CN104645408B - A kind of preparation method of gradient β phase tricalcium phosphate bone alternate material - Google Patents
A kind of preparation method of gradient β phase tricalcium phosphate bone alternate material Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of gradient β phase tricalcium phosphate bone alternate material, the method is β phase tricalcium phosphate, binding agent, pore gas generating agent and surfactant blank to be suppressed through successively, surfactant is used to carry out surface activation process, successively assemble with complex sintered, prepare gradient β phase tricalcium phosphate bone alternate material.Binding agent is the pva powder of 120 mesh ~ 200 mesh；Pore gas generating agent is stearic acid；Surfactant is titanium dioxide suspension.The bone alternate material that the present invention prepares has good biocompatibility, interface biological activity, can be applicable in research and the application of Archaeological iron, this bone alternate material structure designs according to bionics principle, copy the outer close interior thin structure of skeleton, the Gradient distribution structure that i.e. porosity ecto-entad successively increases, grows in material for fibrocyte, osteocyte and provides channel and space, add the bonded area of new bone and material, good mechanical properties simultaneously, close with people's bone.
Description
Technical field
The present invention relates to the preparation method of a kind of gradient β phase tricalcium phosphate bone alternate material.
Background technology
The ingredient that skeleton is wanted as body weight for humans, it plays irreplaceable protection and supporting function, is the most also responsible for the functions such as support trunk, hemopoietic, storage calcium, metabolism, is the basis of human life each internal organs of human body.Human body can be caused greatly infringement by skeletal injury, and major part Cranial defect can not spontaneous recovery, need to carry out bone alternate material transplantation treatment.The bone alternate material that can be used for bone collection treatment is varied, generally comprises metal material, nonmetallic materials and macromolecular material etc., and every kind of material can also continue to classification according to its character and feature.β phase its composition of tricalcium phosphate-based bioceramic material in nonmetallic materials is quite similar with the inorganic phase composition in sclerotin at present, its degradability, the compatibility and have special advantage in terms of induction of bone growth, therefore the application in terms of bone alternate material is quite varied.
Nature bone is made up of with havers' system the hone lamella of concentric arrays, and outer layer is fine and close, hard, thick, and for cortical bone, internal layer arrangement is loose, in cellular, for spongy bone.According to biological nature requirement, gradient β phase tricalcium phosphate bone alternate material should have controllable heterogeneous body many microporous connectivity structure and structure gradient and material distribution gradient.Porous gradient-structure increases the contact area between material and tissue fluid, accelerates course of dissolution, and the depressed area of stomatal limiting value is conducive to Local C a2+、PO4 -3Ion supersaturation, thus accelerate the deposition of β phase tricalcium phosphate, beneficially synostosis.Grow in material provide channel and space additionally, porous gradient-structure is fibrocyte, osteocyte, add the bonded area of new bone and material.Current many gradient pores bioceramic material preparation method mainly uses slip casting method and Polymeric sponge method.Slip casting method generally uses Gypsum Fibrosum being dried and easily damaging during slip casting, causing pollution hence into blank as slip casting mould, gypsum mold, material porosity and performance are produced impact；Polymeric sponge method foam impregnation ceramic size, burns organic foam after drying, and this method causes material hole wall defect more, and stress is concentrated more serious, thus causes mechanical property poor.The present invention puts the surface crushing resistance being both to ensure that Archaeological iron unlike the prior art, in turn ensure that the Biofunctional of Archaeological iron, is a kind of high efficiency method preparing longer bone alternate material.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of gradient β phase tricalcium phosphate bone alternate material, solve current material, the problem that comprcssive strength is little, Biofunctional is poor of gradient bone alternate material prepared by technology, can efficiently prepare the bone alternate material that longitudinal size is longer.
The present invention is β phase tricalcium phosphate, binding agent, pore-gas generating agent and surfactant blank to be suppressed through successively, uses surfactant to carry out surface activation process, successively assembles with complex sintered, prepare gradient β phase tricalcium phosphate bone alternate material.
