CN105196398B - For the ceramic slurry of air pressure extruded type 3 D-printing and the preparation method of bioceramic scaffold - Google Patents
For the ceramic slurry of air pressure extruded type 3 D-printing and the preparation method of bioceramic scaffold Download PDFInfo
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- CN105196398B CN105196398B CN201510591180.XA CN201510591180A CN105196398B CN 105196398 B CN105196398 B CN 105196398B CN 201510591180 A CN201510591180 A CN 201510591180A CN 105196398 B CN105196398 B CN 105196398B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28C—PREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28C5/00—Apparatus or methods for producing mixtures of cement with other substances, e.g. slurries, mortars, porous or fibrous compositions
- B28C5/003—Methods for mixing
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
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Abstract
The invention discloses the preparation method of the ceramic slurry for air pressure extruded type 3 D-printing, comprise the following steps：(11) bioactive ceramics powder is added in a solvent, and using planetary ball mill 3~12h of ball milling, the solid concentration of obtained slurry is 35~55vol%；(12) water-soluble auxiliary rheological agents are added in the slurry obtained to step (1), use 0.5~3h of planetary ball mill ball milling mixing, then slurry is moved into barrel, carries out ultrasonic vibration, low temperature de-bubble successively, obtain the ceramic slurry for air pressure extruded type 3 D-printing.The invention also discloses the preparation method that bioactive ceramics support is prepared using air pressure extruded type 3 D-printing forming technique.The ceramic slurry of the present invention have high solid loading, good print performance and solidifiability, available 100% connective, contour structures of the bioactive ceramics support of preparation and inside dimension it is controllable.
Description
Technical field
It is more particularly to a kind of for air pressure extruded type 3 D-printing the present invention relates to the preparation of the material of rapid shaping technique
The preparation method of ceramic slurry and bioceramic scaffold.
Background technology
Existing Bone Defect Repari technology mainly includes autologous and allogenic bone transplantation technology：Autologous bone contain Gegenbaur's cell living and
BMP with induced osteogenesis effect, and be clinical bone defect healing " gold " standard without immunological rejection, but
Limited source, it is impossible to be used in the treatment of big segmental defects；Homogeneous allogenic bone transplantation have biological characteristics and morphosis with
The advantages of autologous bone is similar, but homogeneous allogenic bone limited source, and immunological rejection easily occurs, have and propagate some diseases
It is dangerous.
In order to solve the reparation problem of tissue and organ defect, the Chemical Engineer of Massachusetts Institute Technology
The R.Langer and doctor J.P.Vacanti of medical college of Harvard University the 1980s mid-term propose organizational project
(Tissue engineering) this concept.Bone tissue engineer is exactly principle and the method regeneration of utilizing works and life science
New bone tissue, it is the future for realizing Bone Defect Repari to repair and substitute lesion or defect bone tissue or the technology for promoting its function
Developing direction.Timbering material in bone tissue engineer is as the extracellular matrix substitute of seed cell and the frame of regenerating tissues
Frame, its characteristic directly affect the biological characteristics of seed cell, influence cells survival, migration, propagation and functional metabolism, final shadow
Ring the success or failure of bone tissue structure.
With people to the continuous improvement and bioceramic of biomaterial quality and security requirement in medical rehabilitation system
In application, bioceramic, particularly bioactive ceramics turn into an important research field of material science and engineering in medicine.
The preparation method of porous tissue engineering scaffold is a lot, and such as foaming, Freeze Drying Technique, sintering process, but these methods are not only right
The profile of support, aperture size and pattern are uncontrollable, and can not realize the personalized customization of three-dimensional rack.3 D-printing is molded
Technology integrates material science, CAD, Numeric Control Technology, using " increasing material " manufacturing process, can accurately copy
With the body of organism same shape.Rapid shaping technique, which can build complete through hole, height rule, form and micro-structural, to be had
The support of repeatability, and macrostructure and the substantially identical three-dimensional structure of defective tissue can be designed.It is more ripe at present
3 D-printing material be resin and metal material, the 3 D-printing of ceramic material is difficult to.Patent CN 103707388A and
Patent CN 103992088A disclose the method that gypsum 3 D workpiece is prepared using powder bonding technique, and it has problem and is
The roughness of finished product is higher, and mechanical property is poor, and prepared porous support pore size is typically more than 500 microns.It is three-dimensional fine
Dimension deposition technique solves shortcoming present in powder bonding technology after being used for 3 D-printing, can prepare 100 microns of pore size
To 1 millimeter of porous support, it is expected to prepare the porous support materials closer to natural bony structure.Patent 201410840236.6
Ceramic shaping is carried out using electric motor boosted extruded type 3 D-printing formation system, but its organic additive addition reaches 30%,
The problem of ceramic firing post-shrinkage ratio is excessive, and accuracy to size is not high can be caused.
