CN106426506B - A kind of manufacturing method of bioceramic green body - Google Patents
A kind of manufacturing method of bioceramic green body Download PDFInfo
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- CN106426506B CN106426506B CN201610817340.2A CN201610817340A CN106426506B CN 106426506 B CN106426506 B CN 106426506B CN 201610817340 A CN201610817340 A CN 201610817340A CN 106426506 B CN106426506 B CN 106426506B
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- green body
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- bioceramic
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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
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/007—Producing shaped prefabricated articles from the material by freezing the material
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped 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 aluminium oxide
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped 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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a kind of manufacturing methods of bioceramic green body, including at low ambient temperatures, are laid with one layer of slurry on print platform by scraping blade, so that the slurry of laying is quickly solidified using freezing plate；The irradiation for carrying out selectivity to the slurry that this layer solidifies according to the contour path data obtained in step S1 using Laser Scanning Equipment, removes the binder in slurry at profile, then adjusts the height of print platform and reduces by one layer；By accumulating layer by layer, the solidification state green body for being solidified slurry encirclement is made；Then solidification state green body is placed in freeze drier after being dried and can be obtained target green body by the solidification slurry outside removal solidification state green body.Said program, available multistage pore structure have many advantages, such as that feed preparation process is simple, material has wide range of applications, process is not necessarily to mold, are not necessarily to design support, are high in machining efficiency, at low cost.
Description
Technical field
The present invention relates to bioceramic material production fields, and in particular to a kind of manufacturing method of bioceramic green body.
Background technology
With the development of Digital Design ＆ Manufacturing Technologies and bioceramic material, the application of bone repair body is increasingly wide
It is general.Skeleton is complex-shaped, and tooth is with more irregular shapes such as thin slice feature and sharp features.Using traditional calculating
Machine digital control processing bone repair body, the development cost of process equipment is high, with a large amount of waste of material in milling process, is not inconsistent
Close the requirement of green manufacturing.Skeleton is made of cancellous bone and compact bone.Cancellous bone is in loose spongy, by bone trabecula phase
It connects to be formed, porosity 30%-90%；Compact bone is relatively closely knit, porosity 5%-30%.Skeleton existing 1~
10 μm of micropore has 100~800 μm of macropore again, belongs to multistage pore structure.To improve the bio-compatibility of bone repair body,
Promote growing into for tissue, dummy that there should be multistage pore structure.
The traditional handicraft for preparing porous ceramics has addition pore creating material method, Polymeric sponge method, foaming, extrusion forming
Method, granulation mass area method etc..These common methods can prepare that porosity is higher, the porous ceramics of uniform pore diameter distribution, but
The multistage pore structure prepared similar to natural bony structure also has certain difficulty.
The principle of freeze-drying is then the distillation of solvent ice is removed to the solvent freezing in slurry under lower pressure
It goes, remaining material is left in place, and is ultimately formed and the identical porous microstructure of ice crystal structure.Since the growth of ice crystal is in tree
Dendritic, there are larger branch and smaller branch, the green compact formed after dry have multistage pore structure.It is dry using freezing
The dry multistage pore structure of technology processing, traditional method are freezing cast.When freezing casting processing 3 d part, need in advance
Corresponding mold is processed, is freeze-dried in slurry injection mold, after demoulding, obtains target green body.Bone repair body
Shape is extremely complex, and there are larger differences between individual, processes bone repair body using freezing casting, need to be each patient
Complicated die customized, and mold is disposable, cost is high.Time-consuming for freezing dry process, wherein being consumed with drying process
When longest, and drying time be multiplied with the increase of material thickness.
3D printing technique is the important branch of high-new processing technology, and process is not necessarily to cutter, mold and fixture, relative to
Traditional subtraction manufacture, has a clear superiority, and greatly reduce the material in process in manufacturing complex shapes product
Waste.Skeleton dummy is processed using 3D printing technique, has the advantages that efficient, at low cost, waste is few.
