Method for magnetron sputtering preparation of (HAú½Zro#-[2]ú½Y#-[2]O#-[3])/Ti#-[6]Al#-[4]V bio-based composites endosteal implant

Abstract

Through the process of composite HA+ZrO2+Y2O3 target material preparation, activation of the Ti2Al4V substrate, setting the composite HA+ZrO2+Y2O3 target and the Ti2Al4V substrate separately in main sputtering chamber and the sample chamber, sputtering under reasonably controlled magnetically controlled sputtering parameters, taking out sample and post-treatment in the sample chamber to obtain the artificial bone implant with composite biological film of composite HA+ZrO2+Y2O3 on the Ti2Al4V substrate. Compared with available prepared technology, the present invention has the advantages of high attachment strength of the composite biological HA+ZrO2+Y2O3 film on the substrate, homogeneous and stable film components without decomposition, capability of gradient varying film, 10-30 % porosity of the film surface favorable to the repairing and re-construction of bone tissue, etc.

Description

technical field

[0001] The present invention relates to a kind of preparation method of biocomposite material film bone implant, especially refers to the preparation of magnetron sputtering (HA+ZrO 2 +Y 2 o 3 ) / Ti 6 al 4 V. Methods for Biocomposite Bone Implants. Background technique

[0002] In the repair and reconstruction of bone tissue, hydroxyapatite (referred to as HA or HAP, its molecular formula is Ca 10 (PO 4 ) 6 (OH) 2 ) is the main component of inorganic matter in human bone tissue. It has good biocompatibility and bioactivity, and is considered to be a most potential human implant replacement material. However, its high brittleness limits the scope of application of hydroxyapatite.

[0003] In view of this, HA / metal biocomposite coating materials have been paid attention to because they combine the good mechanical properties of metal and the good biocompatibility and bioactivity of HA. Among them, titanium and its alloy surface sprayed with HA as an art...

Examples

Embodiment 1

[0022] (1) Magnetron sputtering HA target preparation

[0023] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding polyvinyl alcohol solution accounting for 5% by weight and 8% concentration to HA composite powder for granulation, and dry pressing under 110MPa pressure to form a green sheet, and then heat preservation at a temperature of 900°C 3 hours for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ10mm*2mm is obtained.

[0024] (2) Ti6Al4V substrate surface activation treatment

[0025] Use 360 ​​for Ti6Al4V substrate # SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0026] (3) Magnetron sputtering process

[0027] Put the HA composite target and the Ti6Al4V substrate...

Embodiment 2

[0029] (1) Magnetron sputtering HA target preparation

[0030] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding 7% by weight polyvinyl alcohol solution with a concentration of 9% to the HA composite powder for granulation, and dry pressing under a pressure of 130MPa to form a green sheet, and then heat preservation at a temperature of 1000°C 2 hours for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ40mm*2mm is obtained.

[0031] (2) Ti6Al4V substrate surface activation treatment

[0032] Use 360 ​​for Ti6Al4V substrate # SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0033] (3) Magnetron sputtering process

[0034] Put the HA composite target and the Ti6Al4V substrat...

Embodiment 3

[0036] (1) Magnetron sputtering HA target preparation

[0037] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding 9% by weight polyvinyl alcohol solution with a concentration of 11% to the HA composite powder for granulation, and dry-pressing it into a green sheet under a pressure of 140MPa, and then keeping it warm at a temperature of 1150°C 1 hour for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ60mm*3mm is obtained.

[0038] (2) Ti6Al4V substrate surface activation treatment

[0039] Use 360 ​​for Ti6Al4V substrate# SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0040] (3) Magnetron sputtering process

[0041] Put the HA composite target and the Ti6Al4V substrate in...

technical field

[0001] The present invention relates to a kind of preparation method of biocomposite material film bone implant, especially refers to the preparation of magnetron sputtering (HA+ZrO 2 +Y 2 o 3 ) / Ti 6 al 4 V. Methods for Biocomposite Bone Implants. Background technique

[0002] In the repair and reconstruction of bone tissue, hydroxyapatite (referred to as HA or HAP, its molecular formula is Ca 10 (PO 4 ) 6 (OH) 2 ) is the main component of inorganic matter in human bone tissue. It has good biocompatibility and bioactivity, and is considered to be a most potential human implant replacement material. However, its high brittleness limits the scope of application of hydroxyapatite.

[0003] In view of this, HA / metal biocomposite coating materials have been paid attention to because they combine the good mechanical properties of metal and the good biocompatibility and bioactivity of HA. Among them, titanium and its alloy surface sprayed with HA as an art...

Examples

Embodiment 1

[0022] (1) Magnetron sputtering HA target preparation

[0023] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding polyvinyl alcohol solution accounting for 5% by weight and 8% concentration to HA composite powder for granulation, and dry pressing under 110MPa pressure to form a green sheet, and then heat preservation at a temperature of 900°C 3 hours for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ10mm*2mm is obtained.

[0024] (2) Ti6Al4V substrate surface activation treatment

[0025] Use 360 ​​for Ti6Al4V substrate # SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0026] (3) Magnetron sputtering process

[0027] Put the HA composite target and the Ti6Al4V substrate...

Embodiment 2

[0029] (1) Magnetron sputtering HA target preparation

[0030] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding 7% by weight polyvinyl alcohol solution with a concentration of 9% to the HA composite powder for granulation, and dry pressing under a pressure of 130MPa to form a green sheet, and then heat preservation at a temperature of 1000°C 2 hours for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ40mm*2mm is obtained.

[0031] (2) Ti6Al4V substrate surface activation treatment

[0032] Use 360 ​​for Ti6Al4V substrate # SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0033] (3) Magnetron sputtering process

[0034] Put the HA composite target and the Ti6Al4V substrat...

Embodiment 3

[0036] (1) Magnetron sputtering HA target preparation

[0037] Submicron HA+ZrO with a purity of 99.5% was prepared by sol-gel method 2 +Y 2 o 3 Composite powder, adding 9% by weight polyvinyl alcohol solution with a concentration of 11% to the HA composite powder for granulation, and dry-pressing it into a green sheet under a pressure of 140MPa, and then keeping it warm at a temperature of 1150°C 1 hour for debinding and firing. Thus, a magnetron sputtering HA composite target with a size of Φ60mm*3mm is obtained.

[0038] (2) Ti6Al4V substrate surface activation treatment

[0039] Use 360 ​​for Ti6Al4V substrate# SiO 2 Grinding with sandpaper, sandblasting with 40-mesh corundum sand, ultrasonic cleaning in acetone and absolute ethanol solution for 10 minutes, rinsing with deionized water, drying the Ti6Al4V substrate and placing it in a desiccator for later use.

[0040] (3) Magnetron sputtering process

[0041] Put the HA composite target and the Ti6Al4V substrate in...