CN115137876A - Hectorite bioceramic artificial bone and preparation method thereof - Google Patents

Hectorite bioceramic artificial bone and preparation method thereof Download PDF

Info

Publication number
CN115137876A
CN115137876A CN202210737754.XA CN202210737754A CN115137876A CN 115137876 A CN115137876 A CN 115137876A CN 202210737754 A CN202210737754 A CN 202210737754A CN 115137876 A CN115137876 A CN 115137876A
Authority
CN
China
Prior art keywords
hectorite
artificial bone
bioceramic
printing
bone
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210737754.XA
Other languages
Chinese (zh)
Inventor
曾庆丰
杨智宇
益明星
方亮
魏静
张新平
何蕊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Point Cloud Biology Hangzhou Co ltd
Original Assignee
Point Cloud Biology Hangzhou Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Point Cloud Biology Hangzhou Co ltd filed Critical Point Cloud Biology Hangzhou Co ltd
Priority to CN202210737754.XA priority Critical patent/CN115137876A/en
Publication of CN115137876A publication Critical patent/CN115137876A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/10Ceramics or glasses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/025Other specific inorganic materials not covered by A61L27/04 - A61L27/12
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/12Phosphorus-containing materials, e.g. apatite
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14Macromolecular materials
    • A61L27/16Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/001Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/447Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on phosphates, e.g. hydroxyapatite
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412Tissue-regenerating or healing or proliferative agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427Silicates other than clay, e.g. water glass
    • C04B2235/3436Alkaline earth metal silicates, e.g. barium silicate
    • C04B2235/3454Calcium silicates, e.g. wollastonite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6026Computer aided shaping, e.g. rapid prototyping

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Veterinary Medicine (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dermatology (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Epidemiology (AREA)
  • Transplantation (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Prostheses (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)

Abstract

The invention discloses a hectorite bioceramic artificial bone and a preparation method thereof, wherein hectorite and bioceramic are used as raw materials and are mixed with polyvinyl alcohol to prepare paste with good printability, a host bone prototype model is obtained to design an artificial bone three-dimensional model, a bioceramic 3D printer is used for carrying out non-silk 3D printing, and the printed artificial bone is sintered to prepare the hectorite bioceramic artificial bone. The method is simple in forming, the used raw materials are low in cost and have good biocompatibility, the prepared hectorite bioceramic artificial bone has osteogenic inductivity, good bone tissue repair capacity and good mechanical strength, printing of the personalized artificial bone is achieved through a digital design technology, and the hectorite bioceramic artificial bone is beneficial to clinically applying to repair of human bone injury or bone loss.

