CN1995450A - Magnetron sputtering method for preparing HA/YSZ/polyimide bioactive composite material - Google Patents
Magnetron sputtering method for preparing HA/YSZ/polyimide bioactive composite material Download PDFInfo
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- CN1995450A CN1995450A CN 200610161247 CN200610161247A CN1995450A CN 1995450 A CN1995450 A CN 1995450A CN 200610161247 CN200610161247 CN 200610161247 CN 200610161247 A CN200610161247 A CN 200610161247A CN 1995450 A CN1995450 A CN 1995450A
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Abstract
The invention discloses a making method of biological active composite material of HA/YSZ/polyimide through magnetic control sputtering method, which comprises the following steps: adding 5-40% YSZ powder in the nanometer graded HA powder; making HA/YSZ target material in the vacuum through heat sintering method; cleaning PI base; drying; placing on the base on the carrier of sputtering chamber; extracting the chamber into vacuum; making the pressure below 10-4Pa; activating the surface of PI base surface; placing HA/YSZ target material and PI base in the sputtering chamber; extracting the sputtering chamber into vacuum between 3*10-4 and 5*10-4 Pa; adjusting Ar flow quantity; reducing vacuum degree of sputtering chamber to 2*10-1Pa-1*10-1Pa; adjusting sputtering power to do firing sputter for 6-8h; fetching the sample out of sputtering chamber at 100-200 deg. c; insulating 2-4h; cooling.
Description
Technical field
The present invention relates to the HA bioactive composite material, refer in particular to based on magnetron sputtering technique and prepare HA/YSZ/ polyimide (PI) bioactive composite material bone planting body.
Background technology
Replace and the reparation field in sclerous tissues, correlative study both domestic and external mainly concentrates on medical metal matrix (as Ti or Ti alloy) and goes up deposited hydroxyl apatite (HA) coating, and its preparation technology reaches its maturity.In clinical application, there be " stress shielding " exactly in a shortcoming of metallic matrix, be not matching on the material character of matrix metal and human body bone, mainly be the very big difference of elastic deformation characteristics, cause having compared very big-difference under stress distribution and the state of health around the endosteal implant, exist obvious stress to concentrate and shielding area, bone absorption and osteoporosis will take place in life-time service, cause implant aseptic loosening, reduction of service life." stress shielding " can cause bone resorption, and can avoid with flexible substrate (as polymer matrix film), flexible substrate can be effectively from transplant to the bone transmitted load.The advantage that the HA coating has on the polymer matrix film is that mechanical property can change easily.Therefore, preparation HA coating has very big development potentiality in sclerous tissues's replacement and reparation field on polymeric matrix.
Consider clinical application, between HA and the polymer matrix film preferably tack must at first consider.Therefore, as on metallic matrixes such as titanium alloy, do not launch extensive studies in preparation HA coating on the polymeric matrix.Its technology of preparing also is restricted because of the selection of body material.Y
2O
3Stable ZrO
2(be called for short YSZ, can directly buy from market) has better biocompatibility and biomechanical property, can cooperate with HA and make the HA/YSZ composite granule, and preparation HA/YSZ bioactive coating matrix material is domestic on polyimide (PI) matrix does not appear in the newspapers as yet.
Summary of the invention
The purpose of this invention is to provide a kind of novel hard tissue alternate material of HA/YSZ/PI based on the magnetron sputtering technique preparation.
The object of the present invention is achieved like this:
1. magnetron sputtering HA/YSZ target preparation
Add the YSZ powder in nano level HA powder, the YSZ powder quality accounts for 5%～40% of powder total mass, and vacuum heating-press sintering prepares the HA/YSZ target.
2.PI substrate surface pre-treatment
Substrate vacuumizes through putting into immediately on the Stage microscope of sputtering chamber behind the cleaning, drying, makes air pressure reach 10
-4Below the Pa, the PI substrate surface is carried out activation treatment.
3. magnetron sputtering prepares the HA/YSZ/PI bioactive composite material
HA/YSZ target and PI substrate are inserted sputtering chamber, and sputtering chamber is evacuated to 3 * 10
-5Pa～5 * 10
-5Pa regulates Ar air-flow metered valve, reduces to 2 * 10 in sputtering chamber vacuum tightness
-1Pa～1 * 10
-1Regulate the sputter of sputtering power build-up of luminance during Pa, sputter was taken out sample from sputtering chamber after 6～8 hours, and carried out aftertreatment in heat treatment furnace, and post-processing temperature is 100～200 ℃, is incubated furnace cooling after 2～4 hours.What obtain after the aftertreatment is based on PI surface HA/YSZ biofilm artificial bone planting body.
