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CN-121971709-A - Double-response MXene/HAP composite material and preparation method and application thereof

CN121971709ACN 121971709 ACN121971709 ACN 121971709ACN-121971709-A

Abstract

The invention relates to the technical field of biomedical materials, in particular to a dual-response MXene/HAP composite material, and a preparation method and application thereof. According to the invention, an amide regulator is introduced, the hydroxyapatite is induced to grow in a preferred orientation along the crystallographic c-axis direction on the surface of the MXene in situ, so that the effective control of the orientation structure of the hydroxyapatite is realized, the piezoelectric response performance of the hydroxyapatite under low-intensity ultrasonic stimulation is remarkably enhanced, meanwhile, the near infrared light absorption and the electric conduction characteristics of the MXene enable the composite material to generate a synergistically amplified physical signal under the effects of optical stimulation and acoustic stimulation.

Inventors

  • LIU BING
  • DUAN TINGTING
  • YU JIAHUI
  • Sun Yongran

Assignees

  • 山东第一医科大学(山东省医学科学院)

Dates

Publication Date
20260505
Application Date
20260330

Claims (10)

  1. 1. A method for preparing a dual response MXene/HAP composite material comprising the steps of: (1) Peeling the Al layer by etching the precursor phase Ti 3 AlC 2 through lithium fluoride and hydrochloric acid, centrifuging, and performing ultrasonic treatment to obtain a single-layer MXene; (2) Respectively dissolving calcium chloride and diammonium hydrogen phosphate in a solvent, sequentially adding the solution into the single-layer-containing MXene solution obtained in the step (1), then adding a propionamide solution, adjusting the pH of the system to 3-4, and carrying out hydrothermal reaction after stirring to obtain the product; the hydrothermal reaction temperature is 170-190 ℃.
  2. 2. The method of claim 1, wherein the step (1) comprises mixing lithium fluoride and hydrochloric acid, heating the reaction system to 40-45deg.C, adding the precursor phase Ti 3 AlC 2 , stirring at a constant temperature for reaction of 40-50 h, centrifuging, and performing ultrasonic treatment to obtain a single-layer MXene.
  3. 3. The method of claim 2, wherein in step (1), the ultrasonic treatment is ice bath ultrasonic treatment for a period of time of 20-40 min and a frequency of 20-50 kHz.
  4. 4. The method of claim 2, wherein centrifugation is continued for 10-20 min at 3000-4000 rpm after sonication, and the supernatant is collected.
  5. 5. The method according to claim 1, wherein in the step (2), the mass ratio of calcium chloride to diammonium phosphate is 1.2 to 1.5:1; Or, in the step (2), the mass ratio of the calcium chloride to the single-layer MXene is 0.5-0.6:1.
  6. 6. The method according to claim 1, wherein in the step (2), the mass ratio of the calcium chloride, the diammonium phosphate and the propionamide is 1.2-1.5:1:0.08-0.15.
  7. 7. The method of claim 1, wherein in step (2), the hydrothermal reaction time is 960-1080 min.
  8. 8. The process according to claim 1, wherein in step (2), after the hydrothermal reaction, the mixture is naturally cooled to room temperature, the clear supernatant solution is discarded, and the black precipitate is centrifuged.
  9. 9. The dual-response MXene/HAP composite material prepared by the preparation method according to any one of claims 1-8.
  10. 10. Use of the dual response MXene/HAP composite material of claim 9 for preparing an osteogenic material.

Description

Double-response MXene/HAP composite material and preparation method and application thereof Technical Field The invention relates to the technical field of biomedical materials, in particular to a dual-response MXene/HAP composite material, and a preparation method and application thereof. Background The information disclosed in the background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an admission or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. Bone tissue repair is a highly complex biological process involving multiple stages of inflammatory response, immune regulation, angiogenesis, and osteogenesis remodeling. Under ideal conditions, the biological material for repairing bone defects needs to have excellent biocompatibility and conductivity, and further has the capability of actively regulating and controlling local microenvironment and inducing tissue regeneration. However, synthetic bone substitute materials (such as Hydroxyapatite (HAP), β -tricalcium phosphate, etc.) currently in wide clinical use are "biologically inert" or "passive bioactive" materials, which are limited by the lack of dynamic regulation of the immune response to the body, and difficulty in achieving physiological bone regeneration. As bone immunology research is advanced, more and more studies indicate that bone repair effects are closely related to the post-implantation immune microenvironment. Among them, macrophages, as immune cells that respond earliest to implant materials, have their polarization states directly affecting the inflammatory process and subsequent tissue repair results. In the early stage of bone repair, M1 type macrophages clear tissue fragments by secreting pro-inflammatory cytokines and establish a repair basis, and then timely convert to M2 type macrophages, so that bone formation and vascularization can be started by releasing growth factors. It was found that there is a significant increase in the risk of infection if there is a lack of adequate M1 response around the implant, whereas if the M1 response is too long in duration, fiber encapsulation and osseointegration fail. Accordingly, the presence of M2 macrophages helps promote angiogenesis and bone matrix deposition by secreting anti-inflammatory and osteogenic factors, which are necessary for later repair. Therefore, realizing dynamic regulation and control of immune response in the time dimension is a key for improving bone repair quality. However, the existing bone repair materials are mostly subjected to static regulation and control through chemical components or surface morphology, and staged matching of immune processes is difficult to achieve. Therefore, the development of a biological material capable of dynamically balancing the immune microenvironment has important clinical significance. HAP is widely used in the field of bone repair because of its chemical composition similar to natural bone minerals. However, conventional HAPs rely primarily on passive bone conduction to participate in the repair process, lacking active regulatory capability for early immune responses after implantation. In addition, HAP crystals are randomly oriented, the piezoelectric performance is limited, the bioelectric signals generated under external physical stimulation are weak, and the regulation effect of external field stimulation such as ultrasound on cell behaviors is difficult to effectively amplify. MXene as a novel two-dimensional material has excellent near infrared light absorption capability and conductivity, shows good application prospect in the biomedical field, but lacks osteogenesis induction capability, and has defects in structural stability and biological function synergy when used independently. External field stimulation is increasingly being introduced into bone repair studies due to its non-invasive and controllable nature, where near infrared light can rapidly activate cellular responses through photothermal effects, while low intensity ultrasound can produce mild mechanical and electrical stimulation inside tissues. However, the existing researches mostly adopt a single external field stimulation or a simple superposition mode, and lack a functional system capable of cooperatively responding to light stimulation and sound stimulation at the material structure level. Meanwhile, the existing MXene and HAP composite materials are mostly constructed in a physical mixing or post-loading mode, the interface combination is limited, the structural cooperativity is insufficient, and the effective transmission and amplification of external field signals are not facilitated. Disclosure of Invention In view of the above, the invention provides a dual-response MXene/HAP composite material, and a preparation method and application thereof. According to the invention, the in-situ c-