CN109180168A - A kind of preparation method of high-strength ceramic biology 3D printing material - Google Patents
A kind of preparation method of high-strength ceramic biology 3D printing material Download PDFInfo
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- 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
- C04B35/14—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 silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/448—Sulphates or sulphites
Abstract
The invention discloses a kind of preparation method of high-strength ceramic biology 3D printing material, which passes through high speed ball milling for raw materials such as aluminium oxide, silica, diatom ooze, montmorillonite, graphite, hydroxylamine hydrochloride, magnesium sulfate, polyphenylene sulfide, epoxidized soybean oils respectively, sieving sorts, vacuum nitrogen is catalyzed reaction, vacuum filtration, wash repeatedly, drying, sonic oscillation disperses, high-strength ceramic biology 3D printing material is prepared in cryospray drying and other steps.The high-strength ceramic biology 3D printing material being prepared, cost of material is low, compression strength with higher and biocompatibility, is suitable for the application of a variety of Medical racks, artificial skelecton etc..
Description
Technical field
The present invention relates to this technical fields of 3D printing material, are related specifically to a kind of high-strength ceramic biology 3D printing material
The preparation method of material.
Background technique
3D printing material is the important material base of 3D printing technique development, and to a certain extent, the development of material determines
3D printing can have wider application.Currently, 3D printing material mainly includes engineering plastics, photosensitive resin, rubber material
Material, metal material and ceramic material etc..Ceramic material have high intensity, high rigidity, high temperature resistant, low-density, chemical stability it is good,
The excellent characteristics such as corrosion-resistant have a wide range of applications in industries such as aerospace, automobile, biologies.But since ceramic material is hard
It is particularly difficult that crisp feature shapes it, and especially complicated ceramic component need to be shaped by mold, mold processing cost
Height, development cycle are long, it is difficult to meet the needs of product continuous renewal.The ceramic powders of 3D printing are ceramic powder and certain gluing
Mixture composed by agent powder.Since the fusing point of adhesive powder is low, when laser sintered only by adhesive powder fusing and
Make ceramic powders bonding together, needs for be put into temperature controlling stove ceramic, be post-processed at a higher temperature.Ceramics
The proportion of powder and adhesive powder, mixability influence whether the performance of ceramic component.Binder ratio is higher, and sintering is compared
It is easy, but components contraction is bigger in last handling process, will affect the dimensional accuracy of component.Conversely, adhesive dosage is few,
Easy-sintering is not allowed then.The method of traditional regeneration and injury repair includes autotransplantation, heteroplastic transplantation and artificial synthesized production
3 approach of substitution of product.However the problems such as limited source, immunological rejection, poor biocompatibility, significantly limits these sides
The application of method, it is difficult to be really achieved and repair or the effect tissue engineering technique that substitutes for a long time occurs in due course, to regeneration with
Reparation brings new life.The common Method of Tissue Engineering principle based on biomaterial scaffolds is to make mould first in vitro
The porous support of imitative histoorgan shape and structure, then in conjunction with seed cell formed compound implant further proliferation,
Differentiation.Wherein, the production of porous tissue engineering scaffold is a vital step.Scaffold for tissue engineering is a kind of porous
Three-dimensional structure, it requires the cellular structure for having suitable pore-size to be connected to height, enough and continuous to provide cell
Channel is grown, while also ensuring the bracket that the circulation of moisture, inorganic salts, nutriment and discharged waste has much developed
Preparation method has solution casting/particle leaching method, gas foaming method, fibrage method etc., but the common issue of these methods is
It is difficult to the shape to brace aperture, size, connection form, spatial distribution etc. effectively accurately to be controlled, is not able to satisfy tissue
Engineering cannot be such that different cells are accurately positioned in the space structure of bracket etc. the requirement of the labyrinth of bracket.3D printing skill
The high flexibility and customizability of art are able to solve the above problem just, and file printing simultaneously can be by various growths
The factor, protein or even mixing with cells are into supporting structure.Therefore, 3D printing is in tissue engineering technique especially organizational project
It is constructed with bracket and embodies unrivaled advantage.At present, 3D printing technique is applied to organizational project regeneration/reparation group
It knits comprising bone, cartilage, nerve, muscle, blood vessel etc., and has been achieved for ideal research achievement, to clinical application exhibition
Reveal great potentiality.
