CN107311654A - A kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material - Google Patents
A kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material, this method comprises the following steps：Function-graded material powder preparation；Green compact test material preparation；Test specimen is sintered.The material of the present invention takes full advantage of the good biocompatibilities of n HA, biological activity and bio-inert material ZrO2The high advantage of mechanical strength, have stronger practicality and theory significance.
Description
Technical field
The present invention relates to bioactive materials technical field, specifically, it is related to a kind of oxidation zirconium base nano-hydroxy-apatite
The preparation method of stone function-graded material.
Background technology
Application of the bioactive materials in bone tissue defect and plantation are repaired is more and more extensive, but its produced problem
More and more, the interface cohesion of especially implant and surrounding hard and soft tissue is directly connected to the stability of implant, is treatment
It is successfully crucial.Substantial amounts of research shows that nanometer hydroxyapatite (nano-hydroxyapatite, n-HA) has good
Biocompatibility and bioactivity, are sintered to after bioceramic, still be can induce osteoblastic proliferation, differentiation, are promoted bone shape
Into showing excellent synosteosis, self-bone grafting and osteoconductive, be a kind of comparatively ideal hard tissue substituting material.But deficiency
Place is that hydroxyapatite (hydroxyapatite, HA) bioceramic mechanical property is poor, it is impossible to bears larger tissue and bears
Lotus, more can not be separately as planting body application, thus many scholars are attached to pure titanium or zirconium oxide (ZrO as coating2)
Ceramic implant surface, so as to improve the biology performance of planting body.But due to HA and the thermal coefficient of expansion of pure titanium or zirconium oxide
Difference is larger, and especially when sintering adhesion, interface produces larger thermal stress, and both cause HA to come off with reference to insecure
Or cracking causes plantation to fail.
The content of the invention
It is an object of the invention to provide a kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material,
This method is prepared from pure zirconia end continuous transition to the function-graded material of pure n-HA ceramic ends using graded composite technology
(functionally gradient materials, FGM), makes material both have the excellent mechanical performance of zirconium oxide, has again
Biology performance good n-HA, simultaneously because the consecutive variations of inter-level, eliminate the macroscopic interface in two kinds of materials, keep away
N-HA is exempted from from ZrO2Surface comes off.
Its concrete technical scheme is：
A kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material, comprises the following steps：
(1) function-graded material powder preparation
1) stabilized with yttrium oxide nanometer Zr02Powder preparation：The polyvinyl alcohol (PVA) of volume parts 1% is added to 3mol%
In the nano zirconium oxide powder (3YSZ-n) of stabilized nano yttrium oxide.Zr02For tetragonal, particle diameter 30-50nm, purity 99%；Receive
Rice yittrium oxide particle diameter 40nm, purity 99.5%.
2) prepared by porous n-HA powders：The PVA of volume parts 1% is added in n-HA powders, adds and accounts for cumulative volume
10%vol carbon nano powders, ball milling and sonic oscillation are well mixed.N-HA particle diameter 20-40nm, purity 99%；PVA particle diameter 40nm,
Purity 99.5%.
3) prepared by each gradient layer powder：Preliminary experiment and theory analysis confirm that totality n-HA contents are with ladder in functionally gradient material (FGM)
Spend index p increase and reduce, so that be conducive to the raising of material mechanical performance, but with p increase, each adjacent layer thermal expansion
The difference of coefficient is increasing, and its mechanical property declines therewith, therefore, this experiment set p scope as 2.0,2.5,3.0,
3.5, n=3,5,7.Volume parts f (x)=(x/n) of n-HA in every layer is calculated according to formulap× f (s), will be calculated respectively
N-HA be added in 3YSZ and add the PVA of volume parts 1%, be put into ball mill and ultrasonator and be sufficiently mixed standby
With.
4) it is grouped：Design sample (powder) gross thickness D=50mm, according to zirconia layer D1The difference of thickness is divided into A, B, C
Three big groups, wherein A groups D1=40mm, D2=10mm, B group D1=30mm, D2=20mm, C group D1=20mm, D2=30mm；According to
Number of plies n difference, A groups are divided into A again1、A2、A3Group, B component is BI、B2、B3Group, component C is C1、C2、C3Group.Every group of each 45 sample
Product.
