CN109778352A - A kind of Ti of electrostatic spinning in-situ reducing preparation4O7Nanofiber and its method - Google Patents
A kind of Ti of electrostatic spinning in-situ reducing preparation4O7Nanofiber and its method Download PDFInfo
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- CN109778352A CN109778352A CN201910055838.3A CN201910055838A CN109778352A CN 109778352 A CN109778352 A CN 109778352A CN 201910055838 A CN201910055838 A CN 201910055838A CN 109778352 A CN109778352 A CN 109778352A
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Abstract
The invention discloses a kind of Ti of electrostatic spinning in-situ reducing preparation4O7Nanofiber and its method, belong to technical field of nanometer material preparation.The Ti prepared using electrostatic spinning in-situ reducing4O7Nanofiber average diameter about 100nm, is in item chain structure, and length is 50 μm or more.Ti4O7The preparation method of nanofiber uses polyvinylpyrrolidone (PVP) for fibrous template and carbon source, and butyl titanate (TTIP) is titanium source；In conjunction with electrostatic spinning technique and heat treatment process, presoma PVP/TTIP composite nano fiber is made by electrostatic spinning technique；It is heat-treated, carbon source thermal decomposition generates C and titanium source thermally decomposes to generate TiO2, under certain condition, Ti is made in the two in-situ reducing4O7Nanofiber.The Ti4O7The characteristics of nanofiber has morphology controllable, and particle size is small, large specific surface area.Furthermore preparation method simple process of the present invention is feasible, and process control is strong, easy to industrialized production.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, in particular to a kind of Ti of electrostatic spinning in-situ reducing preparation4O7
Nanofiber and its method.
Background technique
Ti4O7Nano-fiber material is since it is with excellent electric conductivity, corrosion resistance, electrochemical stability, environmentally protective
The advantages that, it can be used as a kind of energy-saving high-efficiency environment-friendly type ceramic electrode material of great application prospect, it is expected to super applied to high-performance
Grade capacitor area.Ti at present4O7Often pass through TiO2The preparation of high temperature reduction method can mutually be divided into following two side by the object of reducing agent
Method: (1) solid phase reduction method: carbon black is as reducing agent and space bit resist, TiO2Reducing degree limited by solid phase interface, compared with
Hardly possible obtains single-phase Ti4O7, conductivity is by Ti4O7Content and granular size influence.(2) gas phase reduction process: due to reduction
Property gas have good diffusivity can improve kinetics behavior so as to shorten the reaction time, but due to lack solid carbon make
For steric hindrance agent, under high temperature reducing conditions, product grain sintering is serious, makes Ti4O7Particle is larger, specific surface area is smaller and pattern
It is more difficult to control.
The Ti that existing preparation method obtains4O7Particle size is big, specific surface area is small, the difficult and pure Ti of pattern control4O7Object is mutually made
Standby difficult and powdered Ti4O7" dead volume " blocking is easily formed because needing bonding agent and conductive additive in electrode fabrication
The transmission of electronics and electrolyte are spread to electrode material surface, to reduce its chemical property, this is limited to a certain extent
Its application in high-performance super capacitor field.
Summary of the invention
In view of this, a kind of it is an object of the invention to overcome the deficiencies of the prior art and provide methods simple, pattern and
Controllable, the easy to industrialized production Ti of particle size4O7The electrostatic spinning in-situ reduction preparation method of nanofiber.
The present invention solves its technical problem institute using technical solution: a kind of electrostatic spinning in-situ reducing preparation Ti4O7Nanometer
The method of fiber, the described method comprises the following steps:
S1: weighing TTIP, EtOH, HAc, prepares titanium source solution；Weigh PVP, EtOH, prepared polymer solution, with polymer P VP
Template and carbon source as nanofiber；
S2: the titanium source solution in S1 is added in polymer solution, stirs evenly and is configured to electrostatic spinning solution；In electrostatic spinning
In solution process for preparation, fixed carbon source content regulates and controls its carbon/titanium ratio by adjusting the additive amount (0 ~ 1.5 g) of TTIP.