Described binding agent is the pva powder of 120 mesh ~ 200 mesh.
Described pore-gas generating agent is stearic acid.
Described surfactant is titanium dioxide suspension.
The present invention comprises the concrete steps that:
First the β phase tricalcium phosphate of mass percent 60% ~ 80% and the binding agent of mass percent 20% ~ 40% are mixed, it is added to pore-gas generating agent afterwards, in raw material, the content ecto-entad of pore-gas generating agent is successively incremented by, and pore-gas generating agent addition mark is mn, n=1,2,3,4 ... .., 4≤n≤12, it is as follows that pore-gas generating agent addition is incremented by formula: mn=m1(1-5%)n, the incremental relation formula of number of apertures N and space average diameter γ is N=A γB, A therein is proportionality coefficient, and B is the number of plies of distribution of pores；Use roller batch mixer to mix afterwards, mix rotating speed 30r/min≤v1≤ 60r/min, incorporation time 20min≤t1≤30min；
Preparation n group batch mixing, 4≤n≤12, be labeled as T the most successively altogether1, T2..., Tn-1, Tn；
The preparation method of gradient-structure comprises the steps:
The most successively suppress blank: using stainless steel mould, molding die mark is Mn, n=1,2,3,4 ... .., 4≤n≤12, wherein molding die MnOuter radius more than molding die Mn-1Outer radius, raw material is the most inwardly suppressed from outermost layer according to correspondence order, compacting pressure be P1, 60MPa≤P1≤ 200MPa, compacting is divided into four-stage, per dwell time in stage to be respectively t1
, t2, t3, t4, 15s≤t1, t2, t3≤ 120s, 600s≤t4≤ 800s, deflation time is respectively t' 1, t' 2, t' 3, 15s≤t' 1, t' 2, t' 3≤150s；
It is F that mold pressing obtains blank markn, n=1,2,3,4 ... .., 4≤n≤12, blank interface is semicircular arc, and external diameter is Rno, internal diameter is Rni, n=2,3,4 ... .., 4≤n≤12, and adjacent two blank internal-and external diameters meet Rno=R(n+1)i+ θ, 0.00mm≤θ≤0.02mm, core blank interface is semicircle, and radius is R1, R1=R2i+ θ, above mold process repeats two cycles, and second round, mold pressing obtained blank F'n, n=1,2,3,4 ... .., 4≤n≤12, mold with the period 1 and obtain blank FnIdentical；
2. surface activation process: using titanium dioxide suspension even application in blank inner surface, dried coating layer thickness is h1, h1=k θ, 0.6≤k≤1.2；
The most successively assemble: above-mentioned mold pressing is obtained blank FnWith F'nThe most outwards carrying out splicing according to correspondence order from innermost layer to assemble, the corner between adjacent two layers blank splicing seams is α, α=30 °, clockwise, obtains n-layer blank FnWith F'nThe cylindrical coaxial complex blank F, a length of L assembledF, 5cm≤LF≤ 60cm, radius is RF, RF=Rno+ (2n-2) θ, stands 30min；Inserting in sintering mold S by cylindrical coaxial complex blank F, sintering mold S is the hollow cylinder that stainless steel material makes, a length of Ls, Ls >=LF, inside radius is Rsi, Rsi=RF+ k θ, 0.8≤k≤1.5；
The most complex sintered: to use gradient temperature repeatedly to sinter gradient porous coaxial complex blank F；
The sintering first stage, sintering temperature T1, T1Be 1 ~ 200 DEG C, heat time heating time ta1, ta1For 63min, temperature retention time tb1, tb1For 30min；
Sintering second stage, sintering temperature T2, T2Be 200 ~ 250 DEG C, heat time heating time ta2, ta2For 25min, temperature retention time tb2, tb2For 30min；
The sintering phase III, sintering temperature is T3, T3Be 250 ~ 380 DEG C, heat time heating time ta3, ta3For 65min, temperature retention time tb3, tb3For 30min；
Sintering fourth stage, sintering temperature is T4, T4Be 380 ~ 1000 DEG C, heat time heating time ta4, ta4For 207min, temperature retention time tb4, tb4For 5h, furnace cooling, obtain a kind of gradient β phase tricalcium phosphate bone alternate material.
