CN106115638A - The preparation method of a kind of titanium nitride, titanium nitride and application thereof - Google Patents
The preparation method of a kind of titanium nitride, titanium nitride and application thereof Download PDFInfo
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- CN106115638A CN106115638A CN201610461003.4A CN201610461003A CN106115638A CN 106115638 A CN106115638 A CN 106115638A CN 201610461003 A CN201610461003 A CN 201610461003A CN 106115638 A CN106115638 A CN 106115638A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0763—Preparation from titanium, zirconium or hafnium halides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses the preparation method that the invention provides a kind of titanium nitride, described preparation method includes: obtain carbamide presoma；Take CH3CH2OH、TiCl4Solution and described carbamide presoma, described carbamide presoma and described TiCl4Volume ratio be (3～8): 1；By described TiCl4Solution is slowly dropped to described CH3CH2In OH, until described CH3CH2OH and described TiCl4Solution is sufficiently mixed as yellow transparent solution；Measure described carbamide presoma and be slowly added into described mixed described CH3CH2OH and described TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved, stands, make described carbamide presoma and described TiCl4Solution fully reacts, and the jellied mixed solution of shape；The mixed solution of described glue is heated to 750 DEG C～850 DEG C, insulation；Stop heating, and be cooled to room temperature, pulverize, solve the complicated process of preparation of titanium nitride in prior art, cost is high, purity is the highest technical problem.
Description
Technical field
The present invention relates to field of material technology, particularly to preparation method, titanium nitride and the application thereof of a kind of titanium nitride.
Background technology
The chemical property of nitrogen element is highly stable, but under some specific conditions, it can form nitridation with a lot of elements
Thing, in these nitride, transition metal nitride titanium nitride becomes the focus of research both at home and abroad.
The synthesis technique preparing titanium nitride in prior art is more complicated, and the sample specific surface area prepared is less, does not has
Have good micro nano structure, semi-conducting material of the prior art do not expanded well do not become have energy storage and
The material of the application such as conversion.The method of conventional synthesis titanium nitride has metallic titanium powder direct nitridation method, utilizes titanium oxide carbon thermal reduction
Method etc., but metallic titanium powder direct nitridation method easily forms thin film and hinders the carrying out of reaction on titanium surface, and also technics comparing is complicated,
Cost is relatively big, and purity is the highest, and utilizes dioxy to turn to titanium material to generally require the highest sintering temperature through carbon thermal reduction and increase
Preparation cost.
Summary of the invention
The present invention provides the preparation method of a kind of titanium nitride, titanium nitride and application thereof, solves titanium nitride in prior art
Complicated process of preparation, cost is high, purity is the highest technical problem, the preparation technology having reached titanium nitride is simple, low cost, pure
Spend high technique effect.
For solving above-mentioned technical problem, the invention provides the preparation method of a kind of titanium nitride, described preparation method includes:
Obtain carbamide presoma；
Take CH3CH2OH、TiCl4Solution and described carbamide presoma, described carbamide presoma and described TiCl4Volume ratio
For (3～8): 1；
By described TiCl4Solution is slowly dropped to described CH3CH2In OH, until described CH3CH2OH and described TiCl4Solution
It is sufficiently mixed as yellow transparent solution；
Measure described carbamide presoma and be slowly added into described mixed described CH3CH2OH and described TiCl4Solution
In, it is stirred continuously, until described carbamide presoma is completely dissolved, stands, make described carbamide presoma and described TiCl4Solution fills
Divide reaction, and the jellied mixed solution of shape；
The mixed solution of described glue is heated to 750 DEG C～850 DEG C, insulation；
Stop heating, and be cooled to room temperature, pulverize.
Preferably, described CH3CH2OH is specially dehydrated alcohol.
Preferably, described carbamide presoma and described TiCl4Volume ratio be 3:1.
Preferably, described CH3CH2OH and described TiCl4The volume ratio of solution is (4～5): 1.
Preferably, described CH3CH2OH and described TiCl4The volume ratio of solution is 5:1.
Preferably, the described mixed solution to described glue is heated to 750 DEG C～850 DEG C, insulation, particularly as follows:
In a nitrogen atmosphere, being heated by the mixed solution of colloidal in high temperature process furnances, the mixing making described glue is molten
Liquid was heated to 800 DEG C in 4 hours, and was incubated 3 hours.
Preferably, measure described carbamide presoma described in and be slowly added into described mixed described CH3CH2OH and institute
State TiCl4In solution, being stirred continuously, until described carbamide presoma is completely dissolved, stand, described standing is specially and stands 7～8
Hour.
Based on same inventive concept, the application also provides for a kind of titanium nitride, and described titanium nitride is such as claim 1 to 5
Titanium nitride prepared by arbitrary described preparation method.
Based on same inventive concept, the application also provides for the application of a kind of above-mentioned titanium nitride, described titanium nitride is applied
In photo cathode material.