The 3D printing method of bioceramic green body is divided into based on powder according to the difference of materials behavior and is based on slurry two
Kind.Bioceramic particle adhesion is made its forming, this method difficult by the 3D printing method based on powder together using binder
To control the pore structure of green body.3D printing method based on slurry, mainly by evaporate solvent method make slurry curing at
Shape, there are gas-liquid interfaces to keep pore structure uncontrollable due to the effect of tension for the process of evaporation of the solvent.3D based on slurry is beaten
Impression method further includes stereolithography apparatus method (SLA), and this method equipment and material cost are higher.
Patent No. CN104108131A discloses a kind of 3D printing forming method of ceramic material and will be starched according to print routine
Expect it is spouting, by freezing so that green body is shaped, finally using be freeze-dried or normal drying by the way of green body is dried
Processing.This technology is limited by its spray technology, the narrow application range of slurry solid content.
Invention content
It is an object of the invention to provide a kind of manufacturing methods of bioceramic green body, can effectively solve the above problems,
The production efficiency of bioceramic green body is high, at low cost, easy to operate.
To achieve the above object, present invention employs following technical schemes：
A kind of manufacturing method of bioceramic green body, including following operating procedure：
S1：The threedimensional model for establishing target green body carries out layered shaping to threedimensional model, obtains every layer of contour path number
According to；Preparing has the slurry of freeze-drying characteristic；
S2：At low ambient temperatures, one layer of slurry is laid on print platform by scraping blade, the slurry of laying is made using freezing plate
Material quickly solidification；The slurry that this layer solidifies is carried out according to the contour path data obtained in step S1 using Laser Scanning Equipment
The irradiation of selectivity removes the binder in slurry at profile, then adjusts the height of print platform and reduces by one layer；
S3：Step S2 is repeated, by accumulating layer by layer, the solidification state green body for being solidified slurry encirclement is made；Removal solidification state
Then solidification state green body is placed in freeze drier after being dried and can be obtained target base by the solidification slurry outside green body
Body.
Specific scheme is that low temperature environment refers to temperature in step S2<- 0 DEG C of environment, preferably<- 20 DEG C of environment；Step
Laser Scanning Equipment is the bis- coordinate Laser Scanning Equipments of X-Y in rapid S3, and optical maser wavelength is 10.6 μm when irradiation, laser power 1
~100W, laser scanning speed are 10~100mm/s.The environment of drying process is environment under low pressure.
The preparation of slurry is the key that realize the present invention, and slurry component includes the bioceramic powder of 5~90 parts by weight, 1
The bonding agent of~30 parts by weight, remaining be solvent.In addition, the additives such as alternative addition dispersant, antifreeze.
Water, amphene can be used in solvent, preferably selects water.
Bonding agent uses water-soluble organic adhesive, and carboxymethyl cellulose, polyvinyl alcohol, acrylic acid, epoxy can be selected
One or more of resin, polyurethane.
Bioceramic powder can be bio-inert ceramic, bioactive ceramics, preferably select aluminium oxide ceramics, zirconium oxide pottery
One or more of porcelain, hydroxylapatite ceramic, calcium phosphate ceramics.
The technical solution of above-mentioned offer compared with the existing technology, has the following advantages that：
1, the characteristic of solid particle fixation in situ in slurry can be made using freeze-drying, can get multistage pore structure, it is former
Expect that preparation process is simple, material has wide range of applications, as long as uniform sizing material can be configured to, has expanded answering for 3D printing technique
Use field；
2, by the way of successively stone, without designing material ejection or extrusion device, the suitable of slurry solid content is expanded
With range, cost is reduced；
3, by the way of successively freezing, lower layer provides solid support for upper layer, reduces the deformation of cantilever design, without for
Cantilever design design support.
In short, technical solution provided by the invention, can get multistage pore structure, the simple, material with feed preparation process
The advantages that material has wide range of applications, process supports without mold, without design, is high in machining efficiency, at low cost.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific implementation mode
In order to make objects and advantages of the present invention be more clearly understood, the present invention is carried out specifically with reference to embodiments
It is bright.It should be appreciated that following word is only used to one or more of specific embodiments of the description present invention, not to the present invention
The protection domain specifically asked carries out considered critical.