Beneficial effects of the present invention:
The gradient β phase tricalcium phosphate bone alternate material prepared, is a kind of bioactive β phase tricalcium phosphate-based bioceramic material, and it is having well application in terms of the Orthopedic Clinical treatments such as osseous tissue disappearance reparation, tissue reconstruction, bone disease treatment.And simulate porous " the interior thin outer close " gradient-structure of nature bone concentric arrays bone plate structure and imitated osseous tissue, internal structure hole rate is high, be conducive to obtaining the absorption skeletal growth factor such as bone morphogenetic protein(BMP) or marrow stromal cell, and reasonably mate the concentration of skeletal growth factor in complex；Layer structure porosity is low, and mechanical property is good, and compressive property is high；Can efficiently prepare, by this method, the bone alternate material that longitudinal size is longer, it is to avoid in pressing process blank be stressed inequality impact；Use surface activation process every layer blank inner surface, strengthen the associativity between every layer of blank；Use successively corner splicing to assemble blank method, be prevented effectively from the problems such as stress at splicing seams is concentrated, mechanical property is unstable；Finally, the present invention uses repeatedly gradient temperature to sinter, and makes blank produce granule under suitable temperature environment and coheres, and produces intensity and causes densification and recrystallization, becoming the gradient β phase tricalcium phosphate bone alternate material of a kind of high-quality.
Accompanying drawing explanation
Fig. 1 is the flow chart of the present invention.
Fig. 2 is the cross section sectional view of four layers of gradient β phase tricalcium phosphate bone alternate material that the present invention prepares.
Detailed description of the invention
The present invention is β phase tricalcium phosphate, binding agent, pore-gas generating agent and surfactant blank to be suppressed through successively, uses surfactant to carry out surface activation process, successively assembles with complex sintered, prepare gradient β phase tricalcium phosphate bone alternate material.
As it is shown in figure 1, the present invention's comprises the concrete steps that:
First the β phase tricalcium phosphate of mass percent 60% ~ 80% and the binding agent of mass percent 20% ~ 40% are mixed, it is added to pore-gas generating agent afterwards, in raw material, the content ecto-entad of pore-gas generating agent is successively incremented by, and pore-gas generating agent addition mark is mn, n=1,2,3,4 ... .., 4≤n≤12, it is as follows that pore-gas generating agent addition is incremented by formula: mn=m1(1-5%)n, the incremental relation formula of number of apertures N and space average diameter γ is N=A γB, A therein is proportionality coefficient, and B is the number of plies of distribution of pores；Use roller batch mixer to mix afterwards, mix rotating speed 30r/min≤v1≤ 60r/min, incorporation time 20min≤t1≤30min；
Preparation n group batch mixing, 4≤n≤12, be labeled as T the most successively altogether1, T2..., Tn-1, Tn；
The preparation method of gradient-structure comprises the steps:
The most successively suppress blank: using stainless steel mould, molding die mark is Mn, n=1,2,3,4 ... .., 4≤n≤12, wherein molding die MnOuter radius more than molding die Mn-1Outer radius, raw material is the most inwardly suppressed from outermost layer according to correspondence order, compacting pressure be P1, 60MPa≤P1≤ 200MPa, compacting is divided into four-stage, per dwell time in stage to be respectively t1