Description

Hectorite bioceramic artificial bone and preparation method thereof
Technical Field
The invention belongs to the field of bone repair, and particularly relates to a hectorite bioceramic artificial bone and a preparation method thereof.
Background
The hectorite is an artificially synthesized nano clay, is a layered silicate material, is also called lithium magnesium silicate/lithium magnesium sodium silicate, is composed of layered disc nanoparticles with the diameter of about 25nm and the thickness of 1nm, and has wide application prospect in the field of nano biological materials due to the advantages of low price, excellent performance, high safety and the like. Clay has been used in many ways as a bioactive agent for the treatment of wounds, hemostasis, intestinal diseases, skin diseases, etc., and also as a stabilizer, thickener, etc. for other liquids due to its structural diversity.
Laponite exhibits good biocompatibility in interaction with cells and can regulate proliferation and differentiation of cells, so that laponite is widely used in the fields of tissue engineering, wound healing, bioprinting and the like, and is one of novel, widely-used and good-performance materials in the field of regenerative medicine. The use of laponite in bone tissue engineering to promote bone regeneration has been a popular study in the field of materials science in recent years. Some studies have demonstrated that laponite has biological activity, and even in the absence of growth factors, laponite induces osteogenic differentiation of various cells such as osteogenic precursor cells, human mesenchymal stem cells, human adipose-derived cells, and the like. Laponite dissociates into individual particles of lithium, magnesium, silicon, etc., which cause upregulation of osteogenesis-related genes and pathways, thereby inducing osteogenic differentiation of cells.
With the accelerated development of 3D printing, more and more materials are used for research. Whereas the most used in the field of bone repair is the silkless 3D printing technique. However, due to the characteristics of hectorite, the paste which meets the silk-free 3D printing is prepared and belongs to the gel class, so that the mechanical property of the printed artificial bone is very low, and even the shape of the artificial bone cannot be maintained, and a method for enhancing the mechanical strength of the hectorite artificial bone is urgently needed.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a hectorite bioceramic artificial bone and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a hectorite bioceramic artificial bone is prepared from hectorite and bioceramic by a silk-free 3D printing process.
Further, the bioceramic comprises one or more of hydroxyapatite, beta-tricalcium phosphate and calcium silicate.
A preparation method of a hectorite bioceramic artificial bone comprises the following steps:
dissolving polyvinyl alcohol in purified water to prepare a polyvinyl alcohol aqueous solution;
adding purified water into printing powder of hectorite and biological ceramics, uniformly stirring, adding a polyvinyl alcohol aqueous solution, uniformly stirring again, and filling into a charging barrel for defoaming to obtain a printing paste body;
acquiring CT/MRI/X rays of a defect part of a host bone, processing the data, acquiring a prototype model of the host bone, and designing a suitable three-dimensional model of the artificial bone;
loading the printing paste into a printing head of a 3D printer, loading the designed three-dimensional model into 3D printing software, setting printing parameters, and starting the 3D printer to finish printing of the artificial bone;
and sintering the printed artificial bone to obtain the hectorite bioceramic artificial bone product.
Further, the mass fraction of the polyvinyl alcohol aqueous solution is 4-10%.
Furthermore, the mass ratio of the hectorite to the bioceramic in the printing paste is 1:1-3, and the added purified water is 2-4 times of the mass of the hectorite and the bioceramic printing powder.
Furthermore, the polyvinyl alcohol aqueous solution added into the printing paste is 1/6-1/4 of the sum of the mass of the laponite, the bioceramic and the purified water.
Further, the data are processed by a software 3D Slicer to obtain a host bone prototype model, a suitable artificial bone three-dimensional model is designed by Free CAD software, the model is stored as an STL format file and loaded into PC Printer software, and the silk-Free 3D printing is carried out by a biological ceramic 3D Printer.
Further, the printing parameters are set to: the filling rate is 40-80%, the printing layer height is 0.1-0.3 mm, the average filament diameter is 500-900 μm, and the average pore diameter is 300-800 μm.
Furthermore, in the sintering process, the sintering temperature is 840-880 ℃, and the heat preservation time is 2-4 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a hectorite bioceramic artificial bone and a preparation method thereof. The method is simple in forming, printing of the personalized artificial bone can be achieved through a digital design technology, the used raw materials are low in cost and have good biocompatibility, the prepared hectorite bioceramic artificial bone has osteoinduction, good bone tissue repair capacity and good mechanical strength, the hectorite bioceramic artificial bone is favorable for clinically repairing bone injury or bone loss of a human body, and the application prospect is very wide.
Drawings
