CN109910131A - A kind of slurry and manufacturing process of enhanced type silicon hydrochlorate porous ceramics scaffold - Google Patents
A kind of slurry and manufacturing process of enhanced type silicon hydrochlorate porous ceramics scaffold Download PDFInfo
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- CN109910131A CN109910131A CN201910287260.4A CN201910287260A CN109910131A CN 109910131 A CN109910131 A CN 109910131A CN 201910287260 A CN201910287260 A CN 201910287260A CN 109910131 A CN109910131 A CN 109910131A
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Abstract
A kind of slurry and manufacturing process of enhanced type silicon hydrochlorate porous ceramics scaffold, the present invention provides a kind of slurry for preparing silicate porous ceramics scaffold, including by silicate powder and the reinforced phase powder being entrained in silicate powder is formed by composite ceramic material and bonding agent forms.The present invention also provides a kind of manufacturing process that porous ceramics scaffold is prepared with extrusion deposition technique, including configuring the above-mentioned composite ceramics slurry containing silicate powder, reinforced phase powder and bonding agent；The three-dimensional entity model of porous ceramics scaffold to be printed is designed and generated, determine printing thickness and print speed and slicing delamination, planning path are carried out to model；Extruded velocity is set or squeezes out pressure, squeezes out and deposits above-mentioned composite ceramics slurry, form porous silicate ceramics bracket idiosome；Above-mentioned porous ceramics scaffold is sintered to obtain porous ceramics scaffold finished product.
Description
Technical field
The present invention relates to the slurries and manufacturing process of a kind of enhanced type silicon hydrochlorate porous ceramics scaffold, and in particular to biological material
Material field and ceramic material increasing field.
Background technique
With the propulsion of aging of population process, the promotion of health of people health care consciousness and the generation of all kinds of accidents, people
The Treatment need of bone tissue is constantly promoted, however bone tissue defect treatment be always perplex relevant medical personnel difficulty
Topic.Currently used implantation technique is often due to the problems such as donor is limited and post-operative recovery, using being subject to certain restrictions.Cause
This, correlative study person places hope on the material and method for being used to treat bone defect of artificial synthesized a new generation.
Currently used artificial synthesized bone defect material includes synthesis high molecular material, metal material, composite material and nothing
Machine nonmetallic materials, the wherein most development potentiality of the bioceramic in inorganic non-metallic material.Metal material and other are inorganic
Inert material often due to " stress shielding " and can not the other reasons such as degradation in vivo, there are still ask for actual therapeutic effect
Topic；That emerged in large numbers in recent years gets growing concern for by the bioceramic of representative of hydroxyapatite, although its bio-compatible
Property it is excellent, but experiments have shown that hydroxyapatite is to the proliferation of osteoblast, differentiation without apparent facilitation.However nearest
The study found that silicon ion has apparent facilitation to osteoblast, and compared to other biological ceramics, one calcium base biology of silicon
Ceramics have faster mineralization velocity, are conducive to the recovery at bone defect position.
Porous ceramics scaffold is the ideal implant for treating bone defect, the aperture and hole that internal connectivity is good, suitable
Rate facilitate neoblast grow into and be proliferated and the transport of nutritional ingredient, limit what ceramic porous bracket further developed at present
Reason is that the mechanical strength of porous ceramics scaffold is to be improved.Traditional stent fabrication techniques include foaming, infusion process with
And pore creating material method etc., although these methods can prepare the porous ceramics scaffold of certain pore size and porosity, there are still brackets
The problems such as connectivity of internal holes is bad and the mechanical strength of bracket is not high.It is latent to be known as great development for 3D printing technique at present
The manufacturing technology of power, 3D printing technique has effigurate 3D solid by accumulating to be formed by material layers, and 3D
Printing technique is also just being increasingly used in biological support manufacture.One kind that deposition technique is 3D printing technique is squeezed out, it should
Method is squeezed out fluidised form material using the motive force that motor or compressed air generate from slurry chamber, is sunk in a manner of continuous fibers
Product is on printing substrate, and successively accumulation forms 3D solid structure.This method can prepare the exemplar, processable more of complicated shape
The factor unfavorable to biomaterial will not be introduced in the material (solution, colloid, suspension etc.) and process of kind state, with
The continuous development and maturation of the technology, the technology be expected to solve the problems, such as bone tissue engineering scaffold processing difficulties.
Summary of the invention
A kind of slurry and manufacturing process of enhanced type silicon hydrochlorate porous ceramics scaffold, based on the above situation, the present invention propose
A kind of slurry and manufacturing process of enhanced type silicon hydrochlorate porous ceramics scaffold, particularly by by reinforced phase powder and silicate
Powder is mixed and made into composite ceramic material in proportion, is then mixed with composite ceramic material and adhesive solution in proportion multiple
Ceramic slurry is closed, prepares porous ceramics scaffold finally by deposition technique is squeezed out.