, t2, t3, t4, 15s≤t1, t2, t3≤ 120s, 600s≤t4≤ 800s, deflation time is respectively t' 1, t' 2, t' 3, 15s≤t' 1, t' 2, t' 3≤150s；
It is F that mold pressing obtains blank markn, n=1,2,3,4 ... .., 4≤n≤12, blank interface is semicircular arc, and external diameter is Rno, internal diameter is Rni, n=2,3,4 ... .., 4≤n≤12, and adjacent two blank internal-and external diameters meet Rno=R(n+1)i+ θ, 0.00mm≤θ≤0.02mm, core blank interface is semicircle, and radius is R1, R1=R2i+ θ, above mold process repeats two cycles, and second round, mold pressing obtained blank F'n, n=1,2,3,4 ... .., 4≤n≤12, mold with the period 1 and obtain blank FnIdentical；
2. surface activation process: using titanium dioxide suspension even application in blank inner surface, dried coating layer thickness is h1, h1=k θ, 0.6≤k≤1.2；
The most successively assemble: above-mentioned mold pressing is obtained blank FnWith F'nThe most outwards carrying out splicing according to correspondence order from innermost layer to assemble, the corner between adjacent two layers blank splicing seams is α, α=30 °, clockwise, obtains n-layer blank FnWith F'nThe cylindrical coaxial complex blank F, a length of L assembledF, 5cm≤LF≤ 60cm, radius is RF, RF=Rno+ (2n-2) θ, stands 30min；Inserting in sintering mold S by cylindrical coaxial complex blank F, sintering mold S is the hollow cylinder that stainless steel material makes, a length of Ls, Ls >=LF, inside radius is Rsi, Rsi=RF+ k θ, 0.8≤k≤1.5；
The most complex sintered: to use gradient temperature repeatedly to sinter gradient porous coaxial complex blank F；
The sintering first stage, sintering temperature T1, T1Be 1 ~ 200 DEG C, heat time heating time ta1, ta1For 63min, temperature retention time tb1, tb1For 30min；
Sintering second stage, sintering temperature T2, T2Be 200 ~ 250 DEG C, heat time heating time ta2, ta2For 25min, temperature retention time tb2, tb2For 30min；
The sintering phase III, sintering temperature is T3, T3Be 250 ~ 380 DEG C, heat time heating time ta3, ta3For 65min, temperature retention time tb3, tb3For 30min；
Sintering fourth stage, sintering temperature is T4, T4Be 380 ~ 1000 DEG C, heat time heating time ta4, ta4For 207min, temperature retention time tb4, tb4For 5h, furnace cooling, obtain a kind of gradient β phase tricalcium phosphate bone alternate material.
Four layers of gradient β phase tricalcium phosphate bone alternate material prepare example:
First 80g β phase tricalcium phosphate and 20g polyvinyl alcohol are weighed, being added to stearic acid afterwards, in raw material, stearic addition the most successively successively decreases, respectively 50.00g, 45.13g, 42.87g, 40.73g, use roller batch mixer to mix, mixing rotating speed 50r/min, incorporation time 30min, prepares 4 groups of batch mixings altogether, is labeled as T the most successively1, T2, T3, T4；
The most successively suppress blank: using stainless steel mould, molding die mark is Mn, n=1,2,3,4, wherein molding die MnOuter radius be greater than molding die Mn-1Outer radius, by raw material TnThe most inwardly suppressing from outermost layer according to correspondence order, compacting pressure is P1, P1=100MPa, compacting is divided into four-stage, per dwell time in stage to be respectively t1, t2, t3, t4, 15s≤t1, t2, t3≤ 120s, 600s≤t4≤ 800s, deflation time is respectively t' 1, t' 2, t' 3, 15s≤t' 1, t' 2, t' 3≤150s；Blank mark is Fn, n=1,2,3,4, blank interface is semicircular arc, and external diameter is Rno, internal diameter is Rni, n=2,3,4, and adjacent two blank internal-and external diameters meet Rno=R( n+1 ) i+ θ, 0.00mm≤θ≤0.02mm, core blank interface is semicircle, and radius is R1, R1=R2i+ θ, above mold process repeats two cycles, and second round, mold pressing obtained blank F'n, n=1,2,3,4, mold with the period 1 and obtain blank FnIdentical；
