Synthesis method for tuning shape, exposed crystal face and size of titanium dioxide

Patent metadata

Field	Value
Publication number	US-9505630-B2
Application number	US-201414165482-A
Country	US
Kind code	B2
Filing date	Jan 27, 2014
Priority date	Jul 31, 2013
Publication date	Nov 29, 2016
Grant date	Nov 29, 2016

Abstract

The present invention relates to a method for tuning shape, exposed crystal face and size of titanium dioxide by using inorganic salts and changing pH value of the reaction environment. The present invention changes the shape of titanium dioxide crystal and the exposed face thereof by adding different inorganic salts during the reaction to utilize different alkali metal ions of the inorganic salts and also can change the size of titanium dioxide crystal by tuning different pH value in the reaction. By this synthesis method, the shape and size of titanium dioxide can be tuned for different applications, such as photocatalysis, dye-sensitized solar cells, photolysis of water and other optoelectronic components or materials, to achieve their optimal efficiencies.

First claim

What is claimed is:

1. A synthesis method of octahedral titanium dioxide material with exposed {101} facet, at least comprising:
a. adding a noncrystalline titanium dioxide material to a sodium hydroxide solution for fabricating a mixed solution;
b. a first heating step for heating the mixed solution;
c. filtering step performed after the first heating step for filtering the unreacted sodium hydroxide of the mixed solution;
d. adding a solvent to the mixed solution after the filtering step to fabricate sodium titanium solution as a precursor;
e. adding an inorganic salt material to the precursor, wherein the inorganic salt material is a salt comprising lithium ions;
f. a second heating step performed after the inorganic salt material for heating the precursor to obtain a reactant; and
g. a drying step performed after the second heating step for drying the reactant to fabricate a crystalline titanium dioxide material.

2. The synthesis method according to claim 1 , wherein the first heating step is performed to heat the mixed solution in an atmospheric pressure reflux environment.

3. The synthesis method according to claim 2 , wherein the first heating step is performed at 150° C. and under atmospheric pressure for 48 hours.

4. The synthesis method according to claim 1 , wherein the second heating step further comprising:
tuning the precursor to pH 6, if the size of the crystalline titanium dioxide material will be ranged around 50 nm; or tuning the precursor to pH 9, if the size of the crystalline titanium dioxide material will be ranged around 100 nm.

5. The synthesis method according to claim 4 using a hydrochloric acid solution in tuning the precursor to pH 6.

6. The synthesis method according to claim 1 , wherein the second heating step is performed to heat the precursor in a high pressure environment.

7. The synthesis method according to claim 6 , wherein the second heating step is performed at high pressure and at 200° C. for 20 hours.

8. The synthesis method according to claim 1 , wherein the drying step is performed at 50° C.

9. The synthesis method according to claim 1 , wherein the salt is lithium chloride.

10. A synthesis method of spindle-shaped titanium dioxide material with exposed {301} facet, at least comprising:
a. adding a noncrystalline titanium dioxide material to a sodium hydroxide solution for fabricating a mixed solution;
b. a first heating step for heating the mixed solution;
c. filtering step performed after the first heating step for filtering the unreacted sodium hydroxide of the mixed solution;
d. adding a solvent to the mixed solution after the filtering step to fabricate a titanate salt solution as a precursor;
e. adding an inorganic salt material to the precursor, wherein the inorganic salt material is a salt comprising sodium ions;
f. a second heating step performed after the inorganic salt material for heating the precursor to obtain a reactant; and
g. a drying step performed after the second heating step for drying the reactant to fabricate a crystalline titanium dioxide material.

11. The synthesis method according to claim 10 , wherein the second heating step further comprising:
tuning the precursor to pH 6, if the long axis of the crystalline titanium dioxide material will be ranged around 100-150 nm; or
tuning the precursor to pH 9, if the long axis of the crystalline titanium dioxide material will be ranged around 300-400 nm.

12. The synthesis method according to claim 10 , wherein the salt is sodium chloride.

13. The synthesis method according to claim 10 , wherein the second heating step further comprising:
tuning the precursor to pH 6, if the long axis of the crystalline titanium dioxide material will be ranged around 200-300 nm; or
tuning the precursor to pH 9, if the long axis of the crystalline titanium dioxide material will be ranged around 500 nm.

14. The synthesis method according to claim 10 , wherein the salt is potassium chloride.

15. A synthesis method of needle-like titanium dioxide material with exposed {301} facet at its tip, at least comprising:
a. adding a noncrystalline titanium dioxide material to a sodium hydroxide solution for fabricating a mixed solution;
b. a first heating step for heating the mixed solution;
c. filtering step performed after the first heating step for filtering the unreacted sodium hydroxide of the mixed solution;
d. adding a solvent to the mixed solution after the filtering step to fabricate a titanate salt solution as a precursor;
e. adding an inorganic salt material to the precursor, wherein the inorganic salt material is a salt comprising potassium ions;
f. a second heating step performed after the inorganic salt material for heating the precursor to obtain a reactant; and
g. a drying step performed after the second heating step for drying the reactant to fabricate a crystalline titanium dioxide material.

Assignees

• Nat Univ Tsing Hua

Inventors

• Lee Chi-Young
• Chiu Hsin-Tien
• Yang Min-Han

Classifications

• B01J35/45

  Nanoparticles · CPC title

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J35/77

  Compounds characterised by their crystallite size · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J35/70

  characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00) · CPC title