(2) green compact test material preparation：In a diameter of 30mm cylinder-shaped steels molding jig, by design and result of calculation, add first
Enter 3YSZ-n powders, then be separately added into gradient layer, be eventually adding between porous n-HA powders, two kinds of powders with the fast molten films of PVA
It is separated by.More than 25 DEG C, (Film Fractionation temperature) pressurizes into green compact test specimen with testing machine with 250Mpa pressure perpendiculars at room temperature.
(3) test specimen is sintered：9 groups of sintering temperatures are set, from 1300 DEG C to 1700 DEG C, 50 DEG C are differed between two adjacent groups.Will examination
Part is respectively put into setting constant-pressure and high-temperature sintering furnace, is to slowly warm up to 300 DEG C of insulation 2h, then rises to design temperature insulation 2h, with
Stove is cooled to room temperature and takes out standby.
(4) test specimen Mechanics Performance Testing：Cylindric test specimen after sintering is machined to 25mm × 5mm with low speed accurate cutting
× 5mm testing bars, for mechanics properties testing.
1) shear strength：Detect different gradient layer interface shear bolt nails respectively with universal material test machine,
Method is loading head contact test specimen bonding part side surface, and shear rate 1mm/min applies and is gradually incremented by vertical to power, to bonding
Face, which is separated, or test specimen is broken stops, and records maximum shear force value, calculation formula：Material shear strength (MPa)=shearing force
(N)/bond area (mm2)。
2) bending strength：Test 3 bending strengths, loading velocity 0.5mm/min, reinforcing to sample fracture, calculation formula
(MPa):δ=3PL/2bh2。
3) fracture toughness：Fracture toughness measure is carried out with indentation method.Surface of test piece is polished to mirror-like, imposes 5kg load,
Continue 15s, test 10 points, fracture toughness calculation formula：Kic=0.0232Pc-3/2。
4) hardness：Indentation method measures Vickers hardness, and each layer is polished smooth and is polished to minute surface.Load 5kg, continues 15s, public
Formula：Hv=0.01854P/ (2a)2(Gpa)。
(5) surface topography is mutually detected with thing：With stereomicroscope observation interfacial fracture type；RXD is to sample fault interface
And the observation of surface layer surface row collection of illustrative plates, interface and Surface Phases are determined, its sintering reaction and reaction product is analyzed.SME is observed
Fault interface and surface microscopic topographic, determine grain size and distribution and the rule varied with temperature,
Data processing
Using SAS6.13 editions statistical analysis softwares, statistical analysis is carried out to data.To variable normal state and the money of variance together
Material carries out one-way analysis of variance and comparing two-by-two using multiple sample averages.With α=0.05 for significance test level.
Preferably, oxidation zirconium base nanometer hydroxyapatite function-graded material below scheme and parameter be mechanical property most
It is good, and Surface Characterization is n-HA and its derivative bata-tricalcium phosphate (β-TCP)：1st, material gradient is designed：Intermediate layer (bottom) is
Add volume parts 1%PVA 3YSZ-n powders, thickness=30mm, gradient layer powder thickness=20mm, gradient index=2, ladder
The number of plies=5 are spent, per thickness degree=4mm；Gradient layer is 3YSZ-n powders and n-HA powder mixtures, mixed proportion (volume ratio) point
Not Wei first layer 3YSZ-n account for 96%, n-HA and account for 4%, second layer 3YSZ-n accounts for 84%, n-HA and accounts for 16%, and third layer 3YSZ-n is accounted for
64%, n-HA account for 36%, and the 4th layer of 3YSZ-n accounts for 36%, n-HA and account for 64%, and layer 5 is that superficial layer is 100%n-HA, every layer
Between be separated by with the fast molten films of PVA.The PVA that volume parts are 1% is added in every layer, layer 5 adds 10%vol and received in addition
Rice powdered carbon.2nd, made in the powder testing machine that will be added at room temperature in columnar mould more than 25 DEG C with the pressurization of 250Mpa pressure perpendiculars
Into base substrate；3rd, base substrate is put into constant-pressure and high-temperature sintering furnace, is to slowly warm up to 300 DEG C of insulation 2h, then rise to design temperature 1400
DEG C -1450 DEG C, 2h is incubated, room temperature taking-up is cooled to the furnace, prepared by the new material completes.
