CN109053185A - A kind of preparation method of biological active ceramic material - Google Patents
A kind of preparation method of biological active ceramic material Download PDFInfo
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- CN109053185A CN109053185A CN201811046798.8A CN201811046798A CN109053185A CN 109053185 A CN109053185 A CN 109053185A CN 201811046798 A CN201811046798 A CN 201811046798A CN 109053185 A CN109053185 A CN 109053185A
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- C04B35/447—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 phosphates, e.g. hydroxyapatite
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- 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
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- 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
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Abstract
The invention discloses a kind of preparation methods of biological active ceramic material, belong to medical material tech field.Using hydroxyapatite, silicoglaserite and discarded bioactivity glass as raw material in the present invention, in conjunction with polycaprolactone and pore creating material etc., a kind of biological active ceramic material is prepared by 3D printing method, the good biocompatibility of bioactivity glass and bioactivity had not only been maintained by the biological active ceramic material that discarded bioactivity glass and polycaprolactone, hydroxyapatite, silicoglaserite form, but also improved mechanical performance and degradation rate in vivo；It is combined using freeze-drying and sintering process and prepares bioactive ceramics, be frozen into eutectic point at low temperature hereinafter, the moisture in bioceramic becomes solid ice, be then sintered, it is vapor that ice, which directly distil, to obtain bioceramic；In sublimation process, physical structure and chemical structure are constant, and bioceramic is able to maintain original solid structure and form, it is ensured that the bioactivity of bracket.
Description
Technical field
The present invention relates to a kind of preparation methods of biological active ceramic material, belong to medical material tech field.
Background technique
The porous structure of biological bone tissue can adapt to a certain range of stress variation, while porous organization can
Make blood circulation, ensure that the normal growth metabolism of bone tissue.The defect of body bone tissue, especially osteomyelitis, bone tumour, bone
The bone defect of larger area caused by the operations such as tumour excision and wound, has seriously affected the physiological function of body bone tissue.
The operative treatment of bone defect repairs defect with filling material of bone appropriate, is fast quick-recovery morbid state or traumatic bone defect
The effective ways of tissue physiology's function.Self bone tissue is the ideal material of bone filling, but source seldom also needs second operation；
Allosome bone tissue the problems such as there may be rejection and transmissions.With the continuous improvement of surgical technic and medical level,
The demand of the bone alternate material of synthesis is continuously increased.The bioactivity of synthesis and application simulation body bone tissue porosity characteristic
With the bioceramic material of biocompatibility, the concern of scientist and clinician are caused.
Bio-medical material is the diagnosis for biosystem disease, treatment, reparation or replacement bio-tissue or organ,
Promote or restore the material of its function.Early stage people repair human body wound using natural material, with medicine and material science
Development, some metal materials, inorganic non-metallic material and organic material for example stainless steel, titanium alloy, noble metal, aluminium oxide pottery
Porcelain, polytetrafluoroethylene (PTFE) etc. are used to manufacturing artificial graft materials, play one to extension human longevity and raising quality of life and are set for
With.But from the point of view of medical application angle, these materials belong to bio-inert material, i.e., are combined with tissue without activity,
Therefore there are many problems and defects in clinical application.
Calcium phosphate ceramics, as the remarkable advantage of hydroxyapatite and bata-tricalcium phosphate ceramics is their composition and bone
Mineralising phase composition it is very similar, it is this kind of ceramics have more excellent compatibility and osteo-conductive, porous hydroxyapatite
Ceramics, porous calcium phosphate ceramic have high bioactivity and biocompatibility, very strong with the binding ability of bone tissue, are good
Good bone tissue defect packing material, but the mechanical strength of calcium phosphate ceramics is lower.Moreover, recent studies have shown that calcium phosphate
The degradability of class ceramics is slower, and especially sintered hydroxyapatite degradation in vivo is very slow.
Summary of the invention
The technical problems to be solved by the invention: lower for existing bioceramic mechanical strength, degradation in vivo is very
Slow problem provides a kind of preparation method of biological active ceramic material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) discarded bioactivity glass is pre-processed, obtains pretreated glass, pretreated glass is crushed, is ground,
Sieving, obtains glass powder；
(2) according to parts by weight, weigh respectively 20~36 parts of glass powders, 30~40 parts of hydroxyapatites, 10~20 parts of silicoglaserites,
Polyvinyl alcohol water solution that polycaprolactone-acetic acid solution that 8~15 parts of mass fractions are 8%, 10~18 parts of mass fractions are 10%,
1~10 part of pore creating material, by glass powder, hydroxyapatite, silicoglaserite, polycaprolactone-acetic acid solution that mass fraction is 8%, quality
Polyvinyl alcohol water solution that score is 10%, pore creating material mixing, stir process obtains mixed slurry, mixed slurry carried out 3D printing
Processing, obtains presoma, presoma is put into freezing processing in liquid nitrogen, obtains freezing presoma, after vacuum drying treatment, takes out, burns
Knot processing, is cooled to room temperature to get biological active ceramic material.