The content of the invention
In order to overcome the disadvantages mentioned above of prior art and deficiency, it is used for air pressure it is an object of the invention to provide one kind and extrudes
The ceramic slurry of formula 3 D-printing, have high solid loading, good print performance and solidifiability.
Another object of the present invention is to provide to use air pressure extruded type 3 D-printing forming technique to prepare bioactivity pottery
Porcelain support, the three-dimensional rack that available 100% is connective, contour structures and inside dimension are controllable, can solve clinically biological
Active ceramic bone repair can not personalized accurate the problem of customizing.
The purpose of the present invention is achieved through the following technical solutions：
For the preparation method of the ceramic slurry of air pressure extruded type 3 D-printing, comprise the following steps：
(11) bioactive ceramics powder is added in a solvent, using planetary ball mill using frequency as 20~30Hz ball millings 3
~12h, the solid concentration of obtained slurry is 35~55vol%；
The solvent is uniformly mixed by deionized water and dispersant；The addition of the dispersant is made pottery for bioactivity
The 0.5~2% of porcelain powder quality；
(12) water-soluble auxiliary rheological agents are added in the slurry obtained to step (11), using planetary ball mill using frequency as 20
~30Hz 0.5~3h of ball milling mixing, then slurry is moved into barrel, carry out ultrasonic vibration, low temperature de-bubble successively, be used for
The ceramic slurry of air pressure extruded type 3 D-printing；
The addition of the water-soluble auxiliary rheological agents is the 0.5~2.5% of ceramic powder quality；
The frequency of the ultrasonic vibration is 100Hz, and time 15-60min, temperature is 20~40 DEG C；
The low temperature de-bubble is in 2~10 DEG C of 3~48h of standing of temperature.
Dispersant described in step (11) is ammonium polyacrylate, Sodium Polyacrylate or stearic acid.
Step (12) water-soluble auxiliary rheological agents are xanthans, agarose, methylcellulose or polyvinyl alcohol.
Bioactive ceramics described in step (11) is hydroxyapatite, bata-tricalcium phosphate powder or bioactivity glass powder
Body.
The preparation method of bioceramic scaffold, prepared using air pressure extruded type 3 D-printing method, specifically include following steps：
(21) it is used for what the preparation method of the described ceramic slurry for air pressure extruded type 3 D-printing was prepared
The ceramic slurry of air pressure extruded type 3 D-printing is placed in barrel, selects syringe needle, and calibrate the height of syringe needle；
(22) size and form of the printer model of In-put design and edit model, is layered to model；
(23) set print parameters, slurry under the extruding of air pressure by 3 D-printing formed have different appearance and sizes and
The three-dimensional ceramic support base substrate of internal microstructure；
(24) the three-dimensional ceramic support body drying for obtaining step (23) printing；
(25) dried three-dimensional ceramic support base substrate is sintered into 1~5h at 1000~1200 DEG C.
Drying described in step (24), it is specially：
First 2~24h of air drying, then microwave drying, samples weighing is taken out every 4h, until front and rear quality no longer changes
Then dry complete.
Step (25) is described to sinter 1~5h at 1000~1200 DEG C, is specially：It is warming up to 2~5 DEG C/min speed
1000~1200 DEG C, 1~5h is incubated, room temperature is dropped to 2~6 DEG C/min speed.
Step (23) described print parameters include platform temperature, barrel temperature, atmospheric pressure, print speed.
