 C 3 , Mo 2 Ta 2 C 3 , Cr 2 Ti 2 C 3 , Cr 2 V 2 C 3 , Cr 2 Nb 2 C 3 , Cr 2 Ta 2 C 3 , Nb 2 Ta 2 C 3 , Ti 2 Nb 2 C 3 , Ti 2 Ta 2 C 3 , V 2 Ta 2 C 3 , V 2 Nb 2 C 3 , or V 2 Ti 2 C 3 , preferably Mo 2 Ti 2 C 3 , Mo 2 V 2 C 3 , Mo 2 Nb 2 C 3 , Mo 2 Ta 2 C 3 , Ti 2 Nb 2 C 3 , Ti 2 Ta 2 C 3 , or V 2 Ta 2 C 3 , or their nitride or carbonitride analogs. 
     
     
         15 . The nanocomposite of  claim 1 , wherein the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride is present as grains within the nanocomposite, the grains having dimensions in a range of from 100 nm to 200 nm, 200 nm to 300 nm, 300 nm to 400 nm, 400 nm to 500 nm, 500 nm to 600 nm, 600 nm to 700 nm, 700 nm to 800 nm, 800 nm to 900 nm, or any combination of two or more of the foregoing ranges. 
     
     
         16 . The nanocomposite of  claim 1 , wherein the nanocomposite exhibits a density greater than 90% of the theoretical density of the nanocomposite. 
     
     
         17 . The nanocomposite of  claim 1 , wherein the MXene composition is distributed along the grain boundaries of the sintered nanocomposite. 
     
     
         18 . The nanocomposite of  claim 1 , wherein the MXene composition is distributed substantially homogeneously throughout the nanocomposite. 
     
     
         19 . The nanocomposite of  claim 1 , wherein the nanocomposite exhibits an electrical conductivity, hardness, and/or elastic modulus that is at least 10% to about 500% greater than an otherwise equivalent nanocomposite not containing the MXene composition, or prepared under otherwise equivalent conditions in the absence of the MXene composition. 
     
     
         20 . The nanocomposite of  claim 1 , wherein the MXene composition is present in an amount of about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 15%, 20%, or 25% by weight relative to the weight of the entire composition. 
     
     
         21 . (canceled) 
     
     
         22 . (canceled) 
     
     
         23 . A method of preparing a nanocomposite, comprising:
 (a) distributing a precursor MXene composition and particle of an inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride into a homogeneous mixture;   (b) compacting the mixture into a compact form; and   (c) cold sintering the compact form at a temperature of 500° C. or less for a period of time to form the nanocomposite comprising   a co-sintered composition of a MXene composition and the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride.   
     
     
         24 . The method of  claim 23 , wherein the cold sintering also comprises pressure-assisted transient liquid phase sintering, where the liquid phase undergoes evaporation during sintering, which wherein the homogeneous mixture compacted into the compact form contains a carboxylic acid, such as acetic acid. 
     
     
         25 . The method of  claim 23 , wherein the compacting is done at a pressure in a range of from 50 MPa to 100 MPa, from 100 MPa to 150 MPa, from 150 MPa to 200 MPa, from 200 MPa to 225 MPa, from 225 MPa to 250 MPa, from 250 MPa to 275 MPa, from 275 MPa to 300 MPa, from 300 MPa to 325 MPa, from 325 MPa to 350 MPa, from 350 MPa to 400 MPa, from 400 MPa to 450 MPa, from 450 MPa to 500 MPa, from 500 MPa to 600 MPa, or a combination of two or more of the foregoing ranges, for example, from 225 MPa to 275 MPa. 
     
     
         26 . The method of  claim 23 , further comprising heat treating the nanocomposite comprising the co-sintered composition of a MXene composition and the inorganic oxide, oxycarbide, oxynitride, or oxycarbonitride at a temperature in a range of from 350° C. to about 1000° C. under inert atmosphere.

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