CN113666753B - Bionic human bone based on digital light processing molding technology and preparation method thereof - Google Patents

Bionic human bone based on digital light processing molding technology and preparation method thereof Download PDF

Info

Publication number
CN113666753B
CN113666753B CN202110898918.2A CN202110898918A CN113666753B CN 113666753 B CN113666753 B CN 113666753B CN 202110898918 A CN202110898918 A CN 202110898918A CN 113666753 B CN113666753 B CN 113666753B
Authority
CN
China
Prior art keywords
human bone
bionic human
ceramic
sintering
bionic
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.)
Active
Application number
CN202110898918.2A
Other languages
Chinese (zh)
Other versions
CN113666753A (en
Inventor
伍尚华
黄生武
孙振飞
杨平
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.)
Guangdong University of Technology
Original Assignee
Guangdong University of Technology
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 Guangdong University of Technology filed Critical Guangdong University of Technology
Priority to CN202110898918.2A priority Critical patent/CN113666753B/en
Publication of CN113666753A publication Critical patent/CN113666753A/en
Application granted granted Critical
Publication of CN113666753B publication Critical patent/CN113666753B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • 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
    • 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
    • B33Y70/10Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • 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
    • 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
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • 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
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/75Products with a concentration gradient

Abstract

The invention discloses a bionic human bone based on a digital light processing forming technology and a preparation method thereof, and relates to the technical field of ceramic bionic human bones. The method comprises the following steps: s1, preparing ceramic slurry with gradient solid phase content; s2, printing out green bodies with solid phase contents; s3, degreasing and sintering the blank to obtain ceramic pieces with solid phase content, and measuring the shrinkage rate of each ceramic piece; s4, adjusting the design size of the adjacent layers of ceramic pieces of the reference ceramic piece according to the multi-layer structure model of the bionic human bone by taking the shrinkage rate of the ceramic piece with one solid content as a reference; and S5, printing a blank according to the adjusted bionic human bone model, degreasing and sintering to obtain the bionic human bone. The invention obtains the ceramic piece with gradient solid content and the shrinkage rate in advance, redesigns the dimension of the bionic human bone model, and further prepares the bionic human bone of the gradient material, and the joint surface of each layer in the bionic human bone can not crack and bend, and the porosity and the bending strength in the bionic human bone are in gradient change.