S3: the electrostatic spinning solution prepared in S2 is subjected to electrostatic spinning, it is fine to obtain presoma PVP/TTIP composite Nano
Dimension, that is, use polymer Polyvinylpyrrolidone (PVP) for template and carbon source, and butyl titanate (TTIP) is titanium source, obtains forerunner
Body PVP/TTIP composite nano fiber.
S4: presoma PVP/TTIP composite nano fiber is sintered, Ti is obtained4O7Nanofiber.
Preferably, in the S1 and S2, during preparing titanium source solution, polymer solution and electrostatic spinning solution,
It is both needed to be uniformly mixed solution using magnetic agitation, until forming light yellow clear electrostatic spinning solution.
Preferably, in the S3, light yellow clear electrostatic spinning solution is packed into the syringe for having stainless steel syringe needle
It is interior, and place it on micro-injection pump and fix, the delivery rate of syringe pump is 1 ~ 1.5 mL/h, the stainless steel syringe needle connection
High voltage power supply, operating voltage are 8 ~ 12 kV, are set as the aluminium foil plate earthing for collecting presoma PVP/TTIP composite nano fiber
It sets, and keeping the operating distance of aluminum foil plate and stainless steel syringe needle is 10 ~ 12 cm.
Preferably, in the S4, the environment of presoma PVP/TTIP composite nano fiber sintering is vacuum atmosphere condition.
Preferably, in the S4, presoma PVP/TTIP composite nano fiber is sintered under the conditions of 1100 DEG C, is being carried out
In the sintering process that heats up, at 500 DEG C or less, heating rate is 5 DEG C/min, at 500 DEG C or more, heating rate for 10 DEG C/
min.The rate to heat up when being lower than 500 DEG C is low, and the rate to heat up when higher than 500 DEG C is high, which can be abundant
The fiber morphology of presoma is kept not to be destroyed while removing polymer residue carbon content, to improve the quality of product.
Preferably, in the S4, sintered presoma PVP/TTIP composite nano fiber is cooled to 100 DEG C or less
It comes out of the stove to get Ti is arrived4O7Nanofiber.
A kind of Ti prepared using the above method4O7Nanofiber, the Ti4O7Nanofiber average diameter is 100 nm,
In item chain structure, length is greater than 50 μm.
The beneficial effects of the present invention are: Ti of the invention4O7The electrostatic spinning in-situ reduction preparation method of nanofiber, is adopted
It is template and carbon source with polyvinylpyrrolidone (PVP), butyl titanate (TTIP) is titanium source；In conjunction with electrostatic spinning technique and Re Chu
Presoma PVP/TTIP composite nano fiber is made by electrostatic spinning technique in science and engineering skill；It is heat-treated, carbon source polymerization
Object thermal decomposition generates C and titanium source thermally decomposes to generate TiO2Under certain condition, Ti is made in the two in-situ reducing4O7Nanofiber.It should
Ti4O7The characteristics of nanofiber has morphology controllable, and particle size is small, large specific surface area.Furthermore preparation method work of the present invention
Skill simple possible, process control is strong, easy to industrialized production.
Detailed description of the invention
Fig. 1 is the Ti prepared in the embodiment of the present invention 34O7The scanning electron microscopic picture of nanofiber；
Fig. 2 is the Ti prepared in the embodiment of the present invention 34O7The X-ray diffractogram of nanofiber.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, rather than comprehensive embodiment.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
A kind of electrostatic spinning in-situ reducing preparation Ti4O7The method of nanofiber, the described method comprises the following steps:
S1: 0 g TTIP, 3 mL EtOH, 3 mL HAc are weighed using 10 min of magnetic agitation and are configured to titanium after mixing evenly
Source solution；7 g PVP, 93 g EtOH are weighed, using 12 h of magnetic agitation, are configured to the PVP/EtOH that mass fraction is 7 wt%
Solution；
S2: the titanium source solution in S1 is added in the PVP/EtOH solution that 6.43 g mass fractions are 7 wt%, is stirred using magnetic force
Mix the electrostatic spinning solution that achromaticity and clarification is configured to after 2 h；
S3: the electrostatic spinning solution being configured in S2 is packed into the syringe that the volume with stainless steel syringe needle is 10 mL, stainless steel
The model G21 of syringe needle, and syringe is placed on micro-injection pump and is fixed, setting delivery rate is 1 mL/h；Stainless steel syringe needle
High voltage power supply is connected, operating voltage is 8 kV；Aluminum foil plate is as receiver and is grounded, and keeps stainless steel syringe needle to the work of receiver board
Making distance is 12 cm；Electrostatic spinning is carried out, presoma PVP nanofiber is collected on aluminum foil plate, and place it in 80 DEG C of baking ovens
Kept dry；
S4: the presoma PVP nanofiber prepared is sintered 2 hours in 1100 DEG C under vacuum conditions.Wherein, sintering heating
In the process, 500 DEG C or less when, adjusting heating rate is 5 DEG C/min, at 500 DEG C or more, adjust heating rate be 10 DEG C/
Min is cooled to 100 DEG C or less and comes out of the stove to get to carbon nano-fiber after sintering, carbon nano-fiber average diameter is 50 nm,
Length is greater than 50 μm.
