CN100577858C - Magnetron sputtering method for preparing HA/YSZ/Ti6Al4V gradient bioactive composite material - Google Patents
Magnetron sputtering method for preparing HA/YSZ/Ti6Al4V gradient bioactive composite material Download PDFInfo
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- CN100577858C CN100577858C CN200610161246A CN200610161246A CN100577858C CN 100577858 C CN100577858 C CN 100577858C CN 200610161246 A CN200610161246 A CN 200610161246A CN 200610161246 A CN200610161246 A CN 200610161246A CN 100577858 C CN100577858 C CN 100577858C
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Abstract
The invention discloses a magnetic control sputtering method of HA/YSZ/Ti6Al4V gradient biological active composite material, which comprises the following steps: adding 20-80% YSZ powder in the HA powder; pressing; sintering; making composite target material of HA/YSZ; polishing Ti6Al4V base through gold phase sandpaper; spraying sand on the base surface; etching base through NaOH solution; placing HA target material, composite target material of HA/YSZ and Ti6Al4V base to presputter and clean for 20-40 min; transmitting Ti6Al4V base into main sputtering chamber with vacuum degree at 5*10-1-9*10-1Pa for 2-4h; sampling from main sputtering chamber; disposing in the heat disposing furnace at 300-500 deg. c; insulating 2-4 h.
Description
Technical field
The present invention relates to Biocomposite material bone planting body technology, refer in particular to the method for preparing the gradient Biocomposite material bone planting body of HA/YSZ/Ti6Al4V based on magnetron sputtering method.
Background technology
At titanium alloy (Ti6Al4V) surface preparation hydroxyapatite (HA) bioactive coating or coating planting body, because it combines metal good mechanical performance and HA excellent biological compatibility and biological activity, can make the artificial bone bigger, position easy to wear that bears a heavy burden such as hip joint, knee joint, tooth root, and can be after implant giving birth to body in the short period rapidly with give birth to biological closely combination of body sclerous tissues formation, non-loosening, indeformable, thus hard tissue repair and one of new focus of replacing area research become.Yet the difference of the heat physical properties between metallic matrix and ceramic coating easily causes the deleterious thermal stresses of the inner generation of coating, thereby reduces coating and high base strength, even causes disbonding, has restricted the reparation damaged to bone to a great extent.If with HA and other material (as ZrO
2, TiO
2, bio-vitric (BG) etc.) cooperate, make the gradient cladding material, then can dwindle the difference of the thermal expansivity between coating and the matrix, slow down the thermal stresses of coating inside, improve Bond Strength of Coating.
Patent of invention is " based on magnetron sputtering method preparation (HA+ZrO
2+ Y
2O
3The method of)/Ti6Al4V Biocomposite material bone planting body " (2004, application number 200410065693.9) mainly described the method for preparing individual layer HA compound coating at the Ti6Al4V matrix surface.The application mainly is provided at the method that the Ti6Al4V matrix surface prepares multi-gradient HA biological coating.
Summary of the invention
The purpose of this invention is to provide a kind of based on the method for magnetron sputtering preparation based on Ti6Al4V surface HA/YSZ gradient biological composite coating artificial bone planting body.
The object of the present invention is achieved like this:
1. magnetic control spattering target preparation
Adopt nano level HA powder, vacuum heating-press sintering prepares pure HA target.
In the HA powder, add Y
2O
3Stable ZrO
2Powder (, can directly buy) from market hereinafter to be referred as YSZ, YSZ powder quality percentage composition accounts for 20%～80% of total mass, the HA/YSZ composite granule of configuration heterogeneity, hot pressed sintering prepares the HA/YSZ composite target material.
2.Ti6Al4V matrix surface sandblast alligatoring and activation treatment
The Ti6Al4V matrix sample that the line cutting is obtained polishes with abrasive paper for metallograph, with varigrained silicon carbide matrix surface is carried out sandblast, substrate after the sandblast carries out acid etching earlier, with NaOH solution it is carried out alkali thermal treatment again, thereby obtains the substrate of sandblast alligatoring and activation treatment.
3. magnetron sputtering technique process
HA target, HA/YSZ composite target material and Ti6Al4V matrix are inserted main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 5 * 10
-5～8 * 10
-5Pa carried out pre-sputter clean 20～40 minutes at Sample Room to the Ti6Al4V matrix, and the Ti6Al4V matrix is sent into main sputtering chamber, in main sputtering chamber vacuum tightness to 5 * 10
-1～9 * 10
-1Regulate the sputter of power build-up of luminance during Pa, sputter was taken out sample from main sputtering chamber after 2～4 hours, carried out aftertreatment in heat treatment furnace, 300～500 ℃ of post-processing temperatures, soaking time 2～4 hours.What obtain after the aftertreatment is based on Ti6Al4V surface HA/YSZ gradient biological coating artificial bone planting body.