Description

Bionic human bone based on digital light processing molding technology and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic bionic human bones, in particular to a bionic human bone based on a digital light processing molding technology and a preparation method thereof.
Background
Silicon nitride (Si) 3 N 4 ) The ceramic is a high-performance structural ceramic, and has high strength, high hardness, good chemical stability, antifriction and wear resistance. The method is widely applied to the high-end technical fields of aerospace, mechano-electronics, chemical metallurgy and the like. At the same time, scholars research and discover Si 3 N 4 Has good biocompatibility and partial ray permeability. For example: when taking X-ray film, the most clear image is obtained of human skeleton tissue. Bone tissue containing calcium salt is the most dense normal human tissue, and contains calcium element capable of absorbing X-rays in a large amount. As with human bones, various metals can also absorb a great deal of X-raysLeaving its shadow on the photo negative. Many metals are even fully X-ray absorbing. When taking X-ray films, the patient is provided with necklace, coin or metal implant and other metal articles, which can cover the human body structure which the doctor wants to see and influence the examination effect. The high density of metal articles leaves behind large, abnormal images with metallic foreign objects as the core, called metallic artifacts, on the computer reconstructed X-ray projection images. The artifact not only can shade human tissues around the metal, so that the image quality is reduced, but also can form a large-scale position-offset shadow, so that the image cannot be observed at all. Thus Si is 3 N 4 Ceramics are also regarded as novel biomedical materials capable of replacing metal alloys, and have great application potential in the field of repairing or replacing bone defects.
In the field of high-end biomedical applications, biomedical material products are often required to have complex structures and functions. For example: human bone is essentially a heterogeneous structure with pores and young's modulus that gradually change from outside to inside. Therefore, the material with single performance is difficult to prepare the material which is completely similar to human bone in terms of structure and function, and the biomedical material with the structure and performance which is more similar to human body is hopeful to be prepared by using multi-material or gradient material. The ceramic material has the characteristics of high hardness and low toughness, and the traditional process (such as grinding, injection molding and the like) cannot be used for processing complex structural parts or parts with higher geometric curved surfaces. Digital Light Processing (DLP) molding has the characteristics of no mold molding, high automation degree in the molding process, high dimensional accuracy and higher system resolution, is very suitable for manufacturing models or parts with complex structures, and can prepare complex structures according to individual requirements, thereby providing a feasible method for preparing products with complex structures and functions.
The current problem of the gradient material 3D printing ceramic is that stress is generated at the joint surface of adjacent layers due to different degreasing and shrinkage rates after sintering of different layers in the gradient material, so that cracks are generated at the joint surface, and a bending phenomenon occurs. For example: printing Si with 3D 3 N 4 In the preparation of biological ceramic human skeleton, si is required 3 N 4 Porosity of the porous materialSequentially increasing from outside to inside. After being printed by DLP, the shrinkage rate of each layer is inconsistent when degreasing and cofiring due to the gradient layer in the bionic human bone. In order to reduce the mismatch of sintering shrinkage, the shrinkage behavior of the two must be made as close as possible. However, in the case of a fixed composition and particle size of the bionic human bone material, the corresponding adjustment space for the sintering shrinkage is limited.
Disclosure of Invention
The invention aims to solve the technical problems that the composition and the particle size of the bionic human bone gradient ceramic material are fixed, and the sintering shrinkage rates of different layers are mismatched, so that cracks appear on a joint surface and the quality is affected.
In this regard, the invention provides a bionic human bone prepared based on a digital light processing molding technology and a method thereof. The principle is as follows: firstly, testing the linear shrinkage rate of a single solid phase after sintering through experiments; then, when designing the bionic human bone print model, the size of one layer of the adjacent layers is proportionally enlarged or reduced by taking the shrinkage rate of the other layer as a reference, so that the sizes of the two adjacent layers after sintering are consistent.
Specifically, the technical scheme of the invention is as follows:
a bionic human bone preparation method based on digital light processing molding technology comprises the following steps:
s1, preparing ceramic slurry with gradient solid phase content;
s2, printing out green bodies with solid phase contents by adopting a digital light processing molding technology;
s3, degreasing and sintering the blank to obtain ceramic pieces with solid phase content, and measuring the shrinkage rate of each ceramic piece;
s4, adjusting the design size of the adjacent layers of ceramic pieces of the reference ceramic piece according to the multi-layer structure model of the bionic human bone by taking the shrinkage rate of the ceramic piece with one solid content as a reference;