Embodiment 2
A kind of electrostatic spinning in-situ reducing preparation Ti4O7The method of nanofiber, the described method comprises the following steps:
S1: 1 g TTIP, 3 mL EtOH, 3 mL HAc are weighed using 10 min of magnetic agitation and are configured to titanium after mixing evenly
Source solution；7 g PVP, 93 g EtOH are weighed, using 12 h of magnetic agitation, are configured to the PVP/EtOH that mass fraction is 7 wt%
Solution；
S2: the titanium source solution in S1 is added in the PVP/EtOH solution that 6.43 g mass fractions are 7 wt%, is stirred using magnetic force
Light yellow clear electrostatic spinning solution is configured to after mixing 2 h；
S3: the electrostatic spinning solution being configured in S2 is packed into the syringe that the volume with stainless steel syringe needle is 10 mL, stainless steel
The model G21 of syringe needle, and syringe is placed on micro-injection pump and is fixed, setting delivery rate is 1.2 mL/h；Stainless pin
Head connection high voltage power supply, operating voltage are 10 kV；Aluminum foil plate is as receiver and is grounded, and keeps stainless steel syringe needle to receiver board
Operating distance be 11 cm；Electrostatic spinning is carried out, presoma PVP nanofiber is collected on aluminum foil plate, and place it in 80 DEG C
Oven drying saves；
S4: the presoma PVP nanofiber prepared is sintered 2 hours in 1100 DEG C under vacuum conditions.Wherein, sintering heating
In the process, 500 DEG C or less when, adjusting heating rate is 5 DEG C/min, at 500 DEG C or more, adjust heating rate be 10 DEG C/
Min is cooled to 100 DEG C or less and comes out of the stove to get C/Ti is arrived after sintering4O7Composite nano fiber, average fibre diameter 80
Nm, length are greater than 50 μm.
Embodiment 3
A kind of electrostatic spinning in-situ reducing preparation Ti4O7The method of nanofiber, the described method comprises the following steps:
S1: 1.5 g TTIP, 3 mL EtOH, 3 mL HAc are weighed and are configured to after mixing evenly using 10 min of magnetic agitation
Titanium source solution；7 g PVP, 93 g EtOH are weighed, using 12 h of magnetic agitation, are configured to the PVP/ that mass fraction is 7 wt%
EtOH solution；
S2: the titanium source solution in S1 is added in the PVP/EtOH solution that 6.43 g mass fractions are 7 wt%, is stirred using magnetic force
Light yellow clear electrostatic spinning solution is configured to after mixing 2 h；
S3: the electrostatic spinning solution being configured in S2 is packed into the syringe that the volume with stainless steel syringe needle is 10 mL, stainless steel
The model G21 of syringe needle, and syringe is placed on micro-injection pump and is fixed, setting delivery rate is 1.5 mL/h；Stainless pin
Head connection high voltage power supply, operating voltage are 12 kV；Aluminum foil plate is as receiver and is grounded, and keeps stainless steel syringe needle to receiver board
Operating distance be 10 cm；Electrostatic spinning is carried out, presoma PVP/TTIP composite nano fiber is collected on aluminum foil plate, and will
It is placed in 80 DEG C of oven dryings and saves；
S4: the presoma PVP/TTIP composite nano fiber prepared is sintered 2 hours in 1100 DEG C under vacuum conditions.Its
In, it being sintered in temperature-rise period, at 500 DEG C or less, adjustings heating rate is 5 DEG C/min, at 500 DEG C or more, adjusting heating rate
For 10 DEG C/min, it is cooled to 100 DEG C or less after sintering and comes out of the stove to get Ti is arrived4O7Nanofiber.