2. surface activation process: configuration titanium dioxide suspension, concentration is 10g/l, suspension configured after even application is in blank inner surface at once, dried coating layer thickness is h1, h1=k θ, 0.6≤k≤1.2；
The most successively assemble: above-mentioned mold pressing is obtained blank FnWith F'n, n=1,2,3,4, the most outwards carry out splicing according to correspondence order from innermost layer and assemble, the corner between adjacent two layers blank splicing seams is α, α=30 °, clockwise, obtains 4 layers of blank FnWith F'nThe cylindrical coaxial complex blank F, a length of L assembledF, 5cm≤LF≤ 60cm, radius is RF, RF=Rno+ 6 θ, stand 30min；Inserting in sintering mold S by cylindrical coaxial complex blank F, sintering mold S is the hollow cylinder that stainless steel material makes, a length of Ls, Ls >=LF, inside radius is Rsi, Rsi=RF+ k θ, 0.8≤k≤1.5；
The most complex sintered: to use gradient temperature repeatedly to sinter gradient porous coaxial complex blank F；
The sintering first stage, sintering temperature T1, T1Be 1 ~ 200 DEG C, heat time heating time ta1, ta1=63min, temperature retention time tb1, tb1=30min；
Sintering second stage, sintering temperature T2, T2Be 200 ~ 250 DEG C, heat time heating time ta2, ta2=25min, temperature retention time tb2, tb2=30min；
The sintering phase III, sintering temperature is T3, T3Be 250 ~ 380 DEG C, heat time heating time ta3, ta3=65min, temperature retention time tb3, tb3=30min；
Sintering fourth stage, sintering temperature is T4, T4Be 380 ~ 1000 DEG C, heat time heating time ta4, ta4=207min, temperature retention time tb4, tb4=5h, furnace cooling, i.e. prepare four layers of gradient β phase tricalcium phosphate bone alternate material.The internal structure of four layers of gradient β phase tricalcium phosphate bone alternate material is as in figure 2 it is shown, ground floor blank 1 therein is obtained by F1 with F'1 assembling.Second layer blank 2 is assembled by F2 with F'2 and obtains.Third layer blank 3 is assembled by F3 with F'3 and obtains.4th layer of blank 4 is assembled by F4 with F'4 and obtains.
Claims (1)
1. the preparation method of a gradient β phase tricalcium phosphate bone alternate material, the method is β phase tricalcium phosphate, binding agent, pore-gas generating agent and surfactant blank to be suppressed through successively, surfactant is used to carry out surface activation process, successively assemble with complex sintered, prepare gradient β phase tricalcium phosphate bone alternate material；
Described binding agent is the pva powder of 120 mesh ~ 200 mesh；
Described pore-gas generating agent is stearic acid；
Described surfactant is titanium dioxide suspension, and concentration is 10g/l；
Comprising the concrete steps that of the method: first the β phase tricalcium phosphate of mass percent 60% ~ 80% and the binding agent of mass percent 20% ~ 40% are mixed, it is added to pore-gas generating agent afterwards, in raw material, the content ecto-entad of pore-gas generating agent is successively incremented by, and pore-gas generating agent addition mark is mn, n=1,2,3,4 ... .., 4≤n≤12, it is as follows that pore-gas generating agent addition is incremented by formula: mn=m1(1-5%)n, the incremental relation formula of number of apertures N and space average diameter γ is N=A γB, A therein is proportionality coefficient, and B is the number of plies of distribution of pores；Use roller batch mixer to mix afterwards, mix rotating speed 30r/min≤v1≤ 60r/min, incorporation time 20min≤t1≤30min；
Preparation n group batch mixing, 4≤n≤12, be labeled as T the most successively altogether1, T2..., Tn-1, Tn；
