Preparation method for doped-element-free black oxide film of titanium surface

A black oxidation, non-doping technology, applied in the direction of surface reaction electrolytic coating, electrolytic coating, coating, etc., can solve the problems that affect the appearance and use of products, easily cause inhalation, percutaneous absorption, and difficult to prepare oxide film layers, etc. , to achieve the effects of low equipment and operating costs, good biocompatibility, and good economic applicability

Active Publication Date: 2018-06-15
博益宁(厦门)医疗器械有限公司 +1
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Problems solved by technology

However, in actual production, it is difficult to prepare a black oxide film layer by means of ordinary direct current.
At the same time, the existing anodic oxidation treatment method in DC voltage mode easily leads to poor compactness of the film layer and many surface defects, which have a certain impact on the color fastness of the black oxide film layer. The corresponding medical titanium and titanium alloy implant products It is easy to change the color to a certain extent during the steam sterilization process of high temperature and humidity, which will affect the appearance and use of the product
[0003] CN101812715B discloses "a black anodizing process for titanium alloy", which uses potassium dichromate K 2 Cr 2 o 7 , manganese sulfate MnSO 4 , blackening agent, ammonium sulfate (NH 4 ) 2 SO 4 , Potassium persulfate K 2 S 2 o 8 , sodium fluoride NaF solution system, the preparation of the black film layer is mainly by adding strong oxidizing chemical reagents such as potassium dichromate and perpotassium sulfate to make the surface electrochemically black, but potassium dichromate And there is a strong carcinogenic oxidant, which is easy to cause inhalation and percutaneous absorption in the actual industrial production process, and has a high risk; at the same time, because the solution system itself is hexavalent chromium, it is easy to cause the oxide film to be mixed in the anodic oxidation process. Assorted hexavalent chromium, the chromium element on the surface of the product may exceed the standard, causing the biocompatibility of the processed product to be unqualified, and it also has a very high risk as an internal plant product
However, in actual use, due to the high loading voltage, high power requirements and long loading time, the equipment cost and processing cost of the micro-arc oxidation power supply are relatively high, which limits the application of the technology to a certain extent. Points are easy to form ablation points and local defects, which have potential risks as products for stress and fatigue applications

Method used

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  • Preparation method for doped-element-free black oxide film of titanium surface
  • Preparation method for doped-element-free black oxide film of titanium surface
  • Preparation method for doped-element-free black oxide film of titanium surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1) Sand blasting treatment: refer to the conventional method, use sand with a certain mesh number to perform sand blasting treatment on the surface of the titanium parts, so that the surface roughness of the titanium parts is Ra≥0.4μm;

[0042] 2) Degreasing and cleaning: Use PWC-401 alkaline cleaning agent to ultrasonically clean the surface of the titanium parts after sandblasting at a cleaning temperature of 60-80 °C for 10-20 minutes to remove machining and cutting oils on the surface of the titanium parts ;

[0043] 3) Pickling: Use a mixed solution of 100-150ml / L hydrofluoric acid (concentration ≥ 40%) and 20-40ml / L nitric acid (concentration 65-68%) to clean the surface of the titanium parts after degreasing and cleaning. Bubbling pickling for 20-30s to remove surface oxides and achieve the purpose of uniform and activating the surface;

[0044] 4) DC anodizing treatment: at room temperature, place the pickled titanium piece in the anolyte, use it as an anode, a...

Embodiment 2

[0051] In this embodiment, the anolyte and the DC anodizing treatment are as follows:

[0052] The anolyte contains 3% formic acid, 2% acetic acid, 1g / 100ml citric acid, 4g / 100ml oxalic acid, 2g / 100ml salicylic acid, 1% hydrochloric acid, 2.5% nitric acid and 0.2g / 100ml manganese sulfate.

[0053] The method of DC anodizing treatment: initial voltage 10V treatment for 1min→15V treatment for 1min→20V treatment for 1min→25V treatment for 1min→30V treatment for 1min→35V treatment for 1min→40V treatment for 1min→45V treatment for 1min→50V treatment for 1min→55V treatment 1min→60V treatment for 1min→65V treatment for 1min→70V treatment for 1min→75V treatment for 1min→80V treatment for 1min→85V treatment for 1min→90V treatment for 1min→95V treatment for 1min→100V treatment for 1min→105V treatment for 1min→110V treatment for 1min→115V treatment for 1min→ 120V treatment for 1min; step-by-step boosting a total of 22 times, the cumulative voltage loading time is 23min.

[0054] All the...

Embodiment 3

[0059] In this embodiment, the anolyte and the DC anodizing treatment are as follows:

[0060] The anolyte contains 5% formic acid, 1% acetic acid, 3g / 100ml citric acid, 5g / 100ml oxalic acid, 1g / 100ml salicylic acid, 3% hydrochloric acid, 3% nitric acid and 0.1g / 100ml manganese sulfate.

[0061] The method of DC anodizing treatment: initial voltage 10V treatment for 2min→20V treatment for 2min→30V treatment for 2min→40V treatment for 2min→50V treatment for 2min→60V treatment for 2min→70V treatment for 2min→80V treatment for 2min→85V treatment for 2min→90V treatment 2min→95V treatment for 2min→100V treatment for 2min→105V treatment for 2min→110V treatment for 2min→120V treatment for 2min; a total of 14 times of step-by-step boosting, and the cumulative voltage loading time was 30min.

[0062] All the other are with embodiment 1.

[0063] After the DC anodizing treatment is completed, a black sample is obtained, that is, a black oxide film without doping other elements is forme...

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Abstract

The invention discloses a preparation method for a doped-element-free black oxide film of a titanium surface. The surface of a titanium part is subjected to sand blasting treatment so that the roughness Ra of the surface can be greater than or equal to 0.4 microns, then degreasing and acid pickling are conducted, and the titanium part subjected to acid pickling is arranged in an anodic electrolyteand used as an anode for direct current anodizing treatment; the anodic electrolyte comprises organic acid and inorganic salt; the direct current anodizing treatment adopts a gradient gradual pressure rise mode; and after treatment is completed, a black sample is obtained, that is, the doped-element-free black oxide film is formed on the surface of the titanium part surface. Through the preparation method, other elements except a matric are not introduced to the surface of the titanium part, and the surface is good in stability, high in color fastness and good in biocompatibility.

Description

technical field [0001] The invention belongs to the field of titanium and titanium alloy surface treatment, and in particular relates to a method for preparing a black oxide film without doping elements on the titanium surface. Background technique [0002] At present, surface coloring on the surface of titanium and alloys is mainly carried out by anodic oxidation. By forming transparent titanium dioxide films with different film thicknesses, different color film layers are formed due to the interference of light. However, it is difficult to prepare a black oxide film layer by means of ordinary direct current in actual production. At the same time, the existing anodic oxidation treatment method in DC voltage mode easily leads to poor compactness of the film layer and many surface defects, which have a certain impact on the color fastness of the black oxide film layer. The corresponding medical titanium and titanium alloy implant products It is easy to change the color to a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26
CPCC25D11/26
Inventor 王老乌陈艳文曾达陈小真
Owner 博益宁(厦门)医疗器械有限公司
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