The present invention compares with existing technology of preparing, and following advantage is arranged:
1, HA/YSZ gradient biological coating and matrix adhesion strength height are greater than 50MPa.
2, the temperature rise of Ti6Al4V matrix is low, and coated component is uniform and stable.
3, HA/YSZ gradient biological coating surface porosity factor 30%～35%, and surperficial HA crystal grain is the needle-like growth distribution, helps the repair and reconstruction of defective bone tissue.
4, cost is lower.Gradient cladding is thinner, and thickness is 20～27um, and used HA powder is less relatively.
Description of drawings
Fig. 1 is the cross-section morphology of the gradient biological composite coating of HA/YSZ/Ti6Al4V
Fig. 2 is the XRD figure spectrum of aftertreatment HA/YSZ/Ti6Al4V gradient biological composite coating
Fig. 3 is the surface topography of the gradient biological composite coating of sputter HA/YSZ/Ti6Al4V
Embodiment
The magnetron sputtering technique preparation is based on Ti6Al4V surface HA/YSZ gradient biological coating artificial bone planting body, and the invention will be further described in conjunction with example now.
(1) magnetron sputtering HA target and HA/YSZ composite target material preparation
Adopt hydrothermal synthesis method to prepare nano level HA powder, take by weighing HA powder 60g, place air dry oven to dry, grinding is sieved.Prepare the HA target with ZRY55 type multifunctional vacuum hot-pressed sintering furnace, hot pressing pressure 5t, 1150 ℃ of hot pressing temperatures, hot pressing atmosphere N
2, furnace cooling behind the pressurize 4h obtains specification and is
Magnetron sputtering HA target.
In the HA powder, add YSZ powder configuration HA/YSZ composite granule respectively, add the YSZ powder quality and account for 20%, 40%, 60%, 80% of composite granule total mass successively, obtain the HA/YSZ composite granule of four kinds of heterogeneities, place air dry oven to dry, grinding is sieved.These four kinds of composite granules are adopted and the same processing parameter hot pressed sintering of HA powder, prepare specification and be
Magnetron sputtering HA/YSZ composite target material.
More than prepared target numbering be respectively: target I:HA-80wt%YSZ; Target II:HA-60wt%YSZ; Target III:HA-40wt%YSZ; Target IV:HA-20wt%YSZ; Target V:100%HA.
(2) Ti6Al4V matrix surface sandblast alligatoring and activation treatment
The Ti6Al4V matrix sample that line cutting is obtained is polished down to 600 orders step by step with abrasive paper for metallograph, is respectively 40 orders, 80 orders, 120 orders, 170 purpose silicon carbide with granularity matrix surface is carried out sandblasting.Substrate after the sandblast is earlier with oxalic acid solution acid etching 30min, place again in the NaOH aqueous solution of 5mol/L, 80 ℃ of water bath heat preservation 10h, take out substrate, clean with deionized water, oven dry is placed in the vacuum furnace, be warming up to 600 ℃, insulation 1h, furnace cooling obtains the substrate of sandblast alligatoring and activation treatment.
(3) magnetron sputtering technique process
HA target, HA/YSZ composite target material and Ti6Al4V matrix are inserted main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 8 * 10
-5Pa carried out pre-sputter clean 30 minutes at Sample Room to the Ti6Al4V matrix, and the Ti6Al4V matrix is sent into main sputtering chamber, when main sputtering chamber vacuum tightness reaches 9 * 10
-1Regulate the sputter of sputtering power build-up of luminance during Pa, target as sputter be in proper order from target I to target V, each target as sputter 0.7 hour, sputter finishes the back and takes out sample from main sputtering chamber, carry out aftertreatment in heat treatment furnace, post-processing temperature is 500 ℃, and soaking time is 3 hours.What obtain after the aftertreatment is based on Ti6Al4V surface HA gradient biological coating artificial bone planting body.
Four groups of case technology schemes of the present invention that table 1 provides.By the magnetron sputtering technique parameter of optimizing, preparing HA gradient biological coating artificial bone planting body through different modes surface-treated Ti6Al4V matrix surface.
The magnetron sputtering technique scheme that table 1 is optimized
| Specimen coding | The matrix surface processing mode | Sputtering power (w) | Matrix and target spacing (mm) | Sputtering atmosphere | Initial depression (Pa) | Sputter vacuum tightness (Pa) | Sputtering time (h) | The atmosphere post-processing temperature (℃) |
| No 1 | 40 order sandblast+activation treatment | 300 | 60 | Ar | 8×10 -5 | 9×10 -1 | 3.5 | 500 |
| No 2 | 80 order sandblast+activation treatment | 300 | 60 | Ar | 8×10 -5 | 9×10 -1 | 3.5 | 500 |
| No 3 | 120 order sandblast+activation treatment | 300 | 60 | Ar | 8×10 -5 | 9×10 -1 | 3.5 | 500 |
| No 4 | 170 order sandblast+activation treatment | 300 | 60 | Ar | 8×10 -5 | 9×10 -1 | 3.5 | 500 |
Above-mentioned HA/YSZ gradient biological coating artificial bone planting body performance characterization is shown in the table 2.