In order to more clearly explain the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a 3D printed image of a hectorite bioceramic artificial bone prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention is described in further detail below with reference to the accompanying drawings:
the invention provides a preparation method of a hectorite bioceramic artificial bone, which comprises the following steps:
preparing a polyvinyl alcohol aqueous solution: dissolving polyvinyl alcohol in purified water to obtain a polyvinyl alcohol solution with the mass fraction of 4% -10%;
preparing a printing paste: weighing hectorite and biological ceramic in a mass ratio of 1:1-3, uniformly stirring the hectorite and the biological ceramic to obtain printing powder, weighing purified water in an amount which is 2-4 times of the printing powder, uniformly stirring the purified water, weighing polyvinyl alcohol aqueous solution which is 1/6-1/4 of the sum of the printing powder and the purified water, uniformly stirring the polyvinyl alcohol aqueous solution again, filling the mixture into a charging barrel, and defoaming the mixture to obtain paste with good printability.
Artificial bone three-dimensional model: acquiring CT/MRI/X rays of a defect part of a host bone, processing data by using software 3D Slicer 4.10.2, acquiring a prototype model of the host bone, and designing an STL (synthetic bone template) file of an applicable artificial bone three-dimensional model by using Free CAD (computer aided design) software;
silkless 3D printing: the artificial bone is printed by a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 40-80%, the printing layer height is 0.1-0.3 mm, the average filament diameter is 500-900 microns, the average pore diameter is 300-800 microns, the printing paste is uniformly extruded through a screw propeller at a constant speed, a workbench performs synthetic motion along an x-y axis, a printing head moves along a z axis, and the printing is sequentially performed layer by layer, so that the printing of the artificial bone is finally completed;
and (3) sintering: and (3) preserving the heat of the printed artificial bone at 840-880 ℃ for 6-8 h, and sintering to obtain the hectorite bioceramic artificial bone.
Example 1:
preparing a polyvinyl alcohol aqueous solution: dissolving 10g of polyvinyl alcohol in 90g of purified water to obtain a polyvinyl alcohol solution with the mass fraction of 10%;
preparing a printing paste body: weighing 10g of hectorite and 10g of hydroxyapatite, uniformly stirring the hectorite and the hydroxyapatite to obtain printing powder, weighing 40g of purified water, uniformly stirring the purified water, weighing 10g of polyvinyl alcohol aqueous solution, uniformly stirring the polyvinyl alcohol aqueous solution again, filling the polyvinyl alcohol aqueous solution into a charging barrel, and defoaming the polyvinyl alcohol aqueous solution to obtain paste with good printability;
artificial bone three-dimensional model: acquiring CT/MRI/X rays of a host bone defect part, processing data by using software 3D Slicer 4.10.2, acquiring a host bone prototype model, and designing an artificial bone three-dimensional model STL file suitable for a bone defect anatomical structure or special requirements by using Free CAD software;
silkless 3D printing: and printing the artificial bone by using a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 45%, the printing layer height is 0.1mm, the average filament diameter is 600 microns, the average pore diameter is 500 microns, the printing paste is uniformly extruded at a constant speed through a spiral propeller, a workbench performs synthetic motion along an x-y axis, a printing head moves along a z axis, and the artificial bone is printed layer by layer in sequence, and finally the printing of the artificial bone is completed;
and (3) sintering: and sintering the printed artificial bone at the sintering temperature of 840 ℃ for 4h to obtain the hectorite bioceramic artificial bone as shown in figure 1.
Example 2:
preparing a polyvinyl alcohol aqueous solution: dissolving 8g of polyvinyl alcohol in 92g of purified water to obtain a polyvinyl alcohol solution with the mass fraction of 8%;
preparing a printing paste: weighing 10g of hectorite and 15g of beta-tricalcium phosphate, uniformly stirring the hectorite and the beta-tricalcium phosphate to obtain printing powder, weighing 62.5g of purified water, uniformly stirring the purified water, weighing 15.91g of polyvinyl alcohol aqueous solution, uniformly stirring the polyvinyl alcohol aqueous solution again, filling the polyvinyl alcohol aqueous solution into a charging barrel, and defoaming the polyvinyl alcohol aqueous solution to obtain paste with good printability;
artificial bone three-dimensional model: acquiring CT/MRI/X rays of a host bone defect part, processing data by using software 3D Slicer 4.10.2, acquiring a host bone prototype model, and designing an artificial bone three-dimensional model STL file suitable for a bone defect anatomical structure or special requirements by using Free CAD software;
silkless 3D printing: the artificial bone is printed by a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 40%, the printing layer height is 0.15mm, the average filament diameter is 500 microns, the average pore diameter is 300 microns, the printing paste is uniformly extruded at a constant speed through a spiral propeller, a workbench performs synthetic motion along an x-y axis, a printing head moves along a z axis, and the artificial bone is printed layer by layer in sequence, and finally the printing of the artificial bone is completed;
