1) 1ml TBT + 0.1-0.2ml acac + 5ml(96% EtOH) = 24h at 70C = clear yellowish gel

2) 1ml TBT + 0.4ml acac + 5ml(96% EtOH) = 24h at 70C = clear yellow solution = + 300ml boiling water = white sol

3) 1ml TBT + 0ml acac + 5ml(96% EtOH) = inhomogen white dense precipitate

It is my recent experiment. For Ti(iPrO)4 it could be faster reactions.

Hi, Your question doesn't come with enough information for an answer- you need to specify which chemical precursor your are using precisely and what it is exactly you are trying to make. Then we can help.

I have titanium isopropoxide precursor. I have micelles in aqueous system. Now I want to use micelles as template to prepare nanomaterials.

Hi, Mohammad, Thanks for the info. It's still unclear because I don't follow how you can control hydrolysis in an aqueous system. All you will get is deposition. There is still something missing in your explanation.

As far as I know even adding a little HCl to carry out hydrolysis of titanium teteraisopropoxide (TTIP) precursor you still get the the white precipitate and not Ti metal. Hydrolysis in acidic medium are preferred over neutral or basic medium to produce nano sized TiO2 particles.

Dear Ian, if I control hydrolysis of Ti precursor then I can use micelle as template to prepare TiO2 otherwise rapid hydrolysis produces aggregates and the TIO2 structure becomes irregular. you can have look the following article: Chem. Com 2011, 47, 6921. However, I tried the same procedure but failed to obtain good nanoparticles. Hope understand my point.

Normally you can dissolve titanium isopropoxide in isopropanol, and then slowly drop this solution into water under rigorously stirring, afterward, such solution needs to be heat up at 70-80 oC for certain time with addition of HCl.

Such procedure is for preparing TiO2 sol.

I think this makes good sense, do you have any idea how much isopropanol I should add? Does it possible to work in basic condition?

I have used titanium isopropoxide in the past, but for a different application. One suggestion I have is to make sure that you do not expose the titanium isopropoxide to the air. Even inside of lab, the humidity in the air can start the rapid hydrolysis. I recommend using a syringe to extract the titanium isopropoxide before adding it to anything to minimize the contact with air, and hence moisture.

good luck

The white precipitate usually is amorphous TiO2. As the Ti-valence is +4 in TTIP, you would normally not get any reduction because of the properties (especially the reactivity) of Ti. I agree with Claire that the contact of the precursor with air (especially with moisture) must be avoided, otherwise your precursor will immediately react. We once tried to measure the structure of TTIP using X-ray absorption spectroscopy, but although this is in principle a very easy experiment, it was hard to realize because the TTIP more or less directly starts to react, and it was hard to isolate the TTIP spectra. You may find more information in the following paper: J. Phys. Chem. C 114 (2010) 6228. Furthermore, we also tried to optimize the hydrolysis of TTIP by influencing the sol-gel chemistry, some results were recently published (J. Sol-Gel Sci. Technol. 64 (2012) 27). Major results are that the use of isopropanol dilution is in principle favourable, but you should always add a thermal treatment after the hydrolysis. Furthermore we also plan to perform the hydrolysis at more elevated temperatures to improve crystalline properties, but this work is still in progress!

Good luck, Dirk

Thanks Dirk and weiss, I am using different alcohol to reduce the hydrolysis of Ti precursor. Some of them shows positive results, especially, isopropyl alcohol. When I used it 20 times more than precursor amount, I did not find any precipitation immediately. Now I am trying to find the right composition.

Acetyl acetone or acetic acid (chelates, usually molar ratio alkoxide:chelate 1:1) and 2-propanol as cosolvent.

I used this kind of precursor before, I used Ar to eliminate the air in the bottle. Using this way, you can eliminate the precipitation of Ti(OH)x. Normally, Ti(iOPr) can react easily with water contain in air

BR,

Dear Benjamin,

I think the white precipitate could be Ti(OH)x-->TiOOH and then transform to TiO2.

BR,

Ti(iOPr) reacts with formic/acetic acid forming a complex and it can precipitate if you do not use a solvent (the parental alcohol).

1) 1ml TBT + 0.1-0.2ml acac + 5ml(96% EtOH) = 24h at 70C = clear yellowish gel

2) 1ml TBT + 0.4ml acac + 5ml(96% EtOH) = 24h at 70C = clear yellow solution = + 300ml boiling water = white sol

3) 1ml TBT + 0ml acac + 5ml(96% EtOH) = inhomogen white dense precipitate

It is my recent experiment. For Ti(iPrO)4 it could be faster reactions.

let say i have to prepare 0.5M of precursor which is titanium butoxide, do i have to dilute if with alcohol 1st or use the extract as a diluent?

the titanium itself 2.9M from its reagent bottle.

Is there any way to recover/redissolve into titanium tetraisopropoxide after hydrolysis has occurred?

Hope the attached article helps you.

https://www.sciencedirect.com/science/article/pii/S0921883117304260

How to make titanium butoxide precursor solution? If I want to make a 0.2 M titanium butoxide solution, should I use water as solvent or some alcohol or acid? I have tries with water and it immediately forms white precipitate which I think is Titanium dioxide. I actually want to go for titanium glycolate by reacting titanium butoxide with ethylene glycol. Can someone suggest the correct way of making the precursor solution?

Make the solution inside a glovebox is the better solution, because it reacts with hthe humidty presents in the air.

i had tried to dissolved titanium butoxide with ethanol 95% but the hydrolysis of titanium had occur as the white precipitate was occur. Next i will try to use absolute ethanol and observed the outcome.

Is there any special care (regarding safety) to use dihydroxybis (ammonium lactate) titanium solution?