Summary of the invention
In order to solve the above-mentioned technical problem, the invention discloses a kind of preparation sides of high-strength ceramic biology 3D printing material
Method, the technique are big by aluminium oxide, silica, diatom ooze, montmorillonite, graphite, hydroxylamine hydrochloride, magnesium sulfate, polyphenylene sulfide, epoxy
The raw materials such as soya-bean oil pass through respectively high speed ball milling, sieving sorting, vacuum nitrogen catalysis reaction, vacuum filtration, wash repeatedly, be dry,
High-strength ceramic biology 3D printing material is prepared in sonic oscillation dispersion, cryospray drying and other steps.The height being prepared
Strength ceramic biology 3D printing material, cost of material is low, compression strength with higher and biocompatibility, is suitable for a variety of
The application of Medical rack, artificial skelecton etc..
Technical solution: to solve the above-mentioned problems, the invention discloses a kind of high-strength ceramic biology 3D printing materials
Preparation method, comprising the following steps:
(1) by 5-10 parts of aluminium oxide, 6-10 parts of silica, 1-3 parts of diatom ooze, -5 parts of montmorillonite 2,1-3 parts of graphite, hydrochloric acid hydroxyl
It 1-4 parts of amine, is added in high speed ball mill, ratio of grinding media to material 98:1 carries out ball milling, obtained mixture of powders sieving sorting, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, magnesium sulfate 1-2 parts, 4-8 parts of polyphenylene sulfide, ring is added
3-7 parts of oxygen soybean oil, 1-3 parts of initiator, 2-3 parts of auxiliary agent are passed through nitrogen and exclude oxygen, then temperature after being heated to 70-75 DEG C
80-85 DEG C is risen to again, continues insulation reaction 6-10h, and air pressure returns back to normal pressure in furnace after reaction, and reactant cooling is standby
With；
(3) vacuum filtration machine is added in the reactant of step (2), with sterile water washing 3 times, it is dry that suction filtration product is placed in 65 DEG C of vacuum
Dry 40-60min in dry case；
(4) it by 3-5 parts of the dried object of step (3), dispersing agent, is added in ultrasonator, carries out ultrasonic disperse；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, carries out powdered material, drying, collection, packet
It fills, get product.
Preferably, the rotational speed of ball-mill in the step (1) is 3000r/min, Ball-milling Time 30-50min.
Preferably, the mesh size of crossing in the step (1) is 5000 mesh.
Preferably, the initiator in the step (2) is selected from azodiisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide first
One or more of acyl, lauroyl peroxide.
Preferably, the auxiliary agent in the step (2) is in stearoylketene amine, oleamide, erucyl amide, zinc stearate
It is one or more of.
Preferably, the nitrogen pressure in the step (2) is 5MPa.
Preferably, the vacuum filtration pressure in the step (3) is 5*10-8Pa。
Preferably, the dispersing agent in the step (4) is in sodium pyrophosphate, more sodium metaphosphates, potassium citrate, sodium metasilicate
One or more.
Preferably, the sonic oscillation power in the step (4) is 500W, ultrasonic time 90min.
Preferably, it is -25 DEG C that the cryospray drying parameter in the step (5), which is cryogenic temperature, and condenser temperature is -75
DEG C, atomisation pressure 5BAR.
Compared with prior art, the present invention has the advantages that:
(1) a kind of preparation method of high-strength ceramic biology 3D printing material of the invention is by aluminium oxide, silica, diatom
The raw materials such as mud, montmorillonite, graphite, hydroxylamine hydrochloride, magnesium sulfate, polyphenylene sulfide, epoxidized soybean oil pass through high speed ball milling, sieving respectively
Sorting, vacuum filtration, washs repeatedly, is dry, sonic oscillation dispersion, cryospray drying and other steps at vacuum nitrogen catalysis reaction
High-strength ceramic biology 3D printing material is prepared.The high-strength ceramic biology 3D printing material being prepared, raw material at
This compression strength low, with higher and biocompatibility, are suitable for the application of a variety of Medical racks, artificial skelecton etc..