The application has the beneficial effect that:
The application provides the preparation method of a kind of titanium nitride, titanium nitride and application thereof, and described titanium nitride is for make at low temperatures
The titanium nitride with micro nano structure with specific morphology structure of the standby preparation obtained is applied to photo cathode material, cancels
Intermediate storage process is compared to conventional anode material more stable, it is to avoid phenomenon overheated and on fire occurs in battery.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, embodiment will be described below
The accompanying drawing used required in is briefly described, it should be apparent that, the accompanying drawing in describing below is only some of the present invention
Embodiment.
Fig. 1 is the SEM figure of the titanium nitride that the preparation method of the application titanium nitride prepares；
Fig. 2 is the EDS figure of the titanium nitride that the preparation method of the application titanium nitride prepares；
Fig. 3 is the XRD figure of the titanium nitride that the preparation method of the application titanium nitride prepares.
Detailed description of the invention
The embodiment of the present application, by providing the preparation method of a kind of titanium nitride, titanium nitride and application thereof, solves existing skill
The technical problem that the complicated process of preparation of titanium nitride in art, cost are high, purity is the highest, has reached the preparation technology letter of titanium nitride
The technique effect that list, low cost, purity are high..
Technical scheme in the embodiment of the present application is for solving above-mentioned technical problem, and general thought is as follows:
Embodiment one
The application provides the preparation method of a kind of titanium nitride, described preparation method to include:
Step S100, obtains carbamide presoma.
Step S200, takes CH3CH2OH、TiCl4Solution and described carbamide presoma, described carbamide presoma is with described
TiCl4Volume ratio be (3～8): 1；
Concrete, described CH3CH2OH is specially dehydrated alcohol.Described carbamide presoma and described TiCl4Volume ratio be
3:1.Described CH3CH2OH and described TiCl4The volume ratio of solution is (4～5): 1.Preferably, described CH3CH2OH is with described
TiCl4The volume ratio of solution is 5:1.
Step S300, by described TiCl4Solution is slowly dropped to described CH3CH2In OH, until described CH3CH2OH is with described
TiCl4Solution is sufficiently mixed as yellow transparent solution；
Step S400, measures described carbamide presoma and is slowly added into described mixed described CH3CH2OH is with described
TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved, stands, make described carbamide presoma with described
TiCl4Solution fully reacts, and the jellied mixed solution of shape.
Concrete, described in measure described carbamide presoma and be slowly added into described mixed described CH3CH2OH and institute
State TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved, in standing, stands 7～8 hours.
Step S500, is heated to 750 DEG C～850 DEG C to the mixed solution of described glue, insulation；
Concrete, the described mixed solution to described glue is heated to 750 DEG C～850 DEG C, insulation, particularly as follows:
In a nitrogen atmosphere, being heated by the mixed solution of colloidal in high temperature process furnances, the mixing making described glue is molten
Liquid was heated to 800 DEG C in 4 hours, and was incubated 3 hours.
Step S600, stops heating, and is cooled to room temperature, pulverize.
The preparation method of titanium nitride that the application provides, prepares, the nitrogen having obtained micro/nano level simple to operate at low temperatures
Change titanium, and this titanium nitride possesses specific morphology, refers to Fig. 1 to Fig. 3.The preparation method of the titanium nitride that the application provides, solves
The complicated process of preparation of titanium nitride in prior art, the technical problem that cost is high, purity is the highest, reached the preparation of titanium nitride
The technique effect that technique is simple, low cost, purity are high.
Embodiment two
Based on same inventive concept, the application also provides for a kind of titanium nitride, and the preparation method of described titanium nitride includes:
Step S100, obtains carbamide presoma.
Step S200, takes CH3CH2OH、TiCl4Solution and described carbamide presoma, described carbamide presoma is with described
TiCl4Volume ratio be (3～8): 1；
Concrete, described CH3CH2OH is specially dehydrated alcohol.Described carbamide presoma and described TiCl4Volume ratio be
3:1.Described CH3CH2OH and described TiCl4The volume ratio of solution is (4～5): 1.Preferably, described CH3CH2OH is with described
TiCl4The volume ratio of solution is 5:1.
Step S300, by described TiCl4Solution is slowly dropped to described CH3CH2In OH, until described CH3CH2OH is with described
TiCl4Solution is sufficiently mixed as yellow transparent solution；
Step S400, measures described carbamide presoma and is slowly added into described mixed described CH3CH2OH is with described
TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved, stands, make described carbamide presoma with described
TiCl4Solution fully reacts, and the jellied mixed solution of shape.
Concrete, described in measure described carbamide presoma and be slowly added into described mixed described CH3CH2OH and institute
State TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved, in standing, stands 7～8 hours.
Step S500, is heated to 750 DEG C～850 DEG C to the mixed solution of described glue, insulation；
Concrete, the described mixed solution to described glue is heated to 750 DEG C～850 DEG C, insulation, particularly as follows:
In a nitrogen atmosphere, being heated by the mixed solution of colloidal in high temperature process furnances, the mixing making described glue is molten
Liquid was heated to 800 DEG C in 4 hours, and was incubated 3 hours.
Step S600, stops heating, and is cooled to room temperature, pulverize.