Embodiment 1
Using following operation preparation bioceramic green body：
1) design softwares such as Pro/E, UG or spatial digitizer is used to establish the STL format models of target green body；
2) computer software is used to carry out the layered shaping along short transverse to built threedimensional model, every layer of thickness is
0.1~1mm；Establish the contour path data of each layer；
3) slurry is prepared：Weigh 100g alumina powders (analysis is pure, crosses 325 mesh)；Weigh 10g polyvinyl alcohol；Measure distillation
Water 100ml.Above-mentioned raw materials are added in corundum ball grinder and carry out high speed ball milling 2h；
4) slurry after ball milling is placed in de-bubble 10min in froth in vacuum machine；
5) Laser Scanning Equipment and laying device are added in the environment of temperature-controllable, Laser Scanning Equipment is sat by X-Y is bis-
Mark workbench and CO2Laser constitution.Barrel is added in slurry after de-bubble, keeps, to slurry agitation, avoiding slurry in barrel
Sedimentation；Keep environment temperature at -20 DEG C or less.One layer of slurry is laid on by scraping blade on print platform, thickness and computer
Thickness when layered shaping is identical；Slurry 30s is covered using the aluminum freezing plate of internal circulating liquid nitrogen from top to bottom, keeps slurry fast
Speed, fully freezing；
6) freezing plate to be removed, laser is opened, laser power is 1~100W, and laser scanning speed is 10~100mm/s,
The bis- coordinate setting tables of X-Y solidify slurry selectivity spoke according to the contour path data control laser established in step 2) to the layer
According to removal contour area binder；
7) laser is closed；
8) it repeats step 5) and arrives step 7), until printing completion, the curdled appearance green body for being solidified slurry encirclement is made；
9) removal is external solidifies slurry, obtains the target green body of curdled appearance；
10) the target green body of curdled appearance is dried in freeze drier, obtains target green body.
Embodiment 2
The oxygen that the ceramic powder that the present embodiment uses as different from Example 1, in step 3) is stablized for Yttrium oxide doping
Change zircon ceramic powder, binder is carboxymethyl cellulose.
Embodiment 3
As different from Example 1, step 5) uses the copper freezing plate of internal circulating liquid nitrogen from top to bottom to the present embodiment
Slurry 10s is covered, the more tiny green body of pore structure is obtained.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, after knowing content described in the present invention, without departing from the principle of the present invention, it can also be made several
Same transformation and replacement, these convert and substitute on an equal basis and also should be regarded as belonging to the scope of protection of the present invention.
Claims (10)
1. a kind of manufacturing method of bioceramic green body, including following operating procedure：
S1：The threedimensional model for establishing target green body carries out layered shaping to threedimensional model, obtains every layer of contour path data；Match
Fixture has the slurry of freeze-drying characteristic；
S2：At low ambient temperatures, one layer of slurry is laid on print platform by scraping blade, keeps the slurry of laying fast using freezing plate
Rapid hardening is solid；The slurry solidified to this layer according to the contour path data obtained in step S1 using Laser Scanning Equipment is selected
Property irradiation, remove the binder in slurry at profile, then adjusting the height of print platform reduces by one layer；
S3：Step S2 is repeated, by accumulating layer by layer, the solidification state green body for being solidified slurry encirclement is made；Removal solidification state green body
Then solidification state green body is placed in freeze drier after being dried and can be obtained target green body by external solidification slurry.
2. the manufacturing method of bioceramic green body according to claim 1, it is characterised in that：With freeze-drying characteristic
Slurry component include the bioceramic powder of 5~90 parts by weight, 1~30 parts by weight bonding agent, remaining be solvent.
3. the manufacturing method of bioceramic green body according to claim 2, it is characterised in that：Bonding agent has to be water-soluble
Machine bonding agent.