Pretreatment described in step (1) is to use the bioactivity glass discarded respectively acetone and deionized water to impregnate ultrasound
4~6h is placed in 60~80 DEG C of baking oven and dries to constant weight.
Glass powder described in step (1) crosses 100~200 meshes.
Pore creating material described in step (2) is that ammonium hydrogen carbonate and starch in mass ratio 1: 2 mix.
Stir process described in step (2) is that 1~2h is stirred in the case where revolving speed is 1000~1500r/min.
It is 1.5~3.8bar that the technological parameter of the processing of 3D printing described in step (2), which is pressure, movement speed is 9~
12mm/s, printing mouth shape be it is rectangular, size is 0.4~0.6mm, print 10~15 layers.
Freezing processing described in step (2) is to be put into 4~6h of freezing in liquid nitrogen.
Vacuum drying treatment described in step (2) is that 40~48h is dried in vacuo in the baking oven that temperature is 40~50 DEG C.
Sintering processes described in step (2) be 1200~1300 DEG C in temperature at 1~2h of sintering processes.
The present invention is compared with other methods, and advantageous effects are:
(1) it using hydroxyapatite, silicoglaserite and discarded bioactivity glass as raw material in the present invention, in conjunction with polycaprolactone and makes
Hole agent etc. prepares a kind of biological active ceramic material by 3D printing method, and bioactivity glass has good bone guided
And osteoinductive, Bone formation-related gene can be activated, promotes vascularization, while bioactivity glass also has good antibacterial
Property, controllable biological degradability, good mechanical performance, higher bioactivity, be added silicoglaserite can improve hydroxyapatite
Degradation rate；The mechanical performance and degradability of polycaprolactone are excellent, to the sticking of cell, are proliferated extremely advantageous, can induce blood vessel
It generates, the biological active ceramic material being made of discarded bioactivity glass and polycaprolactone, hydroxyapatite, silicoglaserite was both
The good biocompatibility of bioactivity glass and bioactivity are maintained, and improves mechanical performance and degradation in vivo
Rate；
(2) present invention is combined using freeze-drying and sintering process, is prepared bioactive ceramics, is frozen into eutectic point at low temperature
Hereinafter, the moisture in bioceramic is made to become solid ice, then it is sintered, so that ice is directly distilled is vapor, is made
Hole agent excludes during heating, to obtain porous bio-ceramic；The porous bio-ceramic of freeze-drying in sublimation process,
Physical structure and chemical structure are almost unchanged, and bioceramic is able to maintain original solid structure and form, in sublimation process,
The distillation of solid ice crystal forms spongy porous structure, biology in sublimation process to leave hole in bioceramic after vapor
The thermal deformation of material is small, can farthest guarantee the bioactivity of bracket.
Specific embodiment
It uses acetone and deionized water to impregnate 4~6h of ultrasound respectively discarded bioactivity glass, is placed in 60~80 DEG C
It dries in baking oven to constant weight, obtains pretreated glass, pretreated glass is crushed, is ground, and cross 100~200 meshes, obtain glass
Glass powder；In mass ratio 1: 2 is uniformly mixed ammonium hydrogen carbonate and starch, obtains pore creating material；According to parts by weight, 20~36 are weighed respectively
Polycaprolactone-acetic acid that part glass powder, 30~40 parts of hydroxyapatites, 10~20 parts of silicoglaserites, 8~15 parts of mass fractions are 8%
Solution, the polyvinyl alcohol water solution that 10~18 parts of mass fractions are 10%, 1~10 part of pore creating material, by glass powder, hydroxyapatite,
Polyvinyl alcohol water solution that polycaprolactone-acetic acid solution that silicoglaserite, mass fraction are 8%, mass fraction are 10%, pore creating material are mixed
It closes, stirs 1~2h in the case where revolving speed is 1000~1500r/min, obtain mixed slurry, be 1.5~3.8bar, movement speed in pressure
For 9~12mm/s, print mouth shape be it is rectangular, size is to print 10~15 layers under 0.4~0.6mm, presoma is obtained, by forerunner
Body is put into 4~6h of freezing in liquid nitrogen, obtains freezing presoma, after being dried in vacuo 40~48h in the baking oven that temperature is 40~50 DEG C,
It takes out, 1~2h of sintering processes at being 1200~1300 DEG C in temperature is cooled to room temperature to get biological active ceramic material.