The present invention compares with existing HA biofilm bone planting body, and following advantage is arranged:
1, the temperature rise of PI substrate is low, and membranous layer ingredient is uniform and stable.
2, film surface presents 15%～35% hole, helps the repair and reconstruction of defective bone tissue.
3, cost is lower.Rete is thinner, and thickness is 4～8 μ m, and used HA powder is less.
4, have good biomechanical property, effectively avoid " stress shielding ".
Description of drawings
Fig. 1 is the XRD figure spectrum of HA/YSZ/PI bioactive coating after the aftertreatment
Fig. 2 is the surface topography of sputter HA/YSZ/PI bioactive coating
Embodiment
The magnetron sputtering technique preparation is based on PI surface HA biofilm artificial bone planting body, and the invention will be further described in conjunction with example now.
(1) magnetron sputtering HA/YSZ target preparation
Adopt sol-gel method to prepare nano level HA powder, get HA powder and YSZ powder and mix, the YSZ powder quality accounts for 5%, 10%, 15% of powder total mass, 20%, 25%, 30%, 35%, 40%, number NO1～NO8 respectively, place air dry oven to dry, grinding is sieved.Prepare the HA/YSZ 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, obtaining specification is the magnetron sputtering HA/YSZ target of 60mm * 5mm.
(2) PI substrate surface pre-treatment
The PI substrate cleans through suds earlier, and the back is put into after the oven dry on the Stage microscope of sputtering chamber with deionized water ultrasonic cleaning 15min, adjusts Stage microscope height (target-matrix spacing), vacuumizes, and makes air pressure reach 10
-5Pa regulates the ECR magnet coil and applies electric current, opens microwave source, adds negative bias to matrix, makes oxygen plasma under the effect of negative bias, quickens to the substrate motion PI substrate surface to be carried out activation treatment, and the negative bias process continues 15min.Processing parameter in this process is as shown in table 1.
Table 1PI matrix surface oxygen plasma pretreatment technology parameter
| Oxygen flow (cm 3/min) | Microwave power (W) | Pre-sputtering bias-voltage (V) | Time (min) | Magnet coil electric current (A) |
| 20 | 800 | 700 | 15 | 60 |
(3) magnetron sputtering prepares the HA/YSZ/PI bioactive composite material
HA/YSZ target and PI substrate are inserted sputtering chamber, and sputtering chamber is evacuated to 4 * 10
-5Pa regulates Ar air-flow metered valve, in sputtering chamber vacuum tightness to 2 * 10
-1Regulate the sputter of sputtering power build-up of luminance during pa, sputter was taken out sample from main sputtering chamber after 7 hours, and carried out aftertreatment in heat treatment furnace, and post-processing temperature is 200 ℃, is incubated furnace cooling after 3 hours.What obtain after the aftertreatment is based on PI surface HA/YSZ biofilm artificial bone planting body.
Eight groups of case technology schemes of the present invention that table 2 provides.Prepare based on PI surface HA biofilm artificial bone planting body by different sputtering powers, substrate and target spacing etc.
Table 2 magnetron sputtering technique scheme
| Specimen coding | Sputtering power (w) | Substrate and target spacing (mm) | Sputtering atmosphere | Initial depression (pa) | Sputter vacuum tightness (pa) | Sputtering time (h) | The atmosphere post-processing temperature (℃) |
| NO 1 | 120 | 50 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| |
120 | 60 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| NO 3 | 140 | 50 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| NO 4 | 140 | 60 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| NO 5 | 160 | 50 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| NO 6 | 160 | 60 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| NO 7 | 180 | 50 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
| |
180 | 60 | Ar | 4×10 -4 | 2×10 -1 | 7 | 200 |
Above-mentioned HA/YSZ/PI biofilm artificial bone planting body performance characterization is shown in the table 3.