4. the manufacturing method of bioceramic green body according to claim 1 or 2, it is characterised in that：It is special with freeze-drying
The slurry component of property further includes dispersant, antifreeze.
5. the manufacturing method of bioceramic green body according to claim 2, it is characterised in that：Solvent is water.
6. the manufacturing method of bioceramic green body according to claim 3, it is characterised in that：Water-soluble organic adhesive
For one or more of carboxymethyl cellulose, polyvinyl alcohol, acrylic acid, epoxy resin, polyurethane.
7. the manufacturing method of bioceramic green body according to claim 3, it is characterised in that：Bioceramic powder is oxidation
One or more of aluminium ceramics, zirconia ceramics, hydroxylapatite ceramic, calcium phosphate ceramics.
8. the manufacturing method of bioceramic green body according to claim 3, it is characterised in that：Low temperature environment is in step S2
Refer to temperature<- 0 DEG C of environment.
9. the manufacturing method of bioceramic green body according to claim 3, it is characterised in that：Laser scanning is set in step S3
Standby is the bis- coordinate Laser Scanning Equipments of X-Y, and optical maser wavelength is 10.6 μm when irradiation, and laser power is 1~100W, and laser scanning is fast
Degree is 10~100mm/s.
10. the manufacturing method of bioceramic green body according to claim 8, it is characterised in that：Low temperature environment in step S2
It refer to temperature<- 20 DEG C of environment.
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| CN201610817340.2A CN106426506B (en) | 2016-09-12 | 2016-09-12 | A kind of manufacturing method of bioceramic green body |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108621289B (en) * | 2017-03-23 | 2019-12-24 | 苏日华 | Method for making ceramic handicraft |
| CN106978559B (en) * | 2017-04-26 | 2018-07-03 | 西安工程大学 | A kind of method of 3D printing manufacture air-texturing jet |
| CN107584631A (en) * | 2017-10-25 | 2018-01-16 | 西安工业大学 | A kind of 3D printing method of ceramic body |
| CN109485430B (en) * | 2018-11-30 | 2021-09-07 | 中南大学 | Method for preparing bionic porous ceramic with complex three-dimensional structure |
| CN109400200B (en) * | 2018-11-30 | 2022-01-04 | 中南大学 | Hydroxyapatite porous ceramic with controllable macro and micro structures and preparation method and application thereof |
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| CN1351927A (en) * | 2001-12-14 | 2002-06-05 | 清华大学 | Process of computer-aided mould-free forming ceramic part blank |
| JP2007152342A (en) * | 2005-11-10 | 2007-06-21 | Ngk Insulators Ltd | Manufacturing method of honeycomb structure |
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| CN103980681A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | 3D printing high-molecular-weight polylactic acid porous materials manufactured by low-temperature deposition and preparation method thereof |
| CN104108131A (en) * | 2014-07-04 | 2014-10-22 | 航天特种材料及工艺技术研究所 | 3D printing forming method for ceramic materials |
| CN104908318A (en) * | 2014-03-12 | 2015-09-16 | 精工爱普生株式会社 | Manufacturing method of three-dimensional structure, three-dimensional structure manufacturing apparatus, and three-dimensional structure |
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2016
- 2016-09-12 CN CN201610817340.2A patent/CN106426506B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351927A (en) * | 2001-12-14 | 2002-06-05 | 清华大学 | Process of computer-aided mould-free forming ceramic part blank |
| JP2007152342A (en) * | 2005-11-10 | 2007-06-21 | Ngk Insulators Ltd | Manufacturing method of honeycomb structure |
| CN103057123A (en) * | 2013-01-23 | 2013-04-24 | 南通大学 | Three-dimensional organism printing system and method for preparing nerve regeneration implant based on three-dimensional organism printing system |
| CN104908318A (en) * | 2014-03-12 | 2015-09-16 | 精工爱普生株式会社 | Manufacturing method of three-dimensional structure, three-dimensional structure manufacturing apparatus, and three-dimensional structure |
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