Compared with prior art, beneficial effects of the present invention：
Present invention application graded composite technology, prepares oxidation zirconium base nanometer hydroxyapatite function-graded material, with pure oxygen
Change zirconium is matrix, and surface is function-graded material ceramic pure porous n-HA, and the design had both given full play to the performance of two kinds of materials
Advantage, makes to produce between the two and firmly mechanically and chemically combines again, thus prepare machinery and biology performance all reach will
The bioactivity hard tissue substituting material or planting body asked, and be the novel oxidized zirconium base nano-hydroxyapatite biological gradient work(
Design, preparation and the clinical practice of energy material provide theoretical and experimental basis.
Present invention application functionally gradient material (FGM) complex technique, designs and produces a kind of oxidation zirconium base nanometer hydroxyapatite gradient function
Material, its intermediate layer is with ZrO2It is around gradient layer structure, n-HA contents change in gradient in each layer for mechanics supporting region.
Material powder is mixed in the ratio after calculating using direct completion method, successively filling is allowed to after distribution gradient, dry pressing
Functionally gradient material (FGM) sample is made in high temperature sintering.For ease of detection, this is designed as unidirectional graded.
Beneficial effects of the present invention are embodied in several aspects
(1) it is that sclerous tissues's defect and planting body reparation provide new function-graded material：This material takes full advantage of n-
Biocompatibility, biological activity and bio-inert material ZrO good HA2The high advantage of mechanical strength, have stronger reality
With property and theory significance.
(2) graded composite technology is applied by n-HA and ZrO2Organically combined by high temperature sintering：ZrO2For biologically inert material
Material, changes with excellent mechanical property, but due to lacking bone-inducting active, thus carrying out face coat etc. to it always for many years
Journal of Sex Research.N-HA possesses excellent biocompatibility and biological activity, is in recent years using the n-HA applications being modified as surface
The problem of focus and difficult point come, material falls back and absorption, fails to solve always, and graded composite is two with high temperature sintering technique
The combination of person provides new thinking.
(3) function-graded material is applied to the design of planting body or defective bone：Graded composite technology is applied to ZrO2With
Between n-HA, the homogeneity chemical reaction at two interfaces was both realized, the difference of thermal coefficient of expansion between two kinds of materials is balanced again, from
And promote ZrO2Combined with n-HA formation Organics, effectively strengthen ZrO2With n-HA adhesion strength, n-HA is solved from mechanism
The defect for coming off and absorbing too early.According to the technical parameter and theory, needed according to according to clinical sclerous tissues difference, by mould
Design and prepare different artificial bones and artificial tooth root (planting body).
Brief description of the drawings
Fig. 1 is oxidation zirconium base n-HA functionally gradient material (FGM) structure design schematic diagrames, and D is sample full thickness, D in figure1For centre
Layer (bottom) thickness, is 100% zirconium oxide (volume fraction), D2For gradient layer gross thickness, d1...dnFor each Thickness of Gradient Layer, its
Middle dnFor superficial layer, its n-HA content (f (s)) is 100% (volume fraction)；
Fig. 2 is the Technology Roadmap of the present invention.
Embodiment
Technical scheme is described in more detail with specific embodiment below in conjunction with the accompanying drawings.
As shown in Figure 1 and Figure 2, a kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material, including with
Lower step：
(1) function-graded material powder preparation
1) stabilized with yttrium oxide nanometer Zr02Powder preparation：The polyvinyl alcohol (PVA) of volume parts 1% is added to 3mol%
In the nano zirconium oxide powder (3YSZ-n) of stabilized nano yttrium oxide.Zr02For tetragonal, particle diameter 30-50nm, purity 99%；Receive
Rice yittrium oxide particle diameter 40nm, purity 99.5%.
2) prepared by porous n-HA powders：The PVA of volume parts 1% is added in n-HA powders, adds and accounts for cumulative volume
10%vol carbon nano powders, ball milling and sonic oscillation are well mixed.N-HA particle diameter 20-40nm, purity 99%；PVA particle diameter 40nm,
Purity 99.5%.
