Titanium IV Sulfide

TITANIUM (IV) SULFIDE TiCl4 + 2H2S - TiS2 + 4HC1 

Submitted bt Richard C. Hall and John P. Mickel Checked bt Henry F. Holtzclaw, JR.,t and A. GalunI 

The apparatus is shown in Fig. 8. A T-tube A for blending nitrogen and hydrogen sulfide is attached to a drying 

The yield varies with the temperature of the furnace as shown by the following data  

The 27.7 g. obtained at 650° is 55% of the theoretical based upon the titanium(IV) chloride used. Reactions run above 650° would require Vycor tubing. 

The synthesis and transport reactions are carried out in silica or Vycor ampules (Fig. 1). Convenient dimensions are 1.5-2.5 cm i.d. and 10-15 cm long. Titanium sponge (0.96 g, 0.020 mol) and resublimed sulfur (1.34 g, slight excess over 0.04 mol) are placed in the tube along with a weighed 

The reactants are added to the transport tube through a long-stemmed funnel, and the tube is attached to a vacuum line and evacuated at 10 torr. A tube containing the calculated weight of purified iodine is attached to the vacuum line and evacuated. The iodine is then sublimed over into the transport tube, which is then sealed off.  

The transport ampule is placed in a horizontal two-zone furnace in which different temperatures may be maintained at either end of the ampule. Such a furnace may be constructed by bolting together two laboratory tube furnaces end to end or by winding a center-tapped heating element on a refractory 

Crystals are visible in the growth zone within 6 h after the reactant zone reaches 900°. The 900 - 800° gradient is maintained for at least 70 h or until no further transport is evident. The ampule is allowed to cool and is cracked open. 

Caution. Wrap the tube in several layers of cloth before attempting to 

If large crystals are desired, some modifications will promote the growth of a smaller number of large crystals. An ampule of at least 2.5 cm. i.d. is desirable. Before the reaction zone is heated above 800°C., the growth zone is heated to 950°C. for 3 hours to minimize seed sites. The growth zone is then allowed to cool to 800°C., the reaction zone is heated to 900°C., and transport is allowed to proceed at 900 — 800°C. for 70 to 80 hours. The yield of transported crystals depends upon tube dimensions, purity of reactants, and duration of the transport process. 

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Titanium(II) sulfide, TiS titanium(III) sulfide, Ti2S3 titanium(IV) sulfide, TiS2 zirconium sulfide, ZrS2 hafnium selenide, HfSe2 hafnium sulfide, HfS2. 

Thorium oxide sulfide, 4826 Tin(II) sulfide, 4900 Tin(IV) sulfide, 4902 Titanium(IV) sulfide, 4904 Uranium(IV) sulfide, 4905... 

Titanium(IV) sulfide, zirconium (IV) sulfide, hafnium(IV) sulfide, and tin(IV) sulfide constitute a group of isostructural compounds that can be prepared by similar methods. A... 

Germanium(II) sulfide, 4419 Gold(lll) sulfide, 0116 Iron disulfide, 4401 Iron(ll) sulfide, 4400 Iron(lll) sulfide, 4404 Mangancse(II) sulfide, 4706 Manganese(IV) sulfide, 4707 Mercury (II) sulfide, 4607 Molybdcnum(IV) sulfide, 4719 Potassium sulfide, 4670 Rhenium(VII) sulfide, 4891 Ruthcnium(IV) sulfide, 4895 Samarium sulfide, 4899 Silver sulfide, 0026 Sodium disulfide, 4812 Sodium polysulfide, 4813 Sodium sulfide, 4811 Strontium sulfide, 4901 Tantalum(lV) sulfide. 4903 Tetrakis(butylthio)uranium, 3731 Thorium oxide sulfide, 4826 Tin(II) sulfide, 4900 Tin(IV) sulfide, 4902 Titanium(IV) sulfide, 4904 Uranium (IV) sulfide, 4905 Zirconium oxide sulfide, 4827... 

Titanium(IV) sulfide is analyzed for titanium by igniting the sample in air and weighing as the dioxide. The ignition temperature must be held below 800° since titanium tends to form nitrides at higher temperatures. Anal. Calcd. for TiS2 Ti, 42.75. Found Ti, 43.49. The high titanium value is due to the presence of a small quantity of titanium(III) sulfide. 

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Titanium (IV) sulfide TiSg is usually prepared by the reaction of a gaseous mixture of TICI4 and HgS in a red-hot tube. A... 

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