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CN-122010572-A - Graphene ceramic composite material and preparation method and application thereof

CN122010572ACN 122010572 ACN122010572 ACN 122010572ACN-122010572-A

Abstract

The invention belongs to the technical field of refractory materials. The invention provides a graphene ceramic composite material, a preparation method and application thereof, wherein the preparation method comprises the steps of adding zirconium boride particles, silicon carbide particles, yttrium oxide and lanthanum doped cerium oxide into graphene oxide dispersion liquid, performing ball milling, drying to obtain raw material powder, loading the raw material powder into a graphite mold, and sintering to obtain the graphene ceramic composite material, wherein the raw material powder comprises, by volume, 5.6-6 parts of graphene oxide, 70-72 parts of zirconium boride particles, 20-21 parts of silicon carbide particles, 1.5-2 parts of yttrium oxide and 1-1.3 parts of lanthanum doped cerium oxide. According to the invention, the content of graphene oxide is increased, so that the relative density of the prepared composite material is increased, and meanwhile, the bending strength of the composite material is further improved.

Inventors

  • REN YONGZENG
  • QIAO DEHUI

Assignees

  • 青岛百顿特种陶瓷技术有限公司

Dates

Publication Date
20260512
Application Date
20260120

Claims (9)

  1. 1. The preparation method of the graphene ceramic composite material is characterized by comprising the following steps of adding zirconium boride particles, silicon carbide particles, yttrium oxide and lanthanum doped cerium oxide into graphene oxide dispersion liquid, performing ball milling and drying to obtain raw material powder, filling the raw material powder into a graphite mold, and sintering to obtain the graphene ceramic composite material; the raw material powder comprises, by volume, 5.6-6 parts of graphene oxide, 70-72 parts of zirconium boride particles, 20-21 parts of silicon carbide particles, 1.5-2 parts of yttrium oxide and 1-1.3 parts of lanthanum-doped cerium oxide.
  2. 2. The method for preparing the graphene ceramic composite material according to claim 1, wherein the graphene oxide dispersion liquid is prepared by performing alcohol ultrasonic dispersion on graphene oxide powder.
  3. 3. The method for preparing the graphene ceramic composite material according to claim 1, wherein the planetary ball mill is used for ball milling, the ball milling time is 8-9h, and the rotating speed is 250-270rpm.
  4. 4. The method for preparing the graphene ceramic composite material according to claim 1, wherein the drying temperature is 45+/-2 ℃ and the drying time is 3-5h.
  5. 5. The preparation method of the graphene ceramic composite material according to claim 1, wherein the specific operation of sintering is that the graphene ceramic composite material is subjected to heat preservation in a vacuum hot-pressing sintering furnace for 1-1.2h at 1950+/-10 ℃ under the conditions of 30+/-2 MPa of pressure, inert atmosphere and temperature rising rate of 15-20 ℃ per minute.
  6. 6. The preparation method of the graphene ceramic composite material according to claim 1, wherein the preparation method of the lanthanum-doped cerium oxide is as follows: a1, 12.99g of lanthanum nitrate hexahydrate and 31.79g of cerium nitrate hexahydrate are taken and dissolved in deionized water to obtain a mixed solution with the volume of 1L; A2, heating the mixed solution obtained in the step A1 to 70+/-2 ℃ under stirring, and dropwise adding 14mL of formic acid solution with the mass fraction of 85% into the mixed solution to fully precipitate metal ions, so as to obtain a white suspension; and A3, centrifuging the white suspension obtained in the step A2, washing, drying and roasting in a muffle furnace to obtain the product.
  7. 7. The method for preparing a graphene ceramic composite material according to claim 6, wherein in A3, the roasting temperature is 400+/-10 ℃ and the roasting time is 3-3.2h.
  8. 8. A graphene ceramic composite material prepared by the preparation method according to any one of claims 1 to 7.
  9. 9. Use of the graphene ceramic composite material according to claim 8, in a heat protection material for use in extreme thermal environments.