3) prepared by each gradient layer powder：Preliminary experiment and theory analysis confirm that totality n-HA contents are with ladder in functionally gradient material (FGM)
Spend index p increase and reduce, so that be conducive to the raising of material mechanical performance, but with p increase, each adjacent layer thermal expansion
The difference of coefficient is increasing, and its mechanical property declines therewith, therefore, this experiment set p scope as 2.0,2.5,3.0,
3.5, n=3,5,7.Volume parts f (x)=(x/n) of n-HA in every layer is calculated according to formulap× f (s), will be calculated respectively
N-HA be added in 3YSZ and add the PVA of volume parts 1%, be put into ball mill and ultrasonator and be sufficiently mixed standby
With.
4) it is grouped：Design sample (powder) gross thickness D=50mm, according to zirconia layer D1The difference of thickness is divided into A, B, C
Three big groups, wherein A groups D1=40mm, D2=10mm, B group D1=30mm, D2=20mm, C group D1=20mm, D2=30mm；According to
Number of plies n difference, A groups are divided into A again1、A2、A3Group, B component is BI、B2、B3Group, component C is C1、C2、C3Group.Every group of each 45 sample
Product.
(2) green compact test material preparation：In a diameter of 30mm cylinder-shaped steels molding jig, by design and result of calculation, add first
Enter 3YSZ-n powders, then be separately added into gradient layer, be eventually adding between porous n-HA powders, two kinds of powders with the fast molten films of PVA
It is separated by.More than 25 DEG C, (Film Fractionation temperature) pressurizes into green compact test specimen with testing machine with 250Mpa pressure perpendiculars at room temperature.
(3) test specimen is sintered：9 groups of sintering temperatures are set, from 1300 DEG C to 1700 DEG C, 50 DEG C are differed between two adjacent groups.Will examination
Part is respectively put into setting constant-pressure and high-temperature sintering furnace, is to slowly warm up to 300 DEG C of insulation 2h, then rises to design temperature insulation 2h, with
Stove is cooled to room temperature and takes out standby.
(4) test specimen Mechanics Performance Testing：Cylindric test specimen after sintering is machined to 25mm × 5mm with low speed accurate cutting
× 5mm testing bars, for mechanics properties testing.
1) shear strength：Detect different gradient layer interface shear bolt nails respectively with universal material test machine,
Method is loading head contact test specimen bonding part side surface, and shear rate 1mm/min applies and is gradually incremented by vertical to power, to bonding
Face, which is separated, or test specimen is broken stops, and records maximum shear force value, calculation formula：Material shear strength (MPa)=shearing force
(N)/bond area (mm2)。
2) bending strength：Test 3 bending strengths, loading velocity 0.5mm/min, reinforcing to sample fracture, calculation formula
(MPa):δ=3PL/2bh2。
3) fracture toughness：Fracture toughness measure is carried out with indentation method.Surface of test piece is polished to mirror-like, imposes 5kg load,
Continue 15s, test 10 points, fracture toughness calculation formula：Kic=0.0232Pc-3/2。
4) hardness：Indentation method measures Vickers hardness, and each layer is polished smooth and is polished to minute surface.Load 5kg, continues 15s, public
Formula：Hv=0.01854P/ (2a)2(Gpa)。
(5) surface topography is mutually detected with thing：With stereomicroscope observation interfacial fracture type；RXD is to sample fault interface
And the observation of surface layer surface row collection of illustrative plates, interface and Surface Phases are determined, its sintering reaction and reaction product is analyzed.SME is observed
Fault interface and surface microscopic topographic, determine grain size and distribution and the rule varied with temperature,
Data processing
Using SAS6.13 editions statistical analysis softwares, statistical analysis is carried out to data.To variable normal state and the money of variance together
Material carries out one-way analysis of variance and comparing two-by-two using multiple sample averages.With α=0.05 for significance test level.
It is that mechanical property is optimal to aoxidize embodiment and parameter below zirconium base nanometer hydroxyapatite function-graded material,
And Surface Characterization is n-HA and its derivative bata-tricalcium phosphate (β-TCP), bone tissue replacement or the mechanical property of planting body are met
It is required that.