To Ti obtained4O7Nanofiber carries out electron-microscope scanning and X-ray diffraction test, and result is respectively such as Fig. 1,2 institutes
Show.The Ti4O7The characteristics of nanofiber has morphology controllable, and particle size is small, large specific surface area, and Ti obtained4O7Nanowire
Dimension average diameter is 100 nm, and length is greater than 50 μm.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (7)
1. a kind of electrostatic spinning in-situ reducing prepares Ti4O7The method of nanofiber, which is characterized in that the method includes following
Step:
S1: weighing TTIP, EtOH, HAc, prepares titanium source solution；Weigh PVP, EtOH, prepared polymer solution；
S2: the titanium source solution in S1 is added in polymer solution, electrostatic spinning solution is configured to after stirring；
S3: the electrostatic spinning solution being configured in S2 is subjected to electrostatic spinning, obtains presoma PVP/TTIP composite nano fiber；
S4: presoma PVP/TTIP composite nano fiber is sintered, Ti is obtained4O7Nanofiber.
2. a kind of electrostatic spinning in-situ reducing according to claim 1 prepares Ti4O7The method of nanofiber, feature exist
In: in the S1 and S2, during preparing titanium source solution, polymer solution and electrostatic spinning solution, it is both needed to using magnetic force
Stirring is uniformly mixed solution, until forming light yellow clear electrostatic spinning solution.
3. a kind of electrostatic spinning in-situ reducing according to claim 1 prepares Ti4O7The method of nanofiber, feature exist
In: in the S3, light yellow clear electrostatic spinning solution is packed into the syringe with stainless steel syringe needle, and is placed it in
Fixed on micro-injection pump, the delivery rate of syringe pump is 1 ~ 1.5 mL/h, and the stainless steel syringe needle connects high voltage power supply, work
Voltage is 8 ~ 12 kV, is arranged as the aluminium foil plate earthing for collecting presoma PVP/TTIP composite nano fiber, and keep aluminum foil plate
Operating distance with stainless steel syringe needle is 10 ~ 12 cm.
4. a kind of electrostatic spinning in-situ reducing according to claim 1 prepares Ti4O7The method of nanofiber, feature exist
In: in the S4, the environment of presoma PVP/TTIP composite nano fiber sintering is vacuum atmosphere condition.
5. a kind of electrostatic spinning in-situ reducing according to claim 1 or 4 prepares Ti4O7The method of nanofiber, feature
Be: in the S4, presoma PVP/TTIP composite nano fiber is sintered under the conditions of 1100 DEG C, sintered heat up
Cheng Zhong, at 500 DEG C or less, heating rate is 5 DEG C/min, and at 500 DEG C or more, heating rate is 10 DEG C/min.
6. a kind of electrostatic spinning in-situ reducing according to claim 5 prepares Ti4O7The method of nanofiber, feature exist
In: in the S4, sintered presoma PVP/TTIP composite nano fiber is cooled to 100 DEG C or less and is come out of the stove to get arriving
Ti4O7Nanofiber.