Table 3HA/YSZ/PI biofilm artificial bone planting body performance
| Specimen coding | Film thickness | Adhesion strength (Mpa) | FTIR analyzes | The XRD facies analysis | The SEM surface topography is observed | The SEM cross-section morphology is observed | Biocompatibility and resist dissolution |
| NO 1 | 4～5μm | 6～7 | OH - PO 4 3- | HA，YSZ CaO，TCP | 30%～32% 2～5 μ m hole | The interface is in conjunction with comparatively tight | |
| NO | |||||||
| 2 | 4～6μm | 5～7 | OH - PO 4 3- | HA，YSZ CaO，TCP | 30%～35% 3～5 μ m hole | The interface is in conjunction with comparatively tight | Better |
| NO 3 | 4～7μm | 7～8 | OH - PO 4 3- | HA，YSZ CaO，TCP | 27%～30% 1～5 μ m hole | The interface is in conjunction with comparatively tight | Better |
| NO 4 | 4～6μm | 7～8 | OH - PO 4 3- | HA，YSZ CaO，TCP | 29%～33% 2～5 μ m hole | The interface is in conjunction with comparatively tight | Better |
| NO 5 | 5～ |
8～9 | OH - PO 4 3- | HA，YSZ CaO，TCP | 22%～25% 1～5 μ m hole | The interface is in conjunction with tight | Well |
| NO 6 | 5～ |
8～9 | OH - PO 4 3- | HA，YSZ CaO，TCP | 24%～28% 1～5 μ m hole | The interface is in conjunction with tight | Well |
| NO 7 | 6～8μm | 9～12 | OH - PO 4 3- | HA，YSZ CaO，TCP | 18%～20% 1～3 μ m hole | The interface is in conjunction with | Well |
| NO | |||||||
| 8 | 5～8μm | 9～12 | OH - PO 4 3- | HA，YSZ CaO，TCP | 20%～23% 1～4 μ m hole | The interface is in conjunction with tight | Well |
Fig. 2 is the surface topography of sputter HA/YSZ/PI bioactive coating.As can be seen from Figure 2 HA/YSZ/PI biological active coating laminar surface is comparatively coarse, is roughness, is porous network structure, and its pore diameter is about 0.5 μ m～4 μ m, and interstitial surface area accounts for 20%～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 HA/YSZ/ polyimide (PI) bioactive composite material, it is characterized in that:
(1) magnetron sputtering HA/YSZ target preparation
Add the YSZ powder in nano level HA powder, the YSZ powder quality accounts for 5%～40% of powder total mass, and vacuum heating-press sintering prepares the HA/YSZ target;
(2) PI substrate surface pre-treatment
Substrate vacuumizes through putting into immediately on the Stage microscope of sputtering chamber behind the cleaning, drying, makes air pressure reach 10
-4Below the Pa, the PI substrate surface is carried out activation treatment;
(3) magnetron sputtering prepares the HA/YSZ/PI bioactive composite material
HA/YSZ target and PI base material are inserted sputtering chamber, and sputtering chamber is evacuated to 3 * 10
-4～5 * 10
-4Pa regulates the Ar airshed, reduces to 2 * 10 in sputtering chamber vacuum tightness
-1Pa～1 * 10
-1Regulate the sputter of sputtering power build-up of luminance during Pa, sputter was taken out sample from sputtering chamber after 6～8 hours, and in heat treatment furnace, carry out aftertreatment, post-processing temperature is 100～200 ℃, be incubated furnace cooling after 2～4 hours, what obtain after the aftertreatment is based on PI surface HA/YSZ biofilm artificial bone planting body.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610161247 CN1995450A (en) | 2006-12-18 | 2006-12-18 | Magnetron sputtering method for preparing HA/YSZ/polyimide bioactive composite material |
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|---|---|---|---|
| CN 200610161247 CN1995450A (en) | 2006-12-18 | 2006-12-18 | Magnetron sputtering method for preparing HA/YSZ/polyimide bioactive composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112522674A (en) * | 2021-02-18 | 2021-03-19 | 中南大学湘雅医院 | Titanium alloy surface composite coating and preparation method thereof |
| CN114081995A (en) * | 2021-11-30 | 2022-02-25 | 广东工业大学 | Hard tissue repair material with polyimide as matrix and preparation method and application thereof |
-
2006
- 2006-12-18 CN CN 200610161247 patent/CN1995450A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112522674A (en) * | 2021-02-18 | 2021-03-19 | 中南大学湘雅医院 | Titanium alloy surface composite coating and preparation method thereof |
| CN114081995A (en) * | 2021-11-30 | 2022-02-25 | 广东工业大学 | Hard tissue repair material with polyimide as matrix and preparation method and application thereof |
| CN114081995B (en) * | 2021-11-30 | 2022-09-27 | 广东工业大学 | Hard tissue repair material with polyimide as matrix and preparation method and application thereof |
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