It uses acetone and deionized water to impregnate ultrasound 4h respectively discarded bioactivity glass, is placed in 60 DEG C of baking oven and does
It is dry to constant weight, obtain pretreated glass, pretreated glass be crushed, is ground, and is sieved with 100 mesh sieve, glass powder is obtained；In mass ratio
Be uniformly mixed ammonium hydrogen carbonate and starch at 1: 2, obtains pore creating material；According to parts by weight, 20 parts of glass powders, 30 parts of hydroxyls are weighed respectively
The poly- second that polycaprolactone-acetic acid solution that apatite, 10 parts of silicoglaserites, 8 parts of mass fractions are 8%, 10 parts of mass fractions are 10%
Enol aqueous solution, 1 part of pore creating material, glass powder, hydroxyapatite, silicoglaserite, mass fraction is molten for 8% polycaprolactone-acetic acid
Liquid, the polyvinyl alcohol water solution that mass fraction is 10%, pore creating material mixing are stirred 1h in the case where revolving speed is 1000r/min, must be mixed
Slurry is 1.5bar, movement speed 9mm/s in pressure, and printing mouth shape is that rectangular, size is to print 10 layers under 0.4mm,
Presoma is obtained, presoma is put into liquid nitrogen and freezes 4h, obtains freezing presoma, is dried in vacuo in the baking oven that temperature is 40 DEG C
It after 40h, takes out, sintering processes 1h at being 1200 DEG C in temperature is cooled to room temperature to get biological active ceramic material.
It uses acetone and deionized water to impregnate ultrasound 5h respectively discarded bioactivity glass, is placed in 70 DEG C of baking oven and does
It is dry to obtain pretreated glass to constant weight, pretreated glass is crushed, is ground, and 150 meshes are crossed, obtain glass powder；In mass ratio
Be uniformly mixed ammonium hydrogen carbonate and starch at 1: 2, obtains pore creating material；According to parts by weight, 28 parts of glass powders, 35 parts of hydroxyls are weighed respectively
The poly- second that polycaprolactone-acetic acid solution that apatite, 15 parts of silicoglaserites, 11 parts of mass fractions are 8%, 14 parts of mass fractions are 10%
Enol aqueous solution, 15 parts of pore creating materials, by glass powder, hydroxyapatite, silicoglaserite, polycaprolactone-acetic acid that mass fraction is 8%
Solution, the polyvinyl alcohol water solution that mass fraction is 10%, pore creating material mixing are stirred 1.5h in the case where revolving speed is 1250r/min, are obtained
Mixed slurry is 2.7bar, movement speed 10mm/s in pressure, and printing mouth shape is that rectangular, size is printing under 0.5mm
12 layers, presoma is obtained, presoma is put into liquid nitrogen and freezes 5h, obtains freezing presoma, the vacuum in the baking oven that temperature is 45 DEG C
It after dry 44h, takes out, sintering processes 1.5h at being 1250 DEG C in temperature is cooled to room temperature to get biological active ceramic material.
It uses acetone and deionized water to impregnate ultrasound 6h respectively discarded bioactivity glass, is placed in 80 DEG C of baking oven and does
It is dry to obtain pretreated glass to constant weight, pretreated glass is crushed, is ground, and 200 meshes are crossed, obtain glass powder；In mass ratio
Be uniformly mixed ammonium hydrogen carbonate and starch at 1: 2, obtains pore creating material；According to parts by weight, 36 parts of glass powders, 40 parts of hydroxyls are weighed respectively
The poly- second that polycaprolactone-acetic acid solution that apatite, 20 parts of silicoglaserites, 15 parts of mass fractions are 8%, 18 parts of mass fractions are 10%
Enol aqueous solution, 10 parts of pore creating materials, by glass powder, hydroxyapatite, silicoglaserite, polycaprolactone-acetic acid that mass fraction is 8%
Solution, the polyvinyl alcohol water solution that mass fraction is 10%, pore creating material mixing are stirred 2h in the case where revolving speed is 1500r/min, are obtained mixed
Slurry is closed, is 3.8bar, movement speed 12mm/s in pressure, printing mouth shape is that rectangular, size is printing 15 under 0.6mm
Layer, obtains presoma, presoma is put into liquid nitrogen and freezes 6h, obtain freezing presoma, and vacuum is dry in the baking oven that temperature is 50 DEG C
It after dry 48h, takes out, sintering processes~2h at being 1300 DEG C in temperature is cooled to room temperature to get biological active ceramic material.