and (3) sintering: and sintering the printed artificial bone at 850 ℃ for 3.5 hours to obtain the hectorite bioceramic artificial bone after sintering.
Example 3:
preparing a polyvinyl alcohol aqueous solution: dissolving 6g of polyvinyl alcohol in 94g of purified water to obtain a polyvinyl alcohol solution with the mass fraction of 6%;
preparing a printing paste body: weighing 10g of hectorite, 8g of hydroxyapatite, 6g of beta-tricalcium phosphate and 6g of calcium silicate, uniformly stirring the mixture to obtain printing powder, weighing 60g of purified water, uniformly stirring the mixture, weighing 18g of polyvinyl alcohol aqueous solution, uniformly stirring the mixture again, filling the mixture into a charging barrel, and defoaming the mixture to obtain paste with good printability;
artificial bone three-dimensional model: acquiring CT/MRI/X rays of a host bone defect part, processing data by using software 3D Slicer 4.10.2, acquiring a host bone prototype model, and designing an artificial bone three-dimensional model STL file suitable for a bone defect anatomical structure or special requirements by using Free CAD software;
silkless 3D printing: the artificial bone is printed by a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 50%, the printing layer height is 0.2mm, the average filament diameter is 700 mu m, the average pore diameter is 400 mu m, the printing paste is uniformly extruded at a constant speed through a spiral propeller, the workbench performs synthetic motion along an x-y axis, the printing head moves along a z axis, and the artificial bone is printed layer by layer in sequence, and finally the printing of the artificial bone is completed;
and (3) sintering: and sintering the printed artificial bone at 860 ℃ for 3h to obtain the hectorite bioceramic artificial bone.
Example 4:
preparing a polyvinyl alcohol aqueous solution: dissolving 5g of polyvinyl alcohol in 95g of purified water to obtain a polyvinyl alcohol solution with the mass fraction of 5%;
preparing a printing paste: weighing 10g of hectorite, 11g of hydroxyapatite, 7g of beta-tricalcium phosphate and 7g of calcium silicate, uniformly stirring the mixture to obtain printing powder, weighing 122.5g of purified water, uniformly stirring the mixture, weighing 35g of polyvinyl alcohol aqueous solution, uniformly stirring the mixture again, filling the mixture into a charging barrel, and defoaming the mixture to obtain paste with good printability;
artificial bone three-dimensional model: acquiring CT/MRI/X rays of a host bone defect part, processing data by using software 3D Slicer 4.10.2, acquiring a host bone prototype model, and designing an artificial bone three-dimensional model STL file suitable for a bone defect anatomical structure or special requirements by using Free CAD software;
silkless 3D printing: the artificial bone is printed by a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 60%, the printing layer height is 0.25mm, the average filament diameter is 800 microns, the average pore diameter is 600 microns, the printing paste is uniformly extruded at a constant speed through a spiral propeller, a workbench performs synthetic motion along an x-y axis, a printing head moves along a z axis, and the artificial bone is printed layer by layer in sequence to finally finish printing of the artificial bone;
and (3) sintering: and sintering the printed artificial bone at 870 ℃ for 2.5h to obtain the hectorite bioceramic artificial bone.
Example 5:
preparing a polyvinyl alcohol aqueous solution: dissolving 4g of polyvinyl alcohol in 96g of purified water to obtain a polyvinyl alcohol solution with the mass fraction of 4%;
preparing a printing paste: weighing 10g of hectorite, 12g of hydroxyapatite, 9g of beta-tricalcium phosphate and 9g of calcium silicate, uniformly stirring the mixture to obtain printing powder, weighing 160g of purified water, uniformly stirring the mixture, weighing 33.33g of polyvinyl alcohol aqueous solution, uniformly stirring the mixture again, filling the mixture into a charging barrel, and defoaming the mixture to obtain paste with good printability;
artificial bone three-dimensional model: acquiring CT/MRI/X rays of a host bone defect part, processing data by using software 3D Slicer 4.10.2, acquiring a host bone prototype model, and designing an artificial bone three-dimensional model STL file suitable for a bone defect anatomical structure or special requirements by using Free CAD software;
silkless 3D printing: and printing the artificial bone by using a biological ceramic printer. Firstly, loading the uniformly mixed printing paste into a printing head, then loading the designed STL file of the artificial bone three-dimensional model into PC Printer software, and setting the printing process parameters as follows: the filling rate is 80%, the printing layer height is 0.3mm, the average filament diameter is 900 microns, the average pore diameter is 800 microns, the printing paste is uniformly extruded at a constant speed through a spiral propeller, a workbench performs synthetic motion along an x-y axis, a printing head moves along a z axis, and the artificial bone is printed layer by layer in sequence, and finally the printing of the artificial bone is completed;
and (3) sintering: and sintering the printed artificial bone at 880 ℃, keeping the temperature for 2 hours, and obtaining the hectorite bioceramic artificial bone after sintering.