The innovative three-dimensional fiber deposition technique using air pressure extruded type of the invention carries out the three-dimensional of porous ceramic film material
Printing shaping, the pressure for controlling compressed air by barograph extrude slurry, and precision is higher, but pressure highest only has 0.6MPa,
Therefore it is higher to the mobility of slurry and the requirement of curing performance.The present invention solves slurry on the basis of system research
Rheological property regulates and controls, the key technical problem such as solidifiability regulation and control, and controls quantity of organic compounds to be less than 3%, and it is low to burn till contraction
In 10%, the 3 D-printing shaping controllable precise manufacture of bioceramic material is realized.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) slurry that the present invention is prepared has good mobility, conformality and solidifiability.Air pressure is applicable to squeeze
Go out formula fiber deposition 3D printing system (3D-BioplotterTMSystem or 3D-BioprinterTMSystem), printing precision reaches
0.001mm, it is much higher than traditional electric motor boosted 3D printing system.
(2) powder used in the present invention is bioactive ceramics powder, has good biocompatibility, addition has
Machine reagent is nontoxic, nuisanceless, there was only bioactive ceramics phase in three-dimensional rack after high temperature sintering, avoids organic additive pair
The influence of support bioactivity.
(3) the organic additive total amount of slurry prepared by the present invention is less than 3wt%, and the contraction of burning till of sample can be controlled to be less than
10%, substantially increase the dimensional accuracy of material.
Brief description of the drawings
Fig. 1 is the rheological property and viscosity of slurry in embodiments of the invention 1.
Fig. 2 (a) is the three-dimensional microphoto of the top view of three-dimensional rack in embodiments of the invention 1.
Fig. 2 (b) is the three-dimensional microphoto of the side view of three-dimensional rack in embodiments of the invention 1.
Fig. 2 (c) is the three-dimensional microphoto of the sectional drawing of three-dimensional rack in embodiments of the invention 1.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
Step 1：The preparation of high solid loading slurry
(1) micro/nano level synthesized with soluble calcium salt and phosphate reaction technique spherical bata-tricalcium phosphate (β-
TCP) powder is raw material, using the mixed liquor of deionized water and ammonium polyacrylate as solvent, uses planetary ball mill ball milling 8h (frequencies
30Hz), the slurry that solid concentration is 45vol% is prepared, its rheological property and viscosity are shown in Fig. 1；
(2) methylcellulose that high polymerization degree is added into slurry is auxiliary rheological agents, and addition is β-TCP powders
1wt%, using planetary ball mill high speed ball milling mixing 2h, then slurry is moved into barrel.Pass through ultrasonic vibration (frequency
100Hz, time 30min, 30 DEG C of temperature), the mode of low temperature de-bubble (time 12h, 4 DEG C of temperature), preparation can be used for three-dimensional beat
The bioactive ceramics slurry of type is printed as, the viscosity of slurry is less than 100PaS, and aerial setting time is less than 1 minute.
Step 2：The preparation of three-dimensional controllable microstructure bioceramic scaffold base substrate
(1) slurry prepared in step 1 is placed in shower nozzle, selects a diameter of 0.41mm TT inclined syringe needles, and calibrate pin
The height of head；
(2) the printer model cuboid of In-put design, and the size of edit model is 20*20*5mm, and model is divided
Layer；
(3) set platform temperature be 37 DEG C, barrel temperature be room temperature, air pressure 0.23MPa, print speed 6mm/s, make
Slurry deposits to be formed with three-dimensional ceramic support under the extruding of air pressure by three-dimensional fiber.
Step 3：The later stage of support is dry and sinters
(1) the support elder generation air drying 4h that will be printed in step 2, then take out sample every 4h after microwave drying 24h and claim
Weight, then dried completely until front and rear quality no longer changes；
(2) 1400 DEG C of high temperature furnaces are used, the sintering temperature of support is 1120 DEG C, soaking time 3h, heating rate 3
DEG C/min, rate of temperature fall is 3 DEG C/min, finally gives the bioactive ceramics three that with higher-strength, shrinkage factor is 5.7%
Dimensional scaffold.
Fig. 1 is the viscosity and rheological characteristic that slurry during auxiliary rheological agents is not added with this implementation.As can be seen that with shear rate
Increase, the viscosity of slurry is 0PaS, illustrates that its mobility is fabulous.
The three-dimensional micro- photograph of the top view of bioactive ceramics three-dimensional rack manufactured in the present embodiment, side view and sectional drawing
Shown in piece such as Fig. 2 (a)~(c).As seen from the figure, three-dimensional rack aperture rule ordered arrangement manufactured in the present embodiment, and be distributed equal
Even, both horizontally and vertically hole connectedness is up to 100%.