Description

Graphene ceramic composite material and preparation method and application thereof Technical Field The invention belongs to the technical field of refractory materials, and particularly relates to a graphene ceramic composite material and a preparation method and application thereof. Background Zirconium boride ceramic matrix composites are considered to be very promising non-ablative ultra-high temperature heat resistant materials due to their excellent thermophysical properties. However, the intrinsic brittleness and poor thermal shock resistance of zirconium boride ceramic matrix composites limit their wide engineering applications. In order to improve the toughness of the zirconium boride ceramic matrix composite, graphene nanoplatelets are added to the zirconium boride ceramic matrix composite. In order to uniformly disperse the graphene nano-sheets in the zirconium boride ceramic matrix composite, the graphene nano-sheets are uniformly dispersed in the zirconium boride ceramic matrix composite by utilizing a large amount of hydrophilic oxygen-containing groups on the surface of graphene oxide and combining an in-situ thermal reduction method. It is known in the art that graphene can promote densification by undergoing a carbothermic reaction with an oxide on the surface of zirconium boride, and the relative density of the resulting composite continues to increase as the content of graphene oxide increases. Thus, in order to obtain a higher relative density, it is possible to choose to maximize the content of graphene oxide. Meanwhile, as the content of graphene oxide increases, the bending strength and fracture toughness of the composite material are also improved. However, because the grain boundaries in the composite material are limited, and aggregation is easily generated between graphene oxide nano-sheets through weak van der Waals force, when the graphene oxide content is increased to be excessive (more than 5 v%), aggregation/aggregation of the graphene oxide nano-sheets in the composite material occurs, so that the bending strength of the composite material starts to be reduced. Disclosure of Invention In order to solve the problems in the background art, the invention provides a graphene ceramic composite material, and a preparation method and application thereof, wherein the relative density of the prepared composite material is increased and the bending strength of the composite material is further improved by increasing the content of graphene oxide. In order to achieve the above object, the present invention provides the following technical solutions: The preparation method of the graphene ceramic composite material comprises the following steps of adding zirconium boride particles, silicon carbide particles, yttrium oxide and lanthanum doped cerium oxide into graphene oxide dispersion liquid, ball milling, drying to obtain raw material powder, filling the raw material powder into a graphite mold, and sintering to obtain the graphene ceramic composite material; the raw material powder comprises, by volume, 5.6-6 parts of graphene oxide, 70-72 parts of zirconium boride particles, 20-21 parts of silicon carbide particles, 1.5-2 parts of yttrium oxide and 1-1.3 parts of lanthanum-doped cerium oxide. Further, the graphene oxide dispersion liquid is prepared by performing ultrasonic dispersion on graphene oxide powder through alcohol. Further, a planetary ball mill is used for ball milling, the ball milling time is 8-9h, and the rotating speed is 250-270rpm. Further, the drying temperature is 45+/-2 ℃ and the drying time is 3-5h. Further, the specific operation of sintering is that the sintering is carried out in a vacuum hot-pressing sintering furnace for 1-1.2h, the temperature is 1950+/-10 ℃, the pressure is 30+/-2 MPa, the inert atmosphere is adopted, and the temperature rising rate is 15-20 ℃ per minute. Further, the preparation method of the lanthanum-doped cerium oxide comprises the following steps: a1, 12.99g of lanthanum nitrate hexahydrate and 31.79g of cerium nitrate hexahydrate are taken and dissolved in deionized water to obtain a mixed solution with the volume of 1L; A2, heating the mixed solution obtained in the step A1 to 70+/-2 ℃ under stirring, and dropwise adding 14mL of formic acid solution with the mass fraction of 85% into the mixed solution to fully precipitate metal ions, so as to obtain a white suspension; And A3, centrifuging the white suspension obtained in the step A2, washing with ethanol, drying, and roasting in a muffle furnace to obtain the lanthanum-doped cerium oxide. Further, in A3, the roasting temperature is 400+/-10 ℃ and the roasting time is 3-3.2h. The graphene ceramic composite material is prepared by the preparation method. The application of the graphene ceramic composite material is used for a heat-resistant material in an extreme heat environment. The application has the following beneficial effects: on one hand, ce 4+/Ce3+ in lanthanum-doped cerium