The application provide titanium nitride be prepare at low temperatures, the titanium nitride having obtained micro/nano level simple to operate, and should
Titanium nitride possesses specific morphology, refers to Fig. 1 to Fig. 3.The preparation method of the titanium nitride that the application provides, solves prior art
The technical problem that the complicated process of preparation of middle titanium nitride, cost are high, purity is the highest, the preparation technology having reached titanium nitride is simple,
The technique effect that low cost, purity are high.
Embodiment three
Based on same inventive concept, the application also provides for the application of a kind of titanium nitride, and described titanium nitride is above-mentioned preparation
The titanium nitride that method prepares, described titanium nitride is applied to photo cathode material.
Wherein, Fig. 1 to Fig. 3, the tool with specific morphology structure of the above-mentioned preparation prepared at low temperatures are referred to
The titanium nitride having micro nano structure is applied to photo cathode material, eliminates intermediate storage process, compared to conventional anode material
More stable, it is to avoid phenomenon overheated and on fire occurs in battery.
The application has the beneficial effect that:
The application provides the preparation method of a kind of titanium nitride, titanium nitride and application thereof, and described titanium nitride is for make at low temperatures
The titanium nitride with micro nano structure with specific morphology structure of the standby preparation obtained is applied to photo cathode material, cancels
Intermediate storage process is compared to conventional anode material more stable, it is to avoid phenomenon overheated and on fire occurs in battery.
It should be noted last that, above detailed description of the invention only in order to technical scheme to be described and unrestricted,
Although the present invention being described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention, it all should be contained
In the middle of scope of the presently claimed invention.
Claims (9)
1. the preparation method of a titanium nitride, it is characterised in that described preparation method includes:
Obtain carbamide presoma；
Take CH3CH2OH、TiCl4Solution and described carbamide presoma, described carbamide presoma and described TiCl4Volume ratio be (3
～8): 1；
By described TiCl4Solution is slowly dropped to described CH3CH2In OH, until described CH3CH2OH and described TiCl4Solution is abundant
It is mixed into yellow transparent solution；
Measure described carbamide presoma and be slowly added into described mixed described CH3CH2OH and described TiCl4In solution, no
Disconnected stirring, until described carbamide presoma is completely dissolved, stands, makes described carbamide presoma and described TiCl4Solution is the most anti-
Should, and the jellied mixed solution of shape；
The mixed solution of described glue is heated to 750 DEG C～850 DEG C, insulation；
Stop heating, and be cooled to room temperature, pulverize.
2. preparation method as claimed in claim 1, it is characterised in that described CH3CH2OH is specially dehydrated alcohol.
3. preparation method as claimed in claim 1, it is characterised in that described carbamide presoma and described TiCl4Volume
Ratio is 3:1.
4. preparation method as claimed in claim 1, it is characterised in that described CH3CH2OH and described TiCl4The volume ratio of solution
For (4～5): 1.
5. preparation method as claimed in claim 4, it is characterised in that described CH3CH2OH and described TiCl4The volume ratio of solution
For 5:1.
6. preparation method as claimed in claim 1, it is characterised in that the described mixed solution to described glue is heated to
750 DEG C～850 DEG C, insulation, particularly as follows:
In a nitrogen atmosphere, the mixed solution of colloidal is heated in high temperature process furnances, make the mixed solution of described glue 4
It is heated to 800 DEG C in hour, and is incubated 3 hours.
7. preparation method as claimed in claim 1, it is characterised in that described in measure described carbamide presoma and be slowly added into
Described mixed described CH3CH2OH and described TiCl4In solution, it is stirred continuously, until described carbamide presoma is completely dissolved,
Standing, described standing is specially and stands 7～8 hours.
8. a titanium nitride, it is characterised in that described titanium nitride is prepared by the preparation method as described in claim 1 to 5 is arbitrary
Titanium nitride.
9. the application of a titanium nitride as claimed in claim 6, it is characterised in that described titanium nitride is applied to photo cathode material
Material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05170411A (en) * | 1991-12-24 | 1993-07-09 | Showa Denko Kk | Production of ultra-fine pulverized titanium nitride |
| CN101462701A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium nitride ceramic powder |
| CN103864030A (en) * | 2012-12-11 | 2014-06-18 | 浙江海洋学院 | Nanometer titanium nitride powder preparation method |
| KR101420653B1 (en) * | 2012-12-28 | 2014-07-21 | 포항공과대학교 산학협력단 | The cathode catalyst of polymer electrolyte fuel cell and method for preparing the same |
-
2016
- 2016-06-22 CN CN201610461003.4A patent/CN106115638A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05170411A (en) * | 1991-12-24 | 1993-07-09 | Showa Denko Kk | Production of ultra-fine pulverized titanium nitride |
| CN101462701A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium nitride ceramic powder |
| CN103864030A (en) * | 2012-12-11 | 2014-06-18 | 浙江海洋学院 | Nanometer titanium nitride powder preparation method |
| KR101420653B1 (en) * | 2012-12-28 | 2014-07-21 | 포항공과대학교 산학협력단 | The cathode catalyst of polymer electrolyte fuel cell and method for preparing the same |
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Application publication date: 20161116 |