Embodiment 2
Step 1：The preparation of high solid loading slurry
(1) ball shaped hydroxy-apatite (HA) powder of the micro/nano level synthesized with soluble calcium salt and phosphate reaction technique
For raw material, using the mixed liquor of deionized water and Sodium Polyacrylate as solvent, using planetary ball mill ball milling 8h (frequency 30Hz), match somebody with somebody
Solid concentration processed is 50vol% slurry；
(2) it is auxiliary rheological agents low melting-point agarose to be added into slurry, and addition is the 2.5wt% of HA powders, uses row
Celestial body grinding machine high speed ball milling mixing 1h, then slurry is moved into barrel.By ultrasonic vibration (frequency 100Hz, time 30min,
30 DEG C of temperature), the mode of stand at low temperature (time 12h, 4 DEG C of temperature), prepare can be used for 3 D-printing shaping bioactivity
Ceramic slurry, the viscosity of slurry are less than 100PaS, and aerial setting time is less than 1 minute.
Step 2：The preparation of three-dimensional controllable microstructure bioceramic scaffold base substrate
(1) slurry prepared in step 1 is placed in shower nozzle, selects a diameter of 0.21mm TT inclined syringe needles, and calibrate pin
The height of head；
(2) the printer model cuboid of In-put design, and the size of edit model is 20*20*5mm, and model is divided
Layer；
(3) setting platform temperature is 0 DEG C, barrel temperature is 30 DEG C, air pressure 0.30MPa, print speed 13mm/s, is made
Slurry deposits to be formed with three-dimensional ceramic support under the extruding of air pressure by three-dimensional fiber.
Step 3：The later stage of support is dry and sinters
(1) the support elder generation air drying 4h that will be printed in step 2, then take out sample every 4h after microwave drying 24h and claim
Weight, then dried completely until front and rear quality no longer changes；
(2) 1400 DEG C of high temperature furnaces are used, the sintering temperature of support is 1200 DEG C, soaking time 3h, heating rate 3
DEG C/min, rate of temperature fall is 3 DEG C/min, and it is three-dimensional to finally give the bioactive ceramics that with higher-strength, shrinkage factor is 4%
Support.
Embodiment 3
Step 1：The preparation of high solid loading slurry
(1) using nanometer level bioactive glass (BG) powder of sol-gel process synthesis as raw material, with deionized water and firmly
The mixed liquor of resin acid is solvent, using planetary ball mill ball milling 3h (frequency 30Hz), prepares the slurry that solid concentration is 40vol%
Material；
(2) xanthans that high polymerization degree is added into slurry is auxiliary rheological agents, and addition is the 2wt% of powder, uses row
Celestial body grinding machine high speed ball milling mixing 1h, then slurry is moved into barrel.By ultrasonic vibration (frequency 100Hz, time 30min,
30 DEG C of temperature), the mode of stand at low temperature (time 12h, 2 DEG C of temperature), prepare for 3 D-printing shaping bioactive ceramics
Slurry；The viscosity of slurry is less than 100PaS, and aerial setting time is less than 1 minute.
Step 2：The preparation of three-dimensional controllable microstructure bioceramic scaffold base substrate
(1) slurry prepared in step 1 is placed in shower nozzle, selects a diameter of 0.25mm TT inclined syringe needles, and calibrate pin
The height of head；
(2) the printer model cuboid of In-put design, and the size of edit model is 20*20*5mm, and model is divided
Layer；
(3) setting platform temperature is 0 DEG C, barrel temperature is 50 DEG C, air pressure 0.17MPa, print speed 5mm/s, is made
Slurry deposits to be formed with three-dimensional ceramic support under the extruding of air pressure by three-dimensional fiber.