and S5, printing out each layer of green body according to the adjusted bionic human bone model, degreasing and sintering to obtain the bionic human bone.
Specifically, the adjustment mode of S4 is to enlarge or reduce the design size of the adjacent layer ceramic piece.
Further, the solid phase content of the ceramic slurry ranges from 30vol% to 45 vol%.
Further, the ceramic slurry comprises silicon nitride powder, a sintering aid, a silane coupling agent, resin, a photoinitiator and a dispersing agent.
Further, the sintering aid accounts for 5-15 wt% of the sum of the sintering aid and the silicon nitride powder.
Further, the usage amount of the silane coupling agent accounts for 1-3 wt% of the sum of the sintering aid and the silicon nitride powder.
Further, the sintering aid is selected from any two of alumina, yttria, and magnesia.
Further, the silane coupling agent is selected from at least one of KH550, KH560 and KH 570.
Furthermore, the silicon nitride powder is alpha-phase silicon nitride, and the purity is more than 99.8%.
Specifically, when ceramic slurry is prepared, firstly, ball milling is carried out on a sintering aid and silicon nitride powder for 4-8 hours at 320-380r/min by using a planetary ball mill, and then, drying and sieving are carried out; the drying temperature is 50-70deg.C, and the sieving is 80-120 mesh.
Further, the degreasing mode is a combination of vacuum degreasing and air degreasing, and the degreasing is a vacuum and air 2-step degreasing method.
Further, the sintering temperature is 1600-2000 ℃, preferably 1800 ℃.
The invention also provides a bionic human bone made of the gradient ceramic material, and the bionic human bone is prepared by the bionic human bone preparation method based on the digital light processing molding technology.
Compared with the prior art, the invention has the following technical effects:
according to the bionic human bone preparation method based on the digital light processing molding technology, according to the ceramic piece with the gradient solid content and the corresponding shrinkage rate obtained in advance, the design size of the adjacent layer ceramic piece of the reference ceramic piece is adjusted based on the shrinkage rate of the ceramic piece with the solid content, and the bionic human bone model is redesigned to obtain, so that the bionic human bone can be prepared by using the ceramic material with the gradient solid content, cracks and bending do not occur on the joint surface of each layer in the bionic human bone, and the porosity and the bending strength in the bionic human bone are changed in a gradient manner.
Drawings
FIG. 1 is a three-dimensional model of a biomimetic human bone, wherein (a) is a single layer model; (b) a pre-adjusted simulated human bone model; (c) a re-designed bionic human bone model after adjustment;
FIG. 2 is a physical diagram of different embodiments;
FIG. 3 is an SEM image of a ceramic part having different solids contents, wherein (a) is the SEM morphology of the ceramic part having a solids content of 35 vol%; (b) SEM morphology of the ceramic part with a solids content of 38 vol%.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments. It will be apparent that the embodiments described below are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention. As used in the specification of the embodiments of the invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The embodiment of the invention provides a bionic human bone preparation method based on a digital light processing molding technology, which comprises the following steps of:
s1, preparing ceramic slurry with gradient solid phase content;
in specific implementation, the ceramic slurry comprises silicon nitride powder, a sintering aid, a silane coupling agent, resin, a photoinitiator and a dispersing agent.
The sintering aid accounts for 8wt% of the sum of the sintering aid and the silicon nitride powder.
The usage amount of the silane coupling agent is 1.5 weight percent of the sum of the sintering aid and the silicon nitride powder.
The sintering aid is selected from the group consisting of a mixture of yttria and magnesia.
The silane coupling agent is selected from KH560.
The silicon nitride powder is alpha-phase silicon nitride with purity more than 99.8%.
The resin is selected from BPA10EODMA, HDDA, PPTTA, n-octanol
In the concrete implementation, when preparing the ceramic slurry, firstly, ball milling the sintering aid and the silicon nitride powder for 6 hours at 350r/min by using a planetary ball mill, fully and uniformly mixing, drying and sieving; the drying temperature is 60 ℃, and the powder is sieved by a 100-mesh sieve.
In a specific implementation, the solid phase content of the ceramic slurry ranges from 30vol% to 45 vol%.
For example, in one embodiment, ceramic slurries having solids contents of 35vol%,38vol%,40vol%,42vol%,45vol% are separately prepared.
S2, printing out green bodies with solid phase contents by adopting a digital light processing molding technology;
in specific implementation, referring to fig. 1, as shown in fig. 1 (a), according to the single-layer printing model of fig. 1 (a), a blank with each solid phase content is printed by using a digital light processing forming technology.
S3, degreasing and sintering the blank to obtain ceramic pieces with solid phase content, and measuring the shrinkage rate of each ceramic piece;
in the concrete implementation, degreasing and sintering the blank to obtain the ceramic piece.
The degreasing mode is a combination of vacuum degreasing and air degreasing, and the degreasing is a vacuum and air 2-step degreasing method.