1st, material gradient is designed：Intermediate layer (bottom) for addition volume parts 1%PVA 3YSZ-n powders, thickness=
30mm, gradient layer powder thickness=20mm, gradient index=2, the gradient number of plies=5, per thickness degree=4mm；Gradient layer is 3YSZ-
N powders and n-HA powder mixtures, mixed proportion (volume ratio) are respectively that first layer 3YSZ-n accounts for 96%, n-HA and accounts for 4%, second
Layer 3YSZ-n accounts for 84%, n-HA and accounts for 16%, and third layer 3YSZ-n accounts for 64%, n-HA and accounts for 36%, and the 4th layer of 3YSZ-n accounts for 36%, n-
HA accounts for 64%, and layer 5 is that superficial layer is that with PVA, molten film is separated by soon between 100%n-HA, every layer.Volume is added in every layer
Number is 1% PVA, and layer 5 adds 10%vol carbon nano powders in addition.
2nd, in the powder testing machine that will be added at room temperature in columnar mould more than 25 DEG C with the pressurization of 250Mpa pressure perpendiculars
Base substrate is made；
3rd, base substrate is put into constant-pressure and high-temperature sintering furnace, is to slowly warm up to 300 DEG C of insulation 2h, then rise to design temperature 1400
DEG C -1450 DEG C, 2h is incubated, is cooled to the furnace standby after room temperature is taken out.
The foregoing is only a preferred embodiment of the present invention, protection scope of the present invention not limited to this, any ripe
Those skilled in the art are known in the technical scope of present disclosure, the letter for the technical scheme that can be become apparent to
Altered or equivalence replacement are each fallen within protection scope of the present invention.
Claims (1)
1. a kind of preparation method for aoxidizing zirconium base nanometer hydroxyapatite function-graded material, it is characterised in that including following step
Suddenly：
(1) function-graded material powder preparation
1) stabilized with yttrium oxide nanometer Zr02Powder preparation：Addition volume parts 1%PVA 3mol% stabilized nano yttrium oxides are received
Rice Zirconium powder 3YSZ-n；Zr02Tetragonal, particle diameter 30-50nm, purity 99%；Nano yttrium oxide particle diameter 40nm, purity
99.5%；PVA particle diameter 40nm, purity 99.5%；
2) prepared by porous n-HA powders：The PVA of volume parts 1% is added in n-HA powders, adds and accounts for cumulative volume 10%
Vol carbon nano powders, ball milling and sonic oscillation are well mixed；N-HA particle diameter 20-40nm, purity 99%；PVA particle diameter 40nm, purity
99.5%；
3) prepared by each gradient layer powder：Bottom powder thickness=30mm, gradient layer powder thickness=20mm, gradient index=2, ladder
Spend the number of plies=5, per thickness degree=4mm, volume parts f (x)=(x/n) of n-HA in every layer is calculated according to formulap× f (s), then
As a result it is that first layer 3YSZ-n accounts for 96%, n-HA and accounts for 4%, and second layer 3YSZ-n accounts for 84%, n-HA and accounts for 16%, third layer 3YSZ-
N accounts for 64%, n-HA and accounts for 36%, and the 4th layer of 3YSZ-n accounts for 36%, n-HA and account for 64%, and layer 5 is that superficial layer is 100%n-HA；Often
It is separated by between layer with the fast molten films of PVA；The PVA that volume parts are 1% is added in every layer, layer 5 adds 10%vol in addition
Carbon nano powder, mixture is put into ball mill and ultrasonator respectively be sufficiently mixed it is rear standby；
(2) green compact test material preparation：In a diameter of 30mm cylinder-shaped steels molding jig, by design and result of calculation, it is firstly added
3YSZ-n powders, then gradient layer is separately added into, it is eventually adding between porous n-HA powders, two kinds of powders with the fast molten film phases of PVA
Every；More than 25 DEG C at room temperature, green compact test specimen is pressurizeed into 250Mpa pressure perpendiculars with testing machine；
(3) test specimen is sintered：Sintering temperature is set as 1400 DEG C -1450 DEG C, green compact test specimen is put into setting constant-pressure and high-temperature sintering furnace
In, 300 DEG C of insulation 2h are to slowly warm up to, then design temperature insulation 2h is risen to, cool to room temperature with the furnace and take out standby.
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| CN113929448A (en) * | 2021-11-29 | 2022-01-14 | 西华师范大学 | Calcium phosphate particle with gradient structure and preparation method and preparation device thereof |
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