And (3) testing the performance of the hectorite bioceramic artificial bone:
the porosity, average filament diameter, average pore diameter and ball indentation strength of the hectorite bioceramic artificial bone prepared in example 1 are tested by the following specific test methods: the porosity, the average silk diameter, the average pore diameter and the pore connectivity refer to a porous metal material X-ray CT detection method for a surgical implant of GB/T36984-2018, a sample is subjected to Micro-CT detection, and three-dimensional reconstruction is carried out on all scanned faults to obtain a sample three-dimensional body model; the ratio of the pore volume to the total sample volume was then calculated as the three-dimensional porosity. And analyzing the image of the Micro-CT, calculating the diameter of the aperture wire, describing the aperture of the circular hole by adopting the diameter of the circular hole, describing the aperture of the slit hole by adopting the distance between two pairs of walls, measuring 12 points on each surface, and taking the average value as the average aperture and the average wire diameter. The ball indentation strength is referred to a ball indentation test method in a YY/T1558.3-2017 material mechanical strength detection method, ten printed samples are taken, the samples are cubes with the length, the width and the height of 10mm, a universal testing machine is used for testing at the loading speed of 0.5mm/min, the maximum load in the testing process is recorded, and the average value of the maximum load is used as the final ball indentation strength. The result shows that the porosity is 46 percent, the average wire diameter is 600 mu m, the average pore diameter is 500 mu m, the ball indentation strength is 152N, and the result shows that the hectorite bioceramic artificial bone has high porosity, uniform wire diameter and pore diameter and highly uniform structure, is very beneficial to cell attachment and drug release, has higher strength, and can ensure the stability of the artificial bone during implantation.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The hectorite bioceramic artificial bone is characterized in that hectorite and bioceramic are used as raw materials and are prepared through a filament-free 3D printing process.
2. The laponite bioceramic artificial bone of claim 1, wherein the bioceramic comprises one or more of hydroxyapatite, β -tricalcium phosphate, calcium silicate.
3. A method for preparing a hectorite bioceramic artificial bone according to any one of claims 1-2, comprising:
dissolving polyvinyl alcohol in purified water to prepare a polyvinyl alcohol aqueous solution;
adding purified water into printing powder of hectorite and biological ceramics, uniformly stirring, adding a polyvinyl alcohol aqueous solution, uniformly stirring again, and filling into a charging barrel for defoaming to obtain a printing paste body;
acquiring CT/MRI/X rays of a defect part of a host bone, processing the data, acquiring a prototype model of the host bone, and designing a suitable three-dimensional model of the artificial bone;
loading the printing paste into a printing head of a 3D printer, loading the designed three-dimensional model into 3D printing software, setting printing parameters, and starting the 3D printer to finish printing of the artificial bone;
and sintering the printed artificial bone to obtain the hectorite bioceramic artificial bone product.
4. The method for preparing the hectorite bioceramic artificial bone according to claim 3, wherein the mass fraction of the polyvinyl alcohol aqueous solution is 4-10%.
5. The method for preparing a hectorite bioceramic artificial bone according to claim 3, wherein the mass ratio of hectorite to bioceramic in the printed paste is 1:1-3, and the added purified water is 2-4 times of the mass of hectorite and bioceramic printed powder.
6. The method for preparing a hectorite bioceramic artificial bone according to claim 3, wherein the polyvinyl alcohol aqueous solution added into the paste for printing is 1/6 to 1/4 of the sum of the mass of the hectorite, the bioceramic and the purified water.
7. The method for preparing a hectorite bioceramic artificial bone according to claim 3, wherein a host bone prototype model is obtained after data is processed by a 3D Slicer software, an applicable artificial bone three-dimensional model is designed by Free CAD software, the model is stored as an STL format file and loaded into a PC Printer software, and the bioceramic 3D Printer is used for 3D printing without silk.
8. The method for preparing a hectorite bioceramic artificial bone according to claim 3, wherein printing parameters are set as follows: the filling rate is 40-80%, the printing layer height is 0.1-0.3 mm, the average filament diameter is 500-900 μm, and the average pore diameter is 300-800 μm.
9. The method for preparing a hectorite bioceramic artificial bone according to claim 3, wherein the sintering temperature is 840-880 ℃ and the heat preservation time is 2-4 h in the sintering process.
CN202210737754.XA 2022-06-27 2022-06-27 Hectorite bioceramic artificial bone and preparation method thereof Pending CN115137876A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210737754.XA CN115137876A (en) 2022-06-27 2022-06-27 Hectorite bioceramic artificial bone and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210737754.XA CN115137876A (en) 2022-06-27 2022-06-27 Hectorite bioceramic artificial bone and preparation method thereof