Sintering the ceramic at 1800 ℃ to obtain ceramic pieces with various solid phase contents.
For example, in one embodiment, a blank printed according to the model shown in fig. 1 (a) is shown in fig. 2 (a); the physical diagram of the blank after degreasing is shown in (b) of fig. 2; the ceramic part physical diagram obtained after sintering is shown in (c) of fig. 2; from the above figures, it is clear that, when a single layer of the model is printed, the sample will not crack or bend after degreasing and sintering for any single solid content sample.
Shrinkage and other properties of each solid content ceramic part were measured and the results are shown in Table 1 below.
TABLE 1 Properties of the ceramic parts with solids content
Ceramic part numbering 11 12 13 14 15
Solid content 35vol% 38vol% 40vol% 42vol% 45vol%
Shrinkage/% 25.41 24.25 23.63 21.53 20.27
Porosity/% 28.42 26.36 25.01 23.47 21.25
Flexural Strength/MPa 442.3 453.4 468.7 488.2 497.1
Wherein, the SEM morphology of the ceramic members 11, 12 with the solid content of 35vol% and 38vol% is shown in (a) and (b) of FIG. 3.
S4, adjusting the design size of the adjacent layers of ceramic pieces of the reference ceramic piece according to the multi-layer structure model of the bionic human bone by taking the shrinkage rate of the ceramic piece with one solid content as a reference;
and S5, printing out each layer of green body according to the adjusted bionic human bone model, degreasing and sintering to obtain the bionic human bone.
For example, in one embodiment, the ceramic part 11 with a solid content of 35vol% is used as a reference ceramic part, and the solid content of the ceramic part of the adjacent layer is 38vol%, and as shown in the results of table 1, the shrinkage of 38vol% of the solid content is smaller, and the design size with 38vol% of the solid content needs to be enlarged, so as to obtain a redesigned bionic human bone model, as shown in fig. 1 (c).
In one embodiment, the ceramic part 12 with a solid content of 38vol% is used as a reference ceramic part, and the solid content of the ceramic part in the adjacent layer is 40vol%, and as shown in the results of table 1, the shrinkage rate of 40vol% of the solid content is smaller, and the design size with the solid content of 40vol% needs to be enlarged, so as to obtain the redesigned bionic human bone model.
In one embodiment, the ceramic piece 13 with a solid content of 40vol% is used as a reference ceramic piece, the solid content of the ceramic piece in the adjacent layer is 42vol%, and according to the results in table 1, the shrinkage rate of the solid content of 42vol% is smaller, and the design size with the solid content of 42vol% needs to be enlarged, so as to obtain the redesigned bionic human bone model.
In one embodiment, the ceramic part 14 with a solid content of 42vol% is used as a reference ceramic part, and the solid content of the ceramic part in the adjacent layer is 45vol%, and as shown in the results of table 1, the shrinkage rate of the solid content of 45vol% is smaller, and the design size with the solid content of 45vol% needs to be enlarged, so as to obtain the redesigned bionic human bone model.
In one embodiment, the redesigned model of the bionic human bone is shown in fig. 1 (c), and the blank printed from this model is shown in fig. 2 (g); the physical diagram of the blank after degreasing is shown in (h) of fig. 2; the ceramic part real object diagram obtained after sintering is shown in (i) of fig. 2; from the above figures, it can be seen that, when a model with a gradient solid content is printed, the shrinkage of the sample with different solid contents is known, so that the dimension of the model with the bionic human bone is redesigned according to the shrinkage, and the sample with the double-layer structure can not crack and bend after degreasing and sintering. Three or more layers of ceramic materials with gradient solid content can be prepared by similar methods.
Comparative example
Preparing gradient bionic human bone with solid content of 42vol% and 45vol%, wherein the sizes of layers in the bionic human bone model are consistent, the model is shown in a figure 1 (b), and the bionic human bone prepared by the model can crack and bend on the joint surfaces with different solid contents after degreasing and sintering, and the figure is shown as (e) and (f) in a figure 2; (e) The degreased physical image, (f) the sintered physical image, and (d) in fig. 2 is a green body physical image printed according to the model of fig. 1 (b). As can be seen from the figure, the silicon nitride solid phase content in each gradient layer is different, and the silicon nitride solid phase content has different linear shrinkage rates in the sintering process, so that stress is generated on the bonding surface of the adjacent layers, cracks appear, and the silicon nitride solid phase layer bends towards the direction with low solid content.
In summary, according to the bionic human bone preparation method based on the digital light processing molding technology, according to the ceramic piece with gradient solid content and the corresponding shrinkage rate obtained in advance, the design size of the adjacent layer ceramic piece of the reference ceramic piece is adjusted based on the shrinkage rate of the ceramic piece with one solid content, and the bionic human bone model is redesigned to obtain, so that the bionic human bone can be prepared by using the ceramic material with the gradient solid content, and the joint surface of each layer in the bionic human bone does not crack or bend, and the porosity and the bending strength in the bionic human bone have the technical effect of gradient change.
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.