In a specific example, the silicate powder includes calcium silicates, diopside, akermanite, bredigite
At least one of, and diameter of particle is in 5nm~50um.
The reinforced phase powder includes at least one of carbon fibre, metal oxide；
The carbon fibre includes at least one of carbon fiber, carbon nanotube, graphene；
The metal oxide includes at least one of zirconium oxide, magnesia, aluminium oxide, titanium oxide.
The binder, which is characterized in that including polyvinyl alcohol, carboxymethyl cellulose, in pluronic F-127 extremely
Few one kind.
In a specific example, the composite ceramic material, feature includes silicate powder in composite powder constitution
Measuring accounting is 70%~95%, and reinforced phase powder quality accounting is 5%~30%.
In a specific example, the bonding agent need to incorporate corresponding solvent, and the mass fraction of adhesive solution is
10%~40%；The composite ceramic material is uniformly mixed to form composite mortar with adhesive solution, wherein composite ceramic material
Mass ratio with adhesive solution is 4: 3~3: 1.
A kind of extrusion deposition ceramic shaping method, specific steps include:
The composite ceramic material and adhesive solution for being used to prepare porous ceramics scaffold configured according to the above ratio is provided；
Above-mentioned composite ceramic material and adhesive solution are mixed according to the above ratio, are configured to prepare porous ceramics branch
The composite ceramics slurry of frame；
Design and generate porous support threedimensional model to be printed, setting printing thickness, extruded velocity and print speed
Composite ceramics slurry is fitted into home-made contrivance barrel, forms porous ceramics scaffold idiosome through extrusion printing by equal print parameters；
In a specific example, above-mentioned printing thickness is 0.1~0.4mm.
The invention has the following beneficial effects:
(1) silicate ceramics not only has excellent biocompatibility, moreover it is possible to which the proliferation and differentiation for promoting osteoblast are expected to
Bone defect healing field is more applied, the present invention using silicate ceramics as composite ceramics substrate and with carbon fibre with
And nano-ceramic particle carries out toughening to silicate ceramics, improves the mechanical strength of silicate porous support, is expected to be used for clinic
In bone defect healing；
(2) the extrusion deposition modeling technology that the present invention uses, this method will using the motive force that motor or compressed air generate
Fluidised form material is squeezed out from slurry chamber, is deposited on printing substrate in a manner of continuous fibers, and successively accumulation forms 3D solid knot
Structure.The processing characteristics for squeezing out deposit manufacture technology are as follows: 1. can realize all highly complex and controllable three-dimensional structure of external and internal compositions
Preparation；2. suitable material range is wide, the material of the states such as solution, colloid, suspension, molten mass is formable；3. using more
Spray head deposition formation is, it can be achieved that change of gradient on ingredient；4. printing environment does not introduce to bioactive materials (such as cell, life
The long factor) harmful factor.It is contemplated that the technology is expected to solve bone tissue work with the continuous development and maturation of the technology
The problem of engineering support processing difficulties.
(3) composite ceramic material provided by the present invention increases the material type for being used to prepare porous ceramics scaffold, certain journey
Solve the problems, such as that conventional porous ceramics bracket mechanical strength is low and internal connectivity is poor on degree, and present invention incorporates squeeze
Deposition technique out prepares different types of porous ceramics scaffold using the slurry of a variety of different conditions and selects for related researcher
With.
Detailed description of the invention
Porous ceramics scaffold preparation process schematic diagram；
Porous ceramics scaffold preparation facilities structural schematic diagram, wherein 1 moves slide unit for X-axis, 2 be forming platform, and 3 be material
Cylinder, 4 be electric linear push rod, and 5 move slide unit for Y-axis, and 6 move slide unit for Z axis, and 7 be sealing piston, and 8 be push rod, and 9 be nozzle.
Specific embodiment
Goal of the invention, technical solution and technical effect of the invention are illustrated to be more clear, and with reference to the accompanying drawing and are had
The present invention is further illustrated for body case study on implementation.
The present invention provides a kind of slurry of enhanced type silicon hydrochlorate porous ceramics scaffold, in a specific embodiment, silicic acid
Salt selects calcium silicates powder, and bonding agent selects polyvinyl alcohol, and reinforced phase selects carbon fiber powder.