Publications (1)

Publication Number Publication Date
CN115137876A true CN115137876A (en) 2022-10-04

Family

ID=83407366

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210737754.XA Pending CN115137876A (en) 2022-06-27 2022-06-27 Hectorite bioceramic artificial bone and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115137876A (en)

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104163622A (en) * 2014-06-06 2014-11-26 上海交通大学附属第一人民医院 Preparation method and application of laponite bioceramics
CN104325644A (en) * 2014-10-20 2015-02-04 西安点云先进材料科技有限公司 Filament-free three-dimensional printing method
CN109180175A (en) * 2018-10-25 2019-01-11 河北大洲智造科技有限公司 A kind of photocuring 3D printing bioceramic slurry and preparation method thereof, bone tissue engineering scaffold and its application
CN110075359A (en) * 2019-03-26 2019-08-02 华南理工大学 A kind of ultrasonic wave added prepares porous bone cement bracket and preparation method thereof
CN110075349A (en) * 2019-04-09 2019-08-02 温州医科大学 A kind of bioactivity glass compound rest and application
CN110357657A (en) * 2019-08-15 2019-10-22 河北大洲智造科技有限公司 A kind of 3D printing bioceramic slurry and preparation method thereof, a kind of bio-ceramic artificial bone and preparation method thereof
CN110665063A (en) * 2019-10-28 2020-01-10 中国人民解放军第四军医大学 3D biological printing ink and preparation method thereof, tissue engineering scaffold and preparation method thereof
CN110721336A (en) * 2019-11-26 2020-01-24 许雄程 Nano lithium magnesium silicate/polycaprolactone composite material and preparation method thereof
CN111012947A (en) * 2019-12-30 2020-04-17 南京财经大学 Injectable and self-healing starch-based hydrogel and preparation method and application thereof
CN111070376A (en) * 2019-12-25 2020-04-28 西安点云生物科技有限公司 3D printing bionic porous bioceramic artificial bone and preparation method thereof
CN112960988A (en) * 2021-02-02 2021-06-15 烟台正海生物科技股份有限公司 3D printing cuttable biological ceramic support and preparation method and application thereof