(2) high-strength ceramic biology 3D printing material feedstock of the invention be easy to get, simple process, be suitable for heavy industrialization
With practical.
Specific embodiment
Embodiment 1
(1) it by 5 parts of aluminium oxide, 6 parts of silica, 1 part of diatom ooze, montmorillonite 2 part, 1 part of graphite, 1 part of hydroxylamine hydrochloride, is added high
In fast ball mill, rotational speed of ball-mill 3000r/min, Ball-milling Time 30min, ratio of grinding media to material 98:1 carry out ball milling, obtained powder
Mixture sieving sorting, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, it is big that 1 part of magnesium sulfate, 4 parts of polyphenylene sulfide, epoxy is added
3 parts of soya-bean oil, 1 part of azodiisobutyronitrile, 2 parts of stearoylketene amine are passed through nitrogen and exclude oxygen, nitrogen pressure after being heated to 70-75 DEG C
For 5Mpa, then temperature rises to 80-85 DEG C again, continues insulation reaction 6h, air pressure returns back to normal pressure in furnace after reaction, instead
Answer object cooling spare；
(3) vacuum filtration machine is added in the reactant of step (2), vacuum filtration pressure is 5*10-8Pa, with sterile water washing 3
It is secondary, it filters product and is placed in 65 DEG C of vacuum ovens dry 40min；
(4) it by 3 parts of the dried object of step (3), sodium pyrophosphate, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation function
Rate is 500W, ultrasonic time 90min；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
Embodiment 2
(1) it by 7 parts of aluminium oxide, 8 parts of silica, 2 parts of diatom ooze, 3 parts of montmorillonite, 2 parts of graphite, 2 parts of hydroxylamine hydrochloride, is added high
In fast ball mill, rotational speed of ball-mill 3000r/min, Ball-milling Time 40min, ratio of grinding media to material 98:1 carry out ball milling, obtained powder
Mixture sieving sorting, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, 1 part of sulfuric acid, 6 parts of polyphenylene sulfide, epoxy soybean is added
Oily 5 parts, 2 parts of azobisisoheptonitrile, 2 parts of oleamide are passed through nitrogen and exclude oxygen after being heated to 70-75 DEG C, nitrogen pressure is
5Mpa, then temperature rises to 80-85 DEG C again, continues insulation reaction 7h, and air pressure returns back to normal pressure in furnace after reaction, reaction
Object cooling is spare；
(3) vacuum filtration machine is added in the reactant of step (2), vacuum filtration pressure is 5*10-8Pa, with sterile water washing 3
It is secondary, it filters product and is placed in 65 DEG C of vacuum ovens dry 50min；
(4) it by 4 parts of the dried object of step (3), more sodium metaphosphates, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation
Power is 500W, ultrasonic time 90min；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
Embodiment 3
(1) it by 9 parts of aluminium oxide, 8 parts of silica, 2 parts of diatom ooze, 4 parts of montmorillonite, 2 parts of graphite, 3 parts of hydroxylamine hydrochloride, is added high
In fast ball mill, rotational speed of ball-mill 3000r/min, Ball-milling Time 45min, ratio of grinding media to material 98:1 carry out ball milling, obtained powder
Mixture sieving sorting, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, it is big that 2 parts of magnesium sulfate, 7 parts of polyphenylene sulfide, epoxy is added
6 parts of soya-bean oil, 2 parts of benzoyl peroxide, 3 parts of erucyl amide are passed through nitrogen and exclude oxygen, nitrogen pressure after being heated to 70-75 DEG C
For 5Mpa, then temperature rises to 80-85 DEG C again, continues insulation reaction 9h, air pressure returns back to normal pressure in furnace after reaction, instead
Answer object cooling spare；
(3) vacuum filtration machine is added in the reactant of step (2), vacuum filtration pressure is 5*10-8Pa, with sterile water washing 3
It is secondary, it filters product and is placed in 65 DEG C of vacuum ovens dry 45min；
(4) it by 4 parts of the dried object of step (3), potassium citrate, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation function
Rate is 500W, ultrasonic time 90min；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
Embodiment 4