Referring to Fig. 1, the present invention also provides a kind of extrusions to deposit ceramic shaping method, the specific steps are as follows:
1. configuring composite ceramic material and adhesive solution in proportion.In proportion by calcium silicate powder and carbon fiber powder
It is mixed to form composite ceramic material, wherein calcium silicate powder is 70%~95% in composite ceramic weight accounting, carbon fiber
Powder quality accounting is 5%~30%；Then polyvinyl alcohol is dissolved in deionized water and forms adhesive solution, wherein poly- second
The mass fraction of enolate solution is 10%~40%.
2. configuring composite ceramics slurry in proportion.Above-mentioned composite ceramic material and bonding solution are mixed to form composite ceramics
Slurry, wherein the mass ratio of above-mentioned composite ceramic material and adhesive solution is 4: 3~3: 1.
3. designing, generating porous ceramics scaffold threedimensional model to be printed, and print parameters are set.It in this step can benefit
Porous ceramics scaffold to be printed is designed with 3 d modeling software Solidworks or Creo and is stored as stl file, then will
Stl file import slices software Cura or Slic3r are arranged after the print parameters such as print speed and thickness and produce phase
The Motor execution code file answered.
4. composite ceramics slurry is fitted into the barrel of printing equipment, porous support idiosome is printed as through squeezing out.Refering to Fig. 2
Printing equipment structural schematic diagram, printing equipment are mainly made of following several parts: X-axis moves slide unit (1), forming platform (2), material
Cylinder (3), electric linear push rod (4), Y-axis move slide unit (5), and Z axis moves slide unit (6).Motor execution code file is imported and is filled
After setting control section, the pusher portion of electric linear push rod will move downward compression seal piston, be pressed further by barrel and work as
In ceramic slurry squeezed out from nozzle, and XYZ axis movement slide unit at this time also simultaneously move drive electric linear push rod by planning
Path movement, can so form porous ceramics scaffold idiosome.
5. porous support is heat-treated to obtain porous ceramics scaffold finished product.
Then with micro- sem observation porous scaffold surface pattern, internal connectivity, and with the hole of SEM measurement porous support
And hole wall thickness.
With the porosity of Archimedes's drainage measurement porous ceramics scaffold.
Claims (8)
1. a kind of slurry of enhanced type silicon hydrochlorate porous ceramics scaffold, it is characterised in that in carbon fibre, metal oxide
At least one is used as reinforced phase powder；
The carbon fibre includes at least one of carbon fiber, carbon nanotube, graphene；
The metal oxide includes at least one of zirconium oxide, magnesia, aluminium oxide, titanium oxide.
2. the slurry of porous ceramics scaffold according to claim 1, it is characterised in that silicate powder and reinforced phase powder
It is mixed to form composite ceramic material in proportion, composite ceramic material and adhesive solution are mixed to form composite ceramics slurry in proportion
Material.
3. composite ceramic material according to claim 2, feature includes that silicate quality accounting in composite granule is
70%~95%, reinforced phase quality accounting is 5%~30%.
4. adhesive solution according to claim 2, it is characterised in that by polyvinyl alcohol, carboxymethyl cellulose, Pu Langni
At least one of gram F-127, which is dissolved into solvent, forms adhesive solution, and the mass fraction of adhesive solution be 10%~
40%.
5. composite ceramics slurry according to claim 2, it is characterised in that the matter of composite ceramic material and adhesive solution
Amount is than being 4: 3~3: 1.
6. a kind of extrusion deposits ceramic shaping method, feature includes: that any one provided in Claims 1 to 5 is prepared again
Close ceramic slurry；The three-dimensional entity model of porous ceramics scaffold to be printed is designed and generated, determines printing thickness and print speed
And slicing delamination, planning path are carried out to model；Extruded velocity is set or squeezes out pressure, squeezes out and deposits above-mentioned composite ceramics slurry
Material forms porous silicate ceramics bracket idiosome, idiosome is heat-treated to obtain porous ceramics scaffold finished product.
7. a kind of extrusion according to claim 6 deposits ceramic shaping method, it is characterised in that through prepared by this method
The porosity of porous ceramics scaffold finished product is 50%~75%, and pore size is 100~500um.
8. a kind of extrusion according to claim 6 deposits ceramic shaping method, it is characterised in that printing thickness is generally 0.1
~0.4mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110357592A (en) * | 2019-08-05 | 2019-10-22 | 吴振行 | A kind of ceramic resin of 3D printing and its preparation method and application |
| WO2022174507A1 (en) * | 2021-02-19 | 2022-08-25 | 南京航空航天大学 | Method for preparing calcium silicate/magnesium oxide porous biological bone scaffold based on in-situ method |
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| CN103656752A (en) * | 2012-09-25 | 2014-03-26 | 中南大学 | Method for strengthening and toughening biological ceramic material by use of graphene and preparing artificial bone prepared from material |
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