Claims (4)

1. The bionic human bone preparation method based on the digital light processing forming technology is characterized by comprising the following steps of:
s1, preparing ceramic slurry with gradient solid phase content ranging from 30vol% to 45 vol%;
s2, printing out green bodies with solid phase contents by adopting a digital light processing molding technology;
s3, degreasing and sintering the blank to obtain ceramic pieces with solid phase content, and measuring the shrinkage rate of each ceramic piece;
s4, adjusting the design size of the adjacent layers of ceramic pieces of the reference ceramic piece according to the multi-layer structure model of the bionic human bone by taking the shrinkage rate of the ceramic piece with one solid content as a reference;
s5, printing each layer of green body according to the adjusted bionic human bone model, degreasing and sintering to obtain the bionic human bone;
the principle of adjusting the design size of the adjacent layer ceramic piece is as follows: firstly, testing the linear shrinkage rate of a ceramic piece with single solid content after sintering through experiments; then, when designing the bionic human bone printing model, the size of one layer of the adjacent layers is proportionally enlarged or reduced by taking the shrinkage rate of the other layer as a reference, so that the sizes of the two adjacent layers after sintering are consistent;
the ceramic slurry comprises silicon nitride powder, a sintering aid, a silane coupling agent, resin, a photoinitiator and a dispersing agent; wherein the sintering aid accounts for 5-15 wt% of the total weight of the sintering aid and the silicon nitride powder; the dosage of the silane coupling agent accounts for 1-3 wt percent of the sum of the sintering aid and the silicon nitride powder; the sintering aid is any two selected from aluminum oxide, yttrium oxide and magnesium oxide; the silicon nitride powder is alpha-phase silicon nitride with purity more than 99.8%.
2. The method for preparing a bionic human bone based on digital light processing molding according to claim 1, wherein the silane coupling agent is at least one selected from KH550, KH560 and KH 570.
3. The method for preparing the bionic human bone based on the digital light processing molding technology as claimed in claim 1, wherein the degreasing is a 2-step degreasing method of vacuum degreasing and air degreasing; the temperature during sintering is 1600-2000 ℃.
4. A bionic human bone, characterized in that the material is a gradient ceramic material, and the bionic human bone is prepared by the bionic human bone preparation method based on the digital light processing molding technology as set forth in any one of claims 1-3.
CN202110898918.2A 2021-07-30 2021-07-30 Bionic human bone based on digital light processing molding technology and preparation method thereof Active CN113666753B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110898918.2A CN113666753B (en) 2021-07-30 2021-07-30 Bionic human bone based on digital light processing molding technology and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110898918.2A CN113666753B (en) 2021-07-30 2021-07-30 Bionic human bone based on digital light processing molding technology and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113666753A CN113666753A (en) 2021-11-19
CN113666753B true CN113666753B (en) 2023-12-26