(1) it by 10 parts of aluminium oxide, 0 part of silica 1,3 parts of diatom ooze, 5 parts of montmorillonite, 3 parts of graphite, 4 parts of hydroxylamine hydrochloride, is added
In high speed ball mill, rotational speed of ball-mill 3000r/min, Ball-milling Time 50min, ratio of grinding media to material 98:1 carry out ball milling, obtained powder
Last mixture sieving sorting, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, it is big that 2 parts of magnesium sulfate, 8 parts of polyphenylene sulfide, epoxy is added
7 parts of soya-bean oil, 3 parts of lauroyl peroxide, 3 parts of zinc stearate are passed through nitrogen and exclude oxygen, nitrogen pressure after being heated to 70-75 DEG C
For 5Mpa, then temperature rises to 80-85 DEG C again, continues insulation reaction 10h, and air pressure returns back to normal pressure in furnace after reaction,
Reactant cooling is spare；
(3) vacuum filtration machine is added in the reactant of step (2), vacuum filtration pressure is 5*10-8Pa, with sterile water washing 3
It is secondary, it filters product and is placed in 65 DEG C of vacuum ovens dry 60min；
(4) it by 5 parts of the dried object of step (3), sodium metasilicate, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation power
For 500W, ultrasonic time 90min；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
Comparative example 1
(1) by 5 parts of aluminium oxide, 6 parts of silica, montmorillonite 2 part, 1 part of graphite, 1 part of hydroxylamine hydrochloride, high speed ball mill is added
Interior, rotational speed of ball-mill 3000r/min, Ball-milling Time 30min, ratio of grinding media to material 98:1 carry out ball milling, obtained mixture of powders mistake
Screening choosing, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, 1 part of magnesium sulfate, 3 parts of epoxidized soybean oil, azo is added
1 part of bis-isobutyronitrile, 2 parts of stearoylketene amine are passed through nitrogen and exclude oxygen after being heated to 70-75 DEG C, nitrogen pressure 5Mpa is then warm
Degree rises to 80-85 DEG C again, continues insulation reaction 6h, and air pressure returns back to normal pressure in furnace after reaction, and reactant cooling is spare；
(3) vacuum filtration machine is added in the reactant of step (2), vacuum filtration pressure is 5*10-8Pa, with sterile water washing 3
It is secondary, it filters product and is placed in 65 DEG C of vacuum ovens dry 40min；
(4) it by 3 parts of the dried object of step (3), sodium pyrophosphate, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation function
Rate is 500W, ultrasonic time 90min；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
Comparative example 2
(1) it by 10 parts of aluminium oxide, 0 part of silica 1,3 parts of diatom ooze, 5 parts of montmorillonite, 3 parts of graphite, 4 parts of hydroxylamine hydrochloride, is added
In high speed ball mill, rotational speed of ball-mill 3000r/min, Ball-milling Time 50min, ratio of grinding media to material 98:1 carry out ball milling, obtained powder
Last mixture sieving sorting, crossing mesh size is 5000 mesh, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, it is big that 2 parts of magnesium sulfate, 8 parts of polyphenylene sulfide, epoxy is added
7 parts of soya-bean oil, 3 parts of lauroyl peroxide, 3 parts of zinc stearate are passed through nitrogen and exclude oxygen, nitrogen pressure after being heated to 70-75 DEG C
For 5Mpa, then temperature rises to 80-85 DEG C again, continues insulation reaction 10h, and air pressure returns back to normal pressure in furnace after reaction,
Reactant cooling is spare；
(3) it by 5 parts of the dried object of step (2), sodium metasilicate, is added in ultrasonator, carries out ultrasonic disperse, sonic oscillation power
For 500W, ultrasonic time 90min；
(4) the ultrasonic disperse product of step (3) is injected into cryospray drying machine, cryospray drying parameter is cryogenic temperature
Be -25 DEG C, condenser temperature be -75 DEG C, atomisation pressure 5BAR, carry out powdered material, drying, collection, packaging, up at
Product.
The high-strength ceramic biology 3D printing material obtained of embodiment 1-4 and comparative example 1-2 is subjected to pressure resistance respectively
This several degree, elasticity modulus, Whole blood experiments, inflammatory reaction performance tests, test result are shown in Table 1.