The preparation method of gradient-structure comprises the steps:
The most successively suppress blank: using stainless steel mould, molding die mark is Mn, n=1,2,3,4 ... .., 4≤n≤12, wherein molding die MnOuter radius more than molding die Mn-1Outer radius, raw material is the most inwardly suppressed from outermost layer according to correspondence order, compacting pressure be P1, 60MPa≤P1≤ 200MPa, compacting is divided into four-stage, per dwell time in stage to be respectively t1, t2, t3, t4, 15s≤t1, t2, t3≤ 120s, 600s≤t4≤ 800s, deflation time is respectively t' 1, t' 2, t' 3, 15s≤t' 1, t' 2, t' 3≤150s；
It is F that mold pressing obtains blank markn, n=1,2,3,4 ... .., 4≤n≤12, blank interface is semicircular arc, and external diameter is Rno, internal diameter is Rni, n=2,3,4 ... .., 4≤n≤12, and adjacent two blank internal-and external diameters meet Rno=R(n+1)i+ θ, 0.00mm≤θ≤0.02mm, core blank interface is semicircle, and radius is R1, R1=R2i+ θ, above mold process repeats two cycles, and second round, mold pressing obtained blank F'n, n=1,2,3,4 ... .., 4≤n≤12, mold with the period 1 and obtain blank FnIdentical；
2. surface activation process: using titanium dioxide suspension even application in blank inner surface, dried coating layer thickness is h1, h1=k θ, 0.6≤k≤1.2；0.00mm≤θ≤0.02mm；
The most successively assemble: above-mentioned mold pressing is obtained blank FnWith F'nThe most outwards carrying out splicing according to correspondence order from innermost layer to assemble, the corner between adjacent two layers blank splicing seams is α, α=30 °, clockwise, obtains n-layer blank FnWith F'nThe cylindrical coaxial complex blank F, a length of L assembledF, 5cm≤LF≤ 60cm, radius is RF, RF=Rno+ (2n-2) θ, stands 30min；Inserting in sintering mold S by cylindrical coaxial complex blank F, sintering mold S is the hollow cylinder that stainless steel material makes, a length of Ls, Ls >=LF, inside radius is Rsi, Rsi=RF+ k θ, 0.8≤k≤1.5；0.00mm≤θ≤0.02mm；
The most complex sintered: to use gradient temperature repeatedly to sinter gradient porous coaxial complex blank F；
The sintering first stage, sintering temperature T1, T1Be 1 ~ 200 DEG C, heat time heating time ta1, ta1For 63min, temperature retention time tb1, tb1For 30min；
Sintering second stage, sintering temperature T2, T2Be 200 ~ 250 DEG C, heat time heating time ta2, ta2For 25min, temperature retention time tb2, tb2For 30min；
The sintering phase III, sintering temperature is T3, T3Be 250 ~ 380 DEG C, heat time heating time ta3, ta3For 65min, temperature retention time tb3, tb3For 30min；
Sintering fourth stage, sintering temperature is T4, T4Be 380 ~ 1000 DEG C, heat time heating time ta4, ta4For 207min, temperature retention time tb4, tb4For 5h, furnace cooling, obtain a kind of gradient β phase tricalcium phosphate bone alternate material.
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| CN107376007A (en) * | 2017-06-15 | 2017-11-24 | 华南理工大学 | A kind of bionical non-homogeneous structural bio-vitric support and preparation method thereof |
| CN108514655B (en) * | 2018-03-20 | 2020-03-31 | 山东大学 | Preparation method of gradient porous calcium polyphosphate ceramic material with non-crystallized surface |
| CN108546107B (en) * | 2018-03-21 | 2021-05-28 | 山东大学深圳研究院 | Gradient porous calcium polyphosphate ceramic material and preparation method thereof |
| CN108480624B (en) * | 2018-04-13 | 2019-09-13 | 昆明理工大学 | A kind of powder is incremented by pressure setting and drawing method |
| CN110721010B (en) * | 2019-10-24 | 2021-10-26 | 重庆大学 | Radial gradient implant lattice structure and design method thereof |
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