Family

ID=78541594

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110898918.2A Active CN113666753B (en) 2021-07-30 2021-07-30 Bionic human bone based on digital light processing molding technology and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113666753B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114213021B (en) * 2021-12-23 2024-03-19 温州医科大学附属口腔医院 Gradient bionic dental ceramic
CN115385721B (en) * 2022-08-29 2023-08-08 广东工业大学 Porous bionic human bone with controllable pore structure based on photo-curing molding and preparation method thereof
CN116177995B (en) * 2022-09-07 2024-03-12 中国科学院上海硅酸盐研究所 Preparation method of fluorescent ceramic based on 3D printing composite structure

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107586136A (en) * 2017-10-17 2018-01-16 广东工业大学 A kind of method of 3D printing silicon nitride ceramics
CN110317059A (en) * 2019-07-09 2019-10-11 成都贝施美医疗科技股份有限公司 A kind of each uniform layering zirconium oxide porcelain block technology of layer contraction

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107586136A (en) * 2017-10-17 2018-01-16 广东工业大学 A kind of method of 3D printing silicon nitride ceramics
CN110317059A (en) * 2019-07-09 2019-10-11 成都贝施美医疗科技股份有限公司 A kind of each uniform layering zirconium oxide porcelain block technology of layer contraction

Also Published As

Publication number Publication date
CN113666753A (en) 2021-11-19

Similar Documents

Publication Publication Date Title
CN113666753B (en) Bionic human bone based on digital light processing molding technology and preparation method thereof
Schwarzer et al. Process development for additive manufacturing of functionally graded alumina toughened zirconia components intended for medical implant application
Du et al. Binder jetting additive manufacturing of ceramics: A literature review
Suwanprateeb et al. Influence of raw powder preparation routes on properties of hydroxyapatite fabricated by 3D printing technique
JP2019513901A (en) Three-dimensional printing of cermet or cemented carbide
CN109865838B (en) Additive manufacturing technology and application thereof
Chen et al. Microstructure and mechanical properties of 3Y-TZP dental ceramics fabricated by selective laser sintering combined with cold isostatic pressing
WO2020245645A1 (en) A green body composition and functional gradient materials prepared thereof
WO2006053044A1 (en) Fine grain titanium-alloy article and articles with clad porous titanium surfaces
KR20120062705A (en) Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body
Xia et al. Effect of solid loading on properties of zirconia ceramic by direct ink writing
Pavón et al. Development of new titanium implants with longitudinal gradient porosity by space-holder technique
de Camargo et al. Additive manufacturing of electrofused mullite slurry by digital light processing
CN111876642A (en) Hard carbide powder for additive manufacturing
Kachit et al. Direct-ink writing and compression behavior by in situ micro-tomography of architectured 316L scaffolds with a two-scale porosity
Miura et al. Mechanical and surface properties of additive manufactured zirconia under the different building directions
Sarkar et al. Uniaxial Compaction‐Based Manufacturing Strategy and 3D Microstructural Evaluation of Near‐Net‐Shaped ZrO2‐Toughened Al2O3 Acetabular Socket
KR101239112B1 (en) Method for Preparing Porous Titanium-Hydroxyapatite Composite
Ortmann et al. Preparation and characterization of ZTA bioceramics with and without gradient in composition
Coffigniez et al. Sinter‐Based Additive Manufacturing of Graded Porous Titanium Scaffolds by Multi‐Inks 3D Extrusion
CN108638494B (en) Preparation method of calcium phosphate porous scaffold
JP5926169B2 (en) Ceramic granules, ceramic sintered body and protective member
Graf et al. Influence of printing procedure and printing axis of dental alloys on dimensional accuracy, surface roughness, and porosity
CN113402282A (en) Bionic human bone based on 3D printing and manufacturing method thereof
İyibilgin et al. Characterization of CP-Titanium produced via binder jetting and conventional powder metallurgy

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
GR01 Patent grant
GR01 Patent grant