The nitrogen of Sol^{^_}Gel TiO₂ film changes research

TiO2 Sols Prepared From Ti(O_i_C3H7)4 Were Dip_coated On The Stainless Steel Substrates To Obtain TiO2 Films.

The XRD Confirmed That TiO2 Films Were Converted To Monstoichiometric Titanium Nitride Films Under The Nitriding Temperature About In NH3 Atmosphere.

Keywords: Nitrogen of TiN Film 　 of 　 of Sol_gel 　 Nitridation changes titanium film to have caustic of tall hardness, high melting point, wear-resisting to reach anti-corrosive wait for good performance, its regard wear-resisting as caustic, anti-corrosive coating and diffuse obstacle layer, use extensively at the industrial domain such as mechanical, electron, aerospace; At the same time because its are beautiful beautiful golden colour and lustre, also be used as material of copy gold coating widely. Current, the method of preparation TiN film is very much, the gas phase method such as traditional PVD and CVD all but deposit TiN is filmy. The TiN film that these methods get is fiber brilliant more or columnar brilliant, the structure is compact, very comfortable operable Yu Dao provides coating and adornment coating. Photograph of fluid of have the aid of grows but the compound of preparation titanium, pass follow-up processing next, also can get TiN film, the porous nitrogen that can get gas phase method is generated hard especially converts titanium film. Seyferth [1] ever from Ti(NR2) go out with the preparation in the benzene solution of R ′ NH2 get together amino titanium, get together amino titanium heats to be TiN to the change when ℃ of 1 000 in NH3. Because this kind of method used the benzene that has a harm to the environment, its application is restricted. But in the preparation that converts titanium film in nitrogen, if choose reaction course reasonably, can get pair of environmental hurtless technology, sol - gel law can solve this problem well. Sol - gel law is the hydrolyze that passes compound in the solution of metallic organic compound, aggregate, make solution into contain metallic oxide or hydroxide corpuscular collosol, the gelation that further reaction makes. If heat gel again, can make pottery and porcelain of the glass that be not brilliant, much brilliant wait. Sol - gel process has its original advantage in preparation film respect, its make velar technology compare CVD, the method such as PVD is simple, also do not have special demand to equipment, dipping process or method of divide evenly glue are used below normal temperature can preparation goes out have very the film of high quality, and do not suffer by the limitation of the dimension of besmear material surface, appearance. Sol - gel law and traditional gas phase method (CVD, what PVD) differs is, this law is oxidize content come out through fluid photograph deposit, can fall in inferior temperature direct or make finished product secondhand, this caused extensive attention in chemical industry and electronic industry. Through sol - the coating of gel process preparation has structure of much smaller hole, it is the mixture structure of the condition that be not brilliant and brilliant condition commonly. Because form the grain dimension of coating material to reduce, make the rate that crystal boundary constituent holds whole data rises (amount to 50% or taller) , cause the mutation of material property thereby. Be based on afore-mentioned reasons, explore pair of collosol - the coating that gel process obtains undertakes nitrogen changes processing is a kind of beneficial attempt. The article uses Sol_gel process, use hurtless reactant to make TiO2 film, recycle nitrogen changes processing to make porous TiN film. 1 test test uses titanium acid fourth ester (TIP) is collosol of precursory content preparation. Mix TIP and the in part that want anhydrous alcohol equably first (the Maerbi of alcohol gross and TIP is 4) ; Mix the hydrochloric acid of 1% and the alcohol photograph that remain again, the Maerbi of water and TIP is 4; Add alcohol dissolve droplet in the TIP alcohol solution of acuteness agitate, in the agitate below room temperature this solution 30 Min makes TIP sufficient hydrolysis. Use dipping process to be in stainless steel and film of hard alloy surface. Matrix is cleaned through ultrasonic, reoccupy synthetic detergent and acetone go fat; Next matrix immerge in the collosol of sufficient hydrolyze, with 0.

The speed upend of 15 Mm/s carries matrix pull; After dry below room temperature 10 Min, heat the matrix after besmear Fu to 500 ℃ inside furnace of vacuum of DEGUSSA A6 VSL10/18, connect nitrogen to regard protection as atmosphere, heat preservation 10 Min. Repeat afore-mentioned measure 10 times, can obtain the TiO2 coating with thick M of μ agreement 1. Put the matrix of film of besmear Fu TiO2 into vacuum undertake nitrogen is changed inside furnace. Turn the result to compare nitrogen, nitrogen changes gas to pick NH3 and N2 gas respectively. Maintain aeriform discharge to be 300 ML/min about, with 100 ℃ / the rate-of-rise of air temperature of Min heats. Heat to 900 ℃ and heat preservation 60 Min, cool next room temperature. The TiO2 film after be being changed to nitrogen undertakes XRD is analysed, comparative TiO2 and TiN brilliant the diffractive intensity of diagnostic diffractive peak, undertake qualitative analysis to filmy composition thereby. 2 tests result and assaying make clear, change mood for nitrogen with tall purity nitrogen, when nitrogen changes temperature to achieve ℃ of 1 100, how was the colour of coating changed, titanium feature diffractive peak is changed to appear without nitrogen on XRD diffractive a collection of illustrative plates (graph 1) , but can see TiO2 brilliant model change. Mine of titanium of brilliant of the TiO2 when 900 ℃ Yourui transforms gradually for rutile; When ℃ of 1 100, tiO2 total change is rutile brilliant model. Graph 1 　 TiO2 in the Cong Ruitai in N2 atmosphere mine arrives the change Fig of rutile.

1 　 Conversion Of TiO2 From Anatase To Rutile In N2 AtmosphereIR: The diffractive peak intensity of acute titanium mine; IA: The diffractive peak intensity of rutile. When changing mood for nitrogen with NH3, the film that converts temperature to get through different to be in nitrogen undertakes XRD is analysed (graph 2) , can see different nitrogen changes temperature to have very big effect to filmy composition. Graph the 2 200 features that change the TiN below temperature in different nitrogen are diffractive the diffractive intensity Fig of the line.

Nitrogen of 2 　 Diffraction Intensity Of 200 Characteristicdiffracted Ray Of TiN At Differentnitriding Temperatures changes mood: NH3(is industrial) ; Discharge: Temperature of 300 ML/min 　 changes the effect to have main effect to nitrogen, different nitrogen changes the result that temperature gets to have very big difference. When nitrogen changes temperature to be 800 ℃ , the color of coating begins to produce change, from the primitive colour of gel film change is bright gray; A dark blue appears when 850 ℃ ; After 1h of heat preservation of 900 ℃ , the color of coating turns into golden color. The chemical reaction equation with the usable and the following course that nitrogen changes TiO2 gel film will express: TiOx may be TiO here, the oxidation titanium composition of Ti2O3 or other form. The TiO2 that have the aid of of 3 last words gets without the Sol_gel process of social effects of pollution is filmy, classics nitrogen changes processing to be able to transform for porous TiN film. Experiment discovery, NH3 compares N2 more the nitrogen that is helpful for TiO2 film is changed. Nitrogen changes a course in, it is certain to be in warm up below speed, the choice that nitrogen influences temperature is crucial, temperature crosses small conference to make nitrogen changes reaction undertake slow. CNC Milling CNC Machining