Table 1
| Compression strength/Mpa | Elasticity modulus/Mpa | Whole blood experiments | Inflammatory reaction | |
| Embodiment 1 | 755 | 8.1 | Without thrombus | Nothing |
| Embodiment 2 | 740 | 7.6 | Without thrombus | Nothing |
| Embodiment 3 | 735 | 7.8 | Without thrombus | Nothing |
| Embodiment 4 | 750 | 8.0 | Without thrombus | Nothing |
| Comparative example 1 | 320 | 3.1 | Slight thrombus | Nothing |
| Comparative example 2 | 455 | 2.5 | Without thrombus | Nothing |
A kind of preparation method of high-strength ceramic biology 3D printing material of the invention is by aluminium oxide, silica, diatom ooze, illiteracy
The raw materials such as de- stone, graphite, hydroxylamine hydrochloride, magnesium sulfate, polyphenylene sulfide, epoxidized soybean oil pass through high speed ball milling respectively, sieving sorts,
Vacuum nitrogen catalysis reaction, vacuum filtration, washing, dry, sonic oscillation dispersion, cryospray drying and other steps are prepared into repeatedly
To high-strength ceramic biology 3D printing material.The high-strength ceramic biology 3D printing material being prepared, cost of material is low, has
There are higher compression strength and biocompatibility, is suitable for the application of a variety of Medical racks, artificial skelecton etc..Of the invention
High-strength ceramic biology 3D printing material feedstock is easy to get, simple process, is suitable for heavy industrialization and uses, practical.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of high-strength ceramic biology 3D printing material, which comprises the following steps:
(1) by 5-10 parts of aluminium oxide, 6-10 parts of silica, 1-3 parts of diatom ooze, -5 parts of montmorillonite 2,1-3 parts of graphite, hydrochloric acid hydroxyl
It 1-4 parts of amine, is added in high speed ball mill, ratio of grinding media to material 98:1 carries out ball milling, obtained mixture of powders sieving sorting, spare；
(2) the sieving powder of step (1) is added in vacuum reaction kettle, magnesium sulfate 1-2 parts, 4-8 parts of polyphenylene sulfide, ring is added
3-7 parts of oxygen soybean oil, 1-3 parts of initiator, 2-3 parts of auxiliary agent are passed through nitrogen and exclude oxygen, then temperature after being heated to 70-75 DEG C
80-85 DEG C is risen to again, continues insulation reaction 6-10h, and air pressure returns back to normal pressure in furnace after reaction, and reactant cooling is standby
With；
(3) vacuum filtration machine is added in the reactant of step (2), with sterile water washing 3 times, it is dry that suction filtration product is placed in 65 DEG C of vacuum
Dry 40-60min in dry case；
(4) it by 3-5 parts of the dried object of step (3), dispersing agent, is added in ultrasonator, carries out ultrasonic disperse；
(5) the ultrasonic disperse product of step (4) is injected into cryospray drying machine, carries out powdered material, drying, collection, packet
It fills, get product.
2. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the rotational speed of ball-mill in (1) is 3000r/min, Ball-milling Time 30-50min.
3. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the mesh size of crossing in (1) is 5000 mesh.
4. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the initiator in (2) in azodiisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide, lauroyl peroxide one
Kind is several.
5. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the auxiliary agent in (2) is selected from one or more of stearoylketene amine, oleamide, erucyl amide, zinc stearate.
6. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the nitrogen pressure in (2) is 5MPa.
7. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the vacuum filtration pressure in (3) is 5*10-8Pa。
8. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the dispersing agent in (4) is selected from one or more of sodium pyrophosphate, more sodium metaphosphates, potassium citrate, sodium metasilicate.
9. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that the step
Suddenly the sonic oscillation power in (4) is 500W, ultrasonic time 90min.
10. the preparation method of high-strength ceramic biology 3D printing material according to claim 1, which is characterized in that described
Cryospray drying parameter in step (5) is that cryogenic temperature is -25 DEG C, and condenser temperature is -75 DEG C, atomisation pressure 5BAR.
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| CN109771701A (en) * | 2019-02-11 | 2019-05-21 | 赵延延 | A kind of preparation method of soft biological 3D printing material |
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| CN109771701A (en) * | 2019-02-11 | 2019-05-21 | 赵延延 | A kind of preparation method of soft biological 3D printing material |
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