Biological active ceramic material prepared by the present invention and commercially available bioceramic are detected, specific detection is as follows:
External degradation test:
It is impregnated, is tested in HH- according to the quality of bioactive ceramics and the ratio of the corresponding 100mL of simulated body fluid volume 1g
Carried out in CP-01P type constant incubator, temperature be set as with 36.8 DEG C similar in body temperature, every for 24 hours to SBF solution into
Row replacement pays attention to observation situation of change daily.After 14 days, taking-up is cleaned under conditions of supersonic oscillations with deionized water repeatedly
After be placed on and set 60 DEG C in 2K-35S type electric vacunm drying case and be dried, it is dry for 24 hours after taken out every half an hour and weigh matter
Amount proves that sample is completely dried when changing unobvious, and with AL204 type electronic balance weighing, its quality is accurate to 0.01g, and
It is compared with the quality before degradation, to obtain degradation rate.
Degradation rate=((quality after quality-degradation before degrading)/quality before degrading) × 100%
Compressive strength:
The test of compressive strength is referring to standard GB/T/T1964-1996 (porous ceramics compressive strength experimental method), by sample
It is put into baking oven, dry 2h, places into drier and be cooled to room temperature at a temperature of 110 ± 5 DEG C；Measure the side of sample compression face
Long or diameter calculates compression face area；Sample is placed on to the centre of Material Testing Machine lower platen, with 1.5~2.5MPa/
The rate of s applies load, until sample destroys.Read peak load value when sample destroys.(high porosity sample is not obvious
When breakoff phenomenon, sample is using height change 10% as sample breakdown point.)
Compressive strength=failing load/sample stress surface area
Specific test result such as table 1.
1 performance characterization contrast table of table
| Project | Example 1 | Example 2 | Example 3 | Reference examples |
| Degradation rate (%) | 5.86 | 5.35 | 5.57 | 2.33 |
| Compressive strength (MPa) | 8.57 | 8.63 | 8.68 | 5.23 |
As shown in Table 1, high strength bioactive ceramics degradation rate prepared by the present invention increases, and compressive strength is preferable, tool
Have broad application prospects.
Claims (9)
1. a kind of preparation method of biological active ceramic material, it is characterised in that specific preparation step are as follows:
(1) discarded bioactivity glass is pre-processed, obtains pretreated glass, pretreated glass is crushed, is ground,
Sieving, obtains glass powder；
(2) according to parts by weight, weigh respectively 20~36 parts of glass powders, 30~40 parts of hydroxyapatites, 10~20 parts of silicoglaserites,
Polyvinyl alcohol water solution that polycaprolactone-acetic acid solution that 8~15 parts of mass fractions are 8%, 10~18 parts of mass fractions are 10%,
1~10 part of pore creating material, by glass powder, hydroxyapatite, silicoglaserite, polycaprolactone-acetic acid solution that mass fraction is 8%, quality
Polyvinyl alcohol water solution that score is 10%, pore creating material mixing, stir process obtains mixed slurry, mixed slurry carried out 3D printing
Processing, obtains presoma, presoma is put into freezing processing in liquid nitrogen, obtains freezing presoma, after vacuum drying treatment, takes out, burns
Knot processing, is cooled to room temperature to get biological active ceramic material.
2. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (1) institute
The pretreatment stated is to use the bioactivity glass discarded respectively acetone and deionized water to impregnate 4~6h of ultrasound, is placed in 60~80
DEG C baking oven in dry to constant weight.
3. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (1) institute
The glass powder stated crosses 100~200 meshes.
4. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The pore creating material stated is that ammonium hydrogen carbonate and starch in mass ratio 1: 2 mix.
5. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The stir process stated is that 1~2h is stirred in the case where revolving speed is 1000~1500r/min.
6. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The technological parameter for the 3D printing processing stated is that pressure is 1.5~3.8bar, and movement speed is 9~12mm/s, and printing mouth shape is
Rectangular, size is 0.4~0.6mm, prints 10~15 layers.
7. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The freezing processing stated is to be put into 4~6h of freezing in liquid nitrogen.
8. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The vacuum drying treatment stated is that 40~48h is dried in vacuo in the baking oven that temperature is 40~50 DEG C.
9. a kind of preparation method of biological active ceramic material according to claim 1, it is characterised in that: step (2) institute
The sintering processes stated be 1200~1300 DEG C in temperature at 1~2h of sintering processes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110227178A (en) * | 2019-07-30 | 2019-09-13 | 广东工业大学 | A kind of bioceramic scaffold and its application |
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| DE102006026000A1 (en) * | 2006-06-01 | 2008-02-21 | Curasan Ag | Binder for calcium phosphate or glass-ceramic particles, useful for producing bone reconstruction materials, comprises an aqueous or alcoholic solution of a carboxylic acid |
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| CN105770987A (en) * | 2016-04-12 | 2016-07-20 | 深圳先进技术研究院 | 3D printing pulp of bone repair stent, bone repair stent and preparing method and application of bone repair stent |
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| CN110227178A (en) * | 2019-07-30 | 2019-09-13 | 广东工业大学 | A kind of bioceramic scaffold and its application |
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