Titanium or titanium-alloy material with micron-nano coarse-structure surface and preparation method thereof

A rough structure, titanium alloy technology, applied in the direction of surface reaction electrolytic coating, electrolytic coating, coating, etc., can solve problems such as easy to cause local inflammation, large difference in physical properties between coating and matrix, and implant loosening.

Inactive Publication Date: 2014-03-26
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Taking titanium or titanium alloy used as an implant as an example, the roughening treatment methods that have been reported and/or adopted mainly include: a granular coating of about 300 μm is attached to the surface of the titanium material body by sintering, and its main disadvantages are: The sintered coating is thick and unevenly distributed, which will affect its mechanical strength and bonding strength with the tissue when used; the hydroxyapatite powder is sent into the plasma flame to melt and sprayed at high speed on the metal substrate to quickly solidify to form a coating. Therefore, it is difficult to maintain the original composition and lattice structure of hydroxyapatite, and the physical properties of the coating and the substrate are quite different, and the interface stress is concentrated, which reduces the bonding strength with the titanium substrate and is easy to dissolve in a long physiological environment. Absorption le

Method used

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  • Titanium or titanium-alloy material with micron-nano coarse-structure surface and preparation method thereof
  • Titanium or titanium-alloy material with micron-nano coarse-structure surface and preparation method thereof
  • Titanium or titanium-alloy material with micron-nano coarse-structure surface and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] After polishing the surface of pure titanium material with sandpaper of different specifications from 400# to 1200#, chemical polishing method is used to clean the surface with 12wt% HF and 33%HNO 3 After soaking in the aqueous solution for 30 seconds, ultrasonically clean with acetone, ethanol and water for 30 minutes in sequence (ultrasonic power can be adjusted within 100-400W, preferably 250W), and vacuum freeze-dry for 24 hours.

[0027] Then, using a two-electrode system with titanium sheet as the anode and graphite as the cathode, electrochemical anodic oxidation was carried out at 20°C and a voltage of 100V / 2000Hz in an aqueous electrolyte solution containing 0.05wt% HF and 85wt% acetic acid. The distance is 4cm and the time is 1h. The titanium sheet after electrochemical anodic oxidation treatment was ultrasonically cleaned in deionized water for 5 minutes (ultrasonic power can be adjusted within 100-400W, preferably 250W), the electrolyte was cleaned, and stored...

Embodiment 2

[0030] After the surface of the pure titanium sheet is polished (or mechanically polished) with sandpaper in the manner of Example 1, chemically polished with a 3 After soaking in the aqueous solution for 30 seconds, the method of Example 1 was followed by ultrasonic cleaning with acetone, ethanol and water for 30min, and vacuum freeze-drying for 24h.

[0031] Then, using a two-electrode system with titanium sheet as the anode and platinum as the cathode, and using an aqueous solution containing 0.05wt% HF and 85wt% acetic acid as the electrolyte, electrochemical anodic oxidation was carried out at 80°C and a voltage of 100V / 2000Hz. The spacing is 5cm, and the time is 2h. The anodized titanium sheet was ultrasonically cleaned in deionized water for 5 minutes according to the method of Example 1, the electrolyte was cleaned, and stored in absolute ethanol for 48 hours. Also formed on the surface of the titanium sheet as Figure 4 The form is a multiple micro-nano rough struct...

Embodiment 3

[0033] After the surface of the pure titanium material was polished with sandpaper or mechanically polished, it was chemically polished with 15wt% HF and 30% HNO 3 After soaking in the aqueous solution for 30 seconds, the method of Example 1 was followed by ultrasonic cleaning with acetone, ethanol and water for 30min, and vacuum freeze-drying for 24h.

[0034] Then, a two-electrode system with titanium sheet as the anode and graphite as the cathode was used, and an aqueous solution containing 0.5wt% HF and 85wt% acetic acid was used as the electrolyte to perform electrochemical anodic oxidation at 40°C and a voltage of 150V / 2000Hz. The spacing is 5cm, and the time is 4h. The titanium sheet after electrochemical anodic oxidation treatment was ultrasonically cleaned in deionized water for 5 minutes according to the method of Example 1, the electrolyte was cleaned, and stored in absolute ethanol for 48 hours.

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Abstract

The invention relates to a titanium or titanium-alloy material with a micron-nano coarse-structure surface and a preparation method thereof. According to the material, micron-scale concave-convex structures are distributed on the surface of the titanium or titanium-alloy material, and nano-scale spur structures are distributed on the surfaces of the micron-scale concave-convex structures. The preparation method comprises the steps of sanding, polishing and cleaning the surface of the titanium or titanium-alloy material, and then, carrying out electrochemical anodizing in an electrolyte containing hydrofluoric acid and an acid additive, so as to form a microscopic coarse structure, which is formed by multiple micron-nano concave-convex structures, on the surface of the titanium or titanium-alloy material. The material has the advantages that the combination with a titanium substrate is firm, the falling off is difficult, the biological activity, surface area and surface energy are higher, the material can be applied to a wide range of fields of photocatalysts, solar cells, bio-implants and the like, a better effect can be obtained, and the preparation method is low in cost and is simple and convenient in operation.

Description

technical field [0001] The invention relates to a titanium or titanium alloy material with a micron-nano rough surface and a preparation method thereof. Background technique [0002] Titanium and titanium alloys have been used in oral implantology for many years due to their excellent biocompatibility, mechanical properties, and low elastic modulus. However, since titanium and its alloys are biologically inert materials, long-term implantation in the body may reduce the strength of osseointegration and cause the implant to loosen and fall off, eventually leading to the failure of the operation. At present, the surface activation treatment of titanium or its alloys can include roughening and coating. After roughening the surface of titanium (and its alloys) materials, the surface tension and surface energy of titanium can be increased, which can promote the adsorption, differentiation, expansion, and early healing of the interface of osteoblasts, and has achieved good result...

Claims

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Application Information

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IPC IPC(8): C25D11/26
Inventor 张利郭志君李玉宝
Owner SICHUAN UNIV
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