**1.2.2.2 Composition analysis of Ti-O film**

4 Ceramic Coatings – Applications in Engineering

TiNi shape memory ally (SMA) (Ti: 49.3 at%, Ni: 50.7%) was used as the experimental material. A sample's size was 20mm×10mm×1mm. The TiNi SMA samples were ground by degrees with abrasive papers (No. W40-W10). After washed ultrasonically with absolute ethyl alcohol and acetone solutions, the samples were put in absolute ethyl alcohol to await

The experimental media were the self-prepared Ti(SO4)2 solution (PH0.71) of 0.606mg/ml, Hank's solution (making up diluted hydrochloric acid and NaOH solutions into PH7.45) to simulate human body balanced salt solution, and simulated saliva[8] (making up lactic acid

Weighing out 1.0108g of Titanium dioxide (99.9%) pre-burned at 800C for 2h, putting it in a platinum crucible with a platinum cover, adding to 3g of potassium pyrosulfate to melt, then putting it in a beaker of 400ml after taken out and cooled; adding sulphuric acid solution of 200ml, leaching the liquid melt at an electric heater, then taking the platinum crucible out and clearing with water, continuing to heat until to the solution clarify entirely, cooling, moving it into a volumetric flask of 1000ml, diluting to the graduation with deionized water, and finally, shaking the flask to be even, in order to get ready to use. And

2 3 2 4 2 4

NaCl 8g/l + Na HCO 0.35g/l + Na HPO 0.0475g/l + KCl 0.4g/l +KH PO 0.06g/l +

KCNS 0.52g/l + NaHCO 1.25g/l + KCl 1.47g/l + NaH PO 0.19 <sup>3</sup> 2 4 g/l + lactic acid 0.75ml.

A standard trielectrode system was used in the experiment. The device sketch is as shown in figure 1-1. The power supply was DJS-292 type of potentiostat; the reference electrode was saturated calomel electrode (SCE); a TiNi SMA sample was connected with copper wire, its working area was 10mm×10mm, and the non-working area was coated with silica gel; the

Before cathodic-depositing the PH value of the Ti(SO4)2 solution was modified to PH1.2 with 300g/l of KOH solution, adding to 20g/l KNO3. Under this circumstance of that let sample be cathode, at a constant current density of 5mA/cm2 for 4 min of electrodepositing, a layer of Ti-O film was formed on the surface of TiNi SMA. After finished deposition, the samples were exposed to air for drying naturally, then put them

MgCl 6H O 0.10g/l + MgSO 7H O 0.10g/l + CaCl 0.18g/l + Glucose 1g/l.

**1.2 Experimental method** 

for using.

**1.2.1 Experimental materials and media** 

and ammonia water into PH6.13).

The method of self-preparation of Ti(SO4)2:

this Ti concentration was 0.06 mg/ml.

2 2 4 2 2

Hank's solution composition:

Fusayama solution composition:

**1.2.2 Experimental methods** 

**1.2.2.1 Cathodic-electrodeposition of Ti-O film** 

electrolyte was the self-prepared Ti(SO4)2 solution.

in drying oven for 1h at 120 C, and then awaited for use.

The surface of the sample cathodically-electrodeposited for 4 min at 5mA/cm2 was observed with XL30 s-FEG type of scanning electronic microscope (SEM). Ti and Ni contents of Ti-O film were analyzed with Finder 1000 type of energy dispersive spectroscopy (EDS). The elemental composition and valent state of Ti-O film were analyzed with MII type of XPS, in order to analyze the film's depositional effect.

The deposited sample was put in a muffle furnace to experience crystallization treatment (annealling) for 1h at 300C and 450C respectively, furnace heating and cooling. The phase analysis of Ti-O film was with D/max 2000 type of X-ray diffractormeter (XRD).
