Preparation method of porous biological activity ceramic film on surface of porous pure titanium or titanium alloy with lattice structure and application thereof

A technology of bioactive ceramics and lattice structure, applied in the direction of surface reaction electrolytic coating, electrolytic coating, coating, etc., to achieve the effect of good combination, high biological activity and uniform thickness

Active Publication Date: 2017-05-17

INST OF METAL RESEARCH - CHINESE ACAD OF SCI

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AI-Extracted Technical Summary

Problems solved by technology

[0007] At present, micro-arc oxidation is limited to the film preparation of titanium alloy bulk materials. For porous materials, especially titanium and titanium alloys wi...

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Abstract

The invention discloses a preparation method of a porous biological activity ceramic film on a surface of a porous pure titanium or titanium alloy with a lattice structure and application thereof, and belongs to the technical field of metal surface treatment. The method comprises chemical polishing, preparation of a prefabricated oxide film under direct-current voltage, and preparation of the porous biological activity ceramic film under square wave pulse voltage. The chemical polishing is a chemical acid washing method. The oxide film prefabrication is a low-voltage direct-current anodic oxidation method; and a porous biologic activity functional ceramic layer adopts a micro arc oxidation preparation method. The ceramic layer obtained by the method is firm in combination with a basal body, has a micron-size cellular structure on the surface, can singly serve as a biologic functional coating layer, and can be subsequently treated to prepare a composite functional coating layer higher in corrosion resistance, wear resistance, biologic activity and bacteria resistance. An interbody fusion cage for the field of orthopedics or an implant for the field of dentistry manufactured based on the method shortens the synostosis time of the implant body.

Application Domain

Surface reaction electrolytic coatingProsthesis

Technology Topic

Micro arc oxidationAnodic oxidation +21

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Examples

Experimental program(3)

Example Embodiment

[0038] Example 1

[0039] 1. Material preparation: using electron beam molten metal forming technology to prepare Ti-6Al-4V titanium alloy with a porosity of 50% and a porous lattice structure ( figure 1 (a)).

[0040] 2. Chemical pickling:

[0041] The composition of the pickling solution is: 40% (volume concentration) HF 2ml/L, 70% (volume concentration) HNO 3 5ml/L, citric acid 5g/L, slow-release agent is o-nitrophenol, and the rest is water.

[0042] Pickling solution temperature: room temperature, treatment time 20 seconds, immediately after taking it out, rinse with tap water for 1 to 2 minutes, and then rinse with deionized water for 1 to 2 minutes.

[0043] 3. Preparation of prefabricated anodic oxide film:

[0044] Electrolyte composition: sodium dihydrogen phosphate with a concentration of 30g/L, sodium oxalate with a concentration of 5g/L, oxalic acid with a concentration of 1g/L, sodium lauryl sulfonate with a concentration of 0.5g/L, the rest is water .

[0045] During the oxide film preparation process, circulating water is used to maintain the electrolyte temperature at 20°C, the power supply mode is DC, and the constant current is 1A/dm. 2 , The final oxidation voltage is 100V, the oxidation time is 5 minutes, the thickness of the non-porous passivation film obtained in this embodiment is about 2μm ( image 3 ).

[0046] 4. Preparation of square wave pulse micro-arc oxide film:

[0047] Electrolyte composition: sodium acetate with a concentration of 10g/L, sodium dihydrogen phosphate with a concentration of 5g/L, sodium carbonate with a concentration of 2g/L, acetic acid with a concentration of 0.5g/L, EDTA with a concentration of 0.5g/L, The rest is water.

[0048] During the preparation of the oxide film, the temperature of the electrolyte is controlled by circulating cooling water to 20°C, the power supply mode is a single forward square wave pulse, and the current density is 3A/dm 2 , The final voltage of forward oxidation is 350V; the oxidation time is 20 minutes, the frequency is 200Hz, the duty cycle is 0.5, the thickness of the oxide film obtained is 10μm, the porosity is 30%, and the surface has a microporous structure (microporous The diameter is 0.5~5μm)( Figure 4 ). The main components of the bioactive ceramic membrane prepared by the present invention are titanium dioxide (anatase) and rutile (rutile). Figure 5 ).

[0049] After drying, a porous biologically active ceramic membrane is obtained on the surface of Ti-6Al-4V titanium alloy with lattice structure ( figure 1 (b)). The relevant performance data of this embodiment is as follows:

[0050] The self-corrosion current density of the ceramic layer in the biological simulation solution is 8.69E-8A/cm 2;

[0051] After cytological testing, compared with the matrix, the surface alkaline phosphatase content determination increased 1.5 times, the osteocalcin secretion detection increased 2 times; the cell proliferation detection increased 2 times; the total protein content increased 3 times.

[0052] The porous bioactive ceramic membrane prepared on the surface of the Ti-6Al-4V titanium alloy implant with the lattice structure by adopting the method has been proved by animal experiments that its osseointegration time is 15 days.

Example Embodiment

[0053] Example 2

[0054] 1. Material preparation: using electron beam molten metal forming technology to prepare Ti-6Al-4V titanium alloy with a porosity of 70% and a porous lattice structure ( figure 1 (c)).

[0055] 2. Chemical pickling:

[0056] The composition of the pickling solution is: 40% (volume concentration) HF 1ml/L, 70% (volume concentration) HNO 3 3ml/L, tartaric acid 3g/L, slow-release agent is p-dinitrophenol, and the rest is water.

[0057] Pickling solution temperature: room temperature, treatment time 20 seconds, immediately after taking it out, rinse with tap water for 1 to 2 minutes, and then rinse with deionized water for 1 to 2 minutes.