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104163622A (en) * 2014-06-06 2014-11-26 上海交通大学附属第一人民医院 Preparation method and application of laponite bioceramics
CN104325644A (en) * 2014-10-20 2015-02-04 西安点云先进材料科技有限公司 Filament-free three-dimensional printing method
CN109180175A (en) * 2018-10-25 2019-01-11 河北大洲智造科技有限公司 A kind of photocuring 3D printing bioceramic slurry and preparation method thereof, bone tissue engineering scaffold and its application
CN110075359A (en) * 2019-03-26 2019-08-02 华南理工大学 A kind of ultrasonic wave added prepares porous bone cement bracket and preparation method thereof
CN110075349A (en) * 2019-04-09 2019-08-02 温州医科大学 A kind of bioactivity glass compound rest and application
CN110357657A (en) * 2019-08-15 2019-10-22 河北大洲智造科技有限公司 A kind of 3D printing bioceramic slurry and preparation method thereof, a kind of bio-ceramic artificial bone and preparation method thereof
CN110665063A (en) * 2019-10-28 2020-01-10 中国人民解放军第四军医大学 3D biological printing ink and preparation method thereof, tissue engineering scaffold and preparation method thereof
CN110721336A (en) * 2019-11-26 2020-01-24 许雄程 Nano lithium magnesium silicate/polycaprolactone composite material and preparation method thereof
CN111070376A (en) * 2019-12-25 2020-04-28 西安点云生物科技有限公司 3D printing bionic porous bioceramic artificial bone and preparation method thereof
CN111012947A (en) * 2019-12-30 2020-04-17 南京财经大学 Injectable and self-healing starch-based hydrogel and preparation method and application thereof
CN112960988A (en) * 2021-02-02 2021-06-15 烟台正海生物科技股份有限公司 3D printing cuttable biological ceramic support and preparation method and application thereof

Similar Documents

Publication Publication Date Title
ES2197046T3 (en) PROCEDURE TO PRODUCE CERAMIC PARTICLES.
Zhao et al. Robocasting of silicon nitride with controllable shape and architecture for biomedical applications
CN110101904B (en) Degradable regenerative medical material for promoting tissue in-situ regeneration and preparation method thereof
Feng et al. Toughening and strengthening mechanisms of porous akermanite scaffolds reinforced with nano-titania
CN105330285B (en) A kind of 3D printing ZrO2Toughening bioactive ceramics powder body material and its preparation and application
Petit et al. Novel calcium phosphate/PCL graded samples: Design and development in view of biomedical applications
CN107235721A (en) A kind of porous Bredigites biological ceramic support of 3 D-printing and preparation method and application
Li et al. Fabrication of bioceramic scaffolds with pre-designed internal architecture by gel casting and indirect stereolithography techniques
CN115177787B (en) 3D printing composite bone repair material and preparation method and application thereof
KR101481988B1 (en) Method for preparing porous ceramic scaffold
CN110882419A (en) Self-curing calcium phosphate bone cement scaffold and preparation method and application thereof
Lin et al. Doping polyvinyl alcohol can improve the injectability of biological ceramics in 3D printing and influence the adhesion of cells to the scaffolds after sintering
CN107050513A (en) A kind of gradient dip-coating HA prepares ZrO2The method of Bone Defect Repari bioceramic scaffold material
CN115137876A (en) Hectorite bioceramic artificial bone and preparation method thereof
CN107007888B (en) Photocuring 3D printing technology-based individualized and customized zirconium dioxide porous biological bone repair scaffold and preparation method thereof
Shahi et al. Evaluation of physical and mechanical properties of B-tri-calcium phosphate/poly-3-hydroxybutyrate nanocomposite scaffold for bone tissue engineering application
CN106178099A (en) The forming technique of direct write without mould prepares the method for titanium/hydroxylapatite biology support
CN115054725B (en) Hectorite 3D printing artificial bone scaffold and preparation method thereof
Yang et al. Fabrication of β-TCP scaffold with pre-designed internal pore architecture by rapid prototyping of mask projection stereolithography
Rumian et al. The influence of sintering conditions on microstructure and mechanical properties of titanium dioxide scaffolds for the treatment of bone tissue defects
CN112704767B (en) Personalized customized bone organ manufactured accurately in 4D mode and preparation method thereof
CN112028620B (en) Porous hydroxyapatite bioactive material and preparation method and application thereof
EP3398922A1 (en) Porous material and method for preparing same
Ignjatović et al. Biodegradable composites based on nanocrystalline calcium phosphate and bioresorbable polymers
Liu et al. Effect of Sr2+ on 3D gel-printed Sr3− x Mg x (PO4) 2 composite scaffolds for bone tissue engineering

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20221004