Table 2HA/YSZ gradient biological coating artificial bone planting body performance
Fig. 1 is the cross-section morphology of the gradient biological composite coating of HA/YSZ/Ti6Al4V.The gradient biological composite coating combines closely with the basal body interface place, does not have any pore and crackle and exists.And matrix is carried out surface sand-blasting handles, cause uneven at the interface, thereby form the favorable mechanical interlock at the interface at matrix and gradient biological composite coating.Fig. 3 is the surface topography of the gradient biological composite coating of sputter HA/YSZ/Ti6Al4V, the gradient biological composite coating surface of HA/YSZ/Ti6Al4V is comparatively coarse as can be seen, be roughness, be porous network structure, its pore diameter is about 0.5 μ m～3 μ m, and interstitial surface area accounts for 30%～35%.The microcosmic surface that this structure has increased the gradient biological composite coating greatly amasss, the gradient biological composite coating is increased greatly with the area at freshman bone tissue bonding interface place behind implant into body, for the growth of freshman bone tissue provides condition, thereby improve the synostosis of implant.
Claims (1)
1, magnetron sputtering method prepares the HA/YSZ/Ti6Al4V gradient bioactive composite material, it is characterized in that:
(1) magnetic control spattering target preparation
In the HA powder, add YSZ powder configuration HA/YSZ composite granule respectively, add the YSZ powder quality and account for 20%, 40%, 60%, 80% of composite granule total mass successively, obtain the HA/YSZ composite granule of four kinds of heterogeneities, hot pressed sintering prepares the HA/YSZ composite target material; Be respectively: target I:HA-80wt%YSZ; Target II:HA-60wt%YSZ; Target III:HA-40wt%YSZ; Target IV:HA-20wt%YSZ; Hot pressed sintering prepares target V:100%HA;
(2) Ti6Al4V matrix surface sandblast alligatoring and activation treatment
The Ti6Al4V matrix sample that the line cutting is obtained polishes with abrasive paper for metallograph, with varigrained silicon carbide matrix surface is carried out sandblast, substrate after the sandblast carries out acid etching earlier, with NaOH solution it is carried out alkali thermal treatment again, thereby obtains the substrate of sandblast alligatoring and activation treatment;
(3) magnetron sputtering technique process
HA target, HA/YSZ composite target material and Ti6Al4V matrix are inserted main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 5 * 1
-5～8 * 10
-5Pa carried out pre-sputter clean 20～40 minutes at Sample Room to the Ti6Al4V matrix, and the Ti6Al4V matrix is sent into main sputtering chamber, in main sputtering chamber vacuum tightness to 5 * 10
-1～9 * 10
-1Regulate the sputter of power build-up of luminance during Pa, the sputter of target is in proper order: target 1 forms the gradient biological coating to target V; Sputter was taken out sample from main sputtering chamber after 2～4 hours, carried out aftertreatment in heat treatment furnace, 300～500 ℃ of post-processing temperatures, and soaking time 2～4 hours, what obtain after the aftertreatment is the HA/YSZ/Ti6Al4V gradient bioactive composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233318A (en) * | 2014-09-27 | 2014-12-24 | 浙江大学 | Method for preparing implant surface with multi-scale complex porous structure |
| CN104233318B (en) * | 2014-09-27 | 2017-01-04 | 浙江大学 | A kind of implant surface preparation method of multiple dimensioned porous labyrinth |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101455859B (en) * | 2008-12-19 | 2012-07-11 | 中南大学 | Titanium alloy surface Ti-YSZ-FHA biological gradient active coatings and preparation method thereof |
| CN101455860B (en) * | 2008-12-19 | 2012-07-11 | 中南大学 | Titanium alloy surface TiO2-FHA biological gradient active coating and preparation method thereof |
| CN102584338B (en) * | 2012-02-20 | 2013-08-28 | 西北工业大学 | Preparation method of composite biological coating on surface of carbon/carbon composite material |
| CN104726874B (en) * | 2014-11-10 | 2017-05-10 | 上海景堂医疗器械有限公司 | Titanium surface material with micro-nano grading permeability and preparation method for titanium surface material |
-
2006
- 2006-12-18 CN CN200610161246A patent/CN100577858C/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 磁控溅射技术制备HA/YSZ/PI生物复合材料. 罗东辉，第27页第14-19行，江苏大学. 2006 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233318A (en) * | 2014-09-27 | 2014-12-24 | 浙江大学 | Method for preparing implant surface with multi-scale complex porous structure |
| CN104233318B (en) * | 2014-09-27 | 2017-01-04 | 浙江大学 | A kind of implant surface preparation method of multiple dimensioned porous labyrinth |
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