[0058] 3. Preparation of prefabricated anodic oxide film:

[0059] Electrolyte composition: sodium dihydrogen phosphate with a concentration of 20g/L, sodium oxalate with a concentration of 8g/L, phosphoric acid with a concentration of 0.5g/L, sodium lauryl sulfonate with a concentration of 0.5g/L, and the rest are water.

[0060] During the preparation of the oxide film, circulating water is used to maintain the electrolyte temperature at 20°C, the power supply mode is DC, and the constant current is 1.5A/dm 2 The final oxidation voltage is 120V, the oxidation time is 8 minutes, and the thickness of the non-porous passivation film obtained in this embodiment is about 2 μm.

[0061] 4. Preparation of square wave pulse micro-arc oxide film:

[0062] Electrolyte composition: sodium acetate with a concentration of 5g/L, sodium dihydrogen phosphate with a concentration of 15g/L, sodium carbonate with a concentration of 1g/L, acetic acid with a concentration of 0.5g/L, EDTA with a concentration of 0.5g/L, The rest is water.

[0063] During the preparation of the oxide film, the temperature of the electrolyte is controlled by circulating cooling water to 20°C, the power supply mode is a single forward square wave pulse, and the current density is 5A/dm 2 , The final forward oxidation voltage is 380V; the oxidation time is 15 minutes, the frequency is 600Hz, the duty cycle is 0.5, the thickness of the oxide film obtained is 12μm, the porosity is 40%, and the surface has a microporous structure (microporous). The diameter is 0.5-5μm).

[0064] After drying, a porous biologically active ceramic membrane is obtained on the surface of Ti-6Al-4V titanium alloy with lattice structure ( figure 1 (d)). The main components of the bioactive ceramic membrane prepared by the invention are titanium dioxide of anatase and rutile. The relevant performance data of this embodiment is as follows:

[0065] The self-corrosion current density of the ceramic layer in the biological simulation solution is 5.72E-8A/cm 2;

[0066] After cytological testing, compared with the matrix, the determination of alkaline phosphatase on the surface was doubled, the secretion of osteocalcin was doubled; the cell proliferation test was doubled; the total protein content was doubled.

[0067] The porous bioactive ceramic membrane prepared on the surface of the Ti-6Al-4V titanium alloy implant with the lattice structure by adopting the method has been proved by animal experiments that its osseointegration time is 15 days.

Example Embodiment

[0068] Example 3

[0069] 1. Material preparation: The electron beam molten metal forming technology is used to prepare a β-titanium alloy with a porosity of 60% and a porous lattice structure.

[0070] 2. Chemical pickling:

[0071] The composition of the pickling solution is: 40% (volume concentration) HF 2ml/L, 70% (volume concentration) HNO 3 7ml/L, malic acid 5g/L, slow-release agent is picric acid, and the rest is water.

[0072] Pickling solution temperature: room temperature, treatment time 20 seconds, immediately after taking it out, rinse with tap water for 1 to 2 minutes, and then rinse with deionized water for 1 to 2 minutes.

[0073] 3. Preparation of prefabricated anodic oxide film:

[0074] Electrolyte composition: sodium dihydrogen phosphate with a concentration of 20 g/L, sodium oxalate with a concentration of 8 g/L, phosphoric acid with a concentration of 2 g/L, sodium lauryl sulfate with a concentration of 0.5 g/L, and the rest is water.

[0075] During the preparation of the oxide film, circulating water is used to maintain the electrolyte temperature at 20°C, the power supply mode is DC, and the constant current is 0.5A/dm 2 The final oxidation voltage is 80V, the oxidation time is 5 minutes, and the thickness of the non-porous passivation film obtained in this embodiment is about 1 μm.

[0076] 4. Square wave pulse micro-arc oxidation film preparation: electrolyte composition: sodium acetate with a concentration of 15g/L, sodium phosphate with a concentration of 10g/L, sodium bicarbonate with a concentration of 1.5g/L, and a concentration of 1g/L acetic acid , Disodium EDTA with a concentration of 0.8g/L, the rest is water.

[0077] During the oxide film preparation process, the electrolyte temperature is controlled by circulating cooling water to 20°C, the power supply mode is a positive square wave pulse, and the current density is 8A/dm 2 , The final forward oxidation voltage is 400V; the oxidation time is 30 minutes, the frequency is 800Hz, the duty cycle is 0.5, the thickness of the oxide film obtained is 18μm, the porosity is 50%, and the surface has a microporous structure (microporous The diameter is 0.5-5μm).

[0078] After drying, a porous bioactive ceramic membrane is obtained on the surface of the β-titanium alloy with a lattice structure. The main components of the bioactive ceramic membrane prepared by the invention are titanium dioxide of anatase and rutile. The relevant performance data of this embodiment is as follows:

[0079] The self-corrosion current density of the ceramic layer in the biological simulation solution is 8.93E-7A/cm 2;

[0080] After cytological testing, compared with the matrix, the determination of alkaline phosphatase on the surface increased 2 times, the detection of osteocalcin secretion increased 1 time; the detection of cell proliferation increased 2 times; the total protein content increased 3 times.

[0081] The porous bioactive ceramic membrane prepared on the surface of the β-titanium alloy implant body with the lattice structure by adopting the method has been proved by animal experiments that its bone integration time is 10 days.

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PUM

Property	Measurement	Unit
Thickness	2.0	µm
Thickness	10.0	µm
Thickness	12.0	µm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Uniform thickness
Well combined

Preparation method of porous biological activity ceramic film on surface of porous pure titanium or titanium alloy with lattice structure and application thereof

A technology of bioactive ceramics and lattice structure, applied in the direction of surface reaction electrolytic coating, electrolytic coating, coating, etc., to achieve the effect of good combination, high biological activity and uniform thickness

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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