Step 3：The later stage of support is dry and sinters
(1) the support elder generation air drying 4h that will be printed in step 2, then take out sample every 4h after microwave drying 24h and claim
Weight, then dried completely until front and rear quality no longer changes；
(2) 1400 DEG C of high temperature furnaces are used, the sintering temperature of support is 1000 DEG C, soaking time 3h, heating rate 3
DEG C/min, rate of temperature fall is 3 DEG C/min, finally gives the bioactive ceramics three that with higher-strength, shrinkage factor is 10%
Dimensional scaffold.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of bioceramic scaffold, it is characterised in that prepared using air pressure extruded type 3 D-printing method, specifically
Comprise the following steps：
(11) in a solvent add bioactive ceramics powder, using planetary ball mill using frequency as 20~30Hz ball millings 3~
12h, the solid concentration of obtained slurry is 35~55vol%；
The solvent is uniformly mixed by deionized water and dispersant；The addition of the dispersant is bioactive ceramics powder
The 0.5~2% of weight；
(12) water-soluble auxiliary rheological agents are added in the slurry obtained to step (11), using planetary ball mill using frequency as 20~
30Hz 0.5~3h of ball milling mixing, then slurry is moved into barrel, carry out ultrasonic vibration, low temperature de-bubble successively, obtain being used for gas
Press the ceramic slurry of extruded type 3 D-printing；
Described bioactive ceramics is hydroxyapatite, bata-tricalcium phosphate powder or bioactive glass powder；
The addition of the water-soluble auxiliary rheological agents is the 0.5~2.5% of ceramic powder quality；
The frequency of the ultrasonic vibration is 100Hz, and time 15-60min, temperature is 20~40 DEG C；
The low temperature de-bubble is in 2~10 DEG C of 3~48h of standing of temperature；
(21) ceramic slurry for air pressure extruded type 3 D-printing being prepared is placed in barrel, selects syringe needle, and calibrate
The height of syringe needle；
(22) size and form of the printer model of In-put design and edit model, is layered to model；
(23) print parameters are set, slurry is formed under the extruding of air pressure by 3 D-printing has different appearance and sizes and inside
The three-dimensional ceramic support base substrate of micro-structural；
(24) the three-dimensional ceramic support body drying for obtaining step (23) printing；
(25) dried three-dimensional ceramic support base substrate is sintered into 1~5h at 1000~1200 DEG C.
2. the preparation method of bioceramic scaffold according to claim 1, it is characterised in that scattered described in step (11)
Agent is ammonium polyacrylate, Sodium Polyacrylate or stearic acid.
3. the preparation method of bioceramic scaffold according to claim 1, it is characterised in that step (12) water-soluble rheology
Auxiliary agent is xanthans, agarose, methylcellulose or polyvinyl alcohol.
4. the preparation method of bioceramic scaffold according to claim 1, it is characterised in that dry described in step (24)
It is dry, be specially：
First 2~24h of air drying, then microwave drying, samples weighing is taken out every 4h, until front and rear quality no longer changes, done
It is dry complete.
5. the preparation method of bioceramic scaffold according to claim 1, it is characterised in that step (25) is described 1000
~1200 DEG C of 1~5h of sintering, it is specially：1000~1200 DEG C are warming up to 2~5 DEG C/min speed, are incubated 1~5h, with 2~
6 DEG C/min speed drops to room temperature.
6. the preparation method of bioceramic scaffold according to claim 1, it is characterised in that step (23) the printing ginseng
Number includes platform temperature, barrel temperature, atmospheric pressure, print speed.
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| CN1505495A (en) * | 2001-02-23 | 2004-06-16 | 史密夫和内修有限公司 | Manufacture of bone graft substitutes |
| CN103948456A (en) * | 2014-04-22 | 2014-07-30 | 上海大学 | Automatic control turntable pneumatic multi-sprayer biological 3D (three dimensional) printing forming system and method |
| CN104478463A (en) * | 2014-11-21 | 2015-04-01 | 大连理工大学 | Preparation method of laminar porous hydroxyapatite ceramic |
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2015
- 2015-09-16 CN CN201510591180.XA patent/CN105196398B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1505495A (en) * | 2001-02-23 | 2004-06-16 | 史密夫和内修有限公司 | Manufacture of bone graft substitutes |
| CN103948456A (en) * | 2014-04-22 | 2014-07-30 | 上海大学 | Automatic control turntable pneumatic multi-sprayer biological 3D (three dimensional) printing forming system and method |
| CN104478463A (en) * | 2014-11-21 | 2015-04-01 | 大连理工大学 | Preparation method of laminar porous hydroxyapatite ceramic |
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Effective date of registration: 20230413 Address after: Room 503, Building B, No. 190 Banhe Road, Huangpu District, Guangzhou City, Guangdong Province, 510535 Patentee after: Guangzhou Kangrui Medical Equipment Co.,Ltd. Address before: 510640 No. five, 381 mountain road, Guangzhou, Guangdong, Tianhe District Patentee before: SOUTH CHINA University OF TECHNOLOGY |