7. a kind of Ti prepared using claim 1 the method4O7Nanofiber, it is characterised in that: the Ti4O7Nanofiber
Average diameter is 100 nm, is in item chain structure, and length is greater than 50 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036095A (en) * | 2019-12-31 | 2020-04-21 | 济南大学 | Flexible self-supporting MoO2@ C nanofiber film material and preparation method and application thereof |
| CN111249521A (en) * | 2020-03-04 | 2020-06-09 | 昆明理工大学 | Preparation method of composite porous scaffold material for bone repair |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1590298A2 (en) * | 2003-01-10 | 2005-11-02 | Advanced Power Devices, Inc. | ELECTRICALLY CONDUCTIVE FIBERS OF Ti sb 4 /sb O sb 7 /sb AND Ti sb 5 /sb O sb 9 /sb |
| KR101384215B1 (en) * | 2012-09-28 | 2014-04-10 | 충남대학교산학협력단 | The nanofiber for electrode of DSSC includes porous TiO2 and the manufacturing method thereof |
| CN105489863A (en) * | 2015-12-31 | 2016-04-13 | 长沙矿冶研究院有限责任公司 | C/Ti4O7 composite nanofiber based lithium-sulfur battery positive electrode material and preparation method therefor |
| CN105609687A (en) * | 2015-12-31 | 2016-05-25 | 长沙矿冶研究院有限责任公司 | Lithium-sulfur battery taking C/Ti4O7 composite fiber non-woven fabrics as intercalation layer |
| CN105696110A (en) * | 2016-02-26 | 2016-06-22 | 哈尔滨工业大学深圳研究生院 | Conductive nanofiber and preparation method and application thereof |
| CN106978652A (en) * | 2017-04-25 | 2017-07-25 | 山东大学 | A kind of preparation method of the sour oxygen titanium precursors colloidal sol spinning solution of poly-vinegar and TiOx nano fiber photocatalyst |
| CN108793103A (en) * | 2018-05-14 | 2018-11-13 | 肇庆市华师大光电产业研究院 | A method of metal nitride is prepared with carbonitride |
| CN108914250A (en) * | 2018-08-16 | 2018-11-30 | 山东大学 | The preparation method of poly- acetyl acetone titanium precursors colloidal sol spinning solution, titanium oxide continuous fiber and nanofiber |
| CN109119636A (en) * | 2018-07-10 | 2019-01-01 | 华南师范大学 | A kind of titanium vanadium nitrogen nano fiber collector and preparation method thereof |
-
2019
- 2019-01-22 CN CN201910055838.3A patent/CN109778352B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1590298A2 (en) * | 2003-01-10 | 2005-11-02 | Advanced Power Devices, Inc. | ELECTRICALLY CONDUCTIVE FIBERS OF Ti sb 4 /sb O sb 7 /sb AND Ti sb 5 /sb O sb 9 /sb |
| KR101384215B1 (en) * | 2012-09-28 | 2014-04-10 | 충남대학교산학협력단 | The nanofiber for electrode of DSSC includes porous TiO2 and the manufacturing method thereof |
| CN105489863A (en) * | 2015-12-31 | 2016-04-13 | 长沙矿冶研究院有限责任公司 | C/Ti4O7 composite nanofiber based lithium-sulfur battery positive electrode material and preparation method therefor |
| CN105609687A (en) * | 2015-12-31 | 2016-05-25 | 长沙矿冶研究院有限责任公司 | Lithium-sulfur battery taking C/Ti4O7 composite fiber non-woven fabrics as intercalation layer |
| CN105696110A (en) * | 2016-02-26 | 2016-06-22 | 哈尔滨工业大学深圳研究生院 | Conductive nanofiber and preparation method and application thereof |
| CN106978652A (en) * | 2017-04-25 | 2017-07-25 | 山东大学 | A kind of preparation method of the sour oxygen titanium precursors colloidal sol spinning solution of poly-vinegar and TiOx nano fiber photocatalyst |
| CN108793103A (en) * | 2018-05-14 | 2018-11-13 | 肇庆市华师大光电产业研究院 | A method of metal nitride is prepared with carbonitride |
| CN109119636A (en) * | 2018-07-10 | 2019-01-01 | 华南师范大学 | A kind of titanium vanadium nitrogen nano fiber collector and preparation method thereof |
| CN108914250A (en) * | 2018-08-16 | 2018-11-30 | 山东大学 | The preparation method of poly- acetyl acetone titanium precursors colloidal sol spinning solution, titanium oxide continuous fiber and nanofiber |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036095A (en) * | 2019-12-31 | 2020-04-21 | 济南大学 | Flexible self-supporting MoO2@ C nanofiber film material and preparation method and application thereof |
| CN111249521A (en) * | 2020-03-04 | 2020-06-09 | 昆明理工大学 | Preparation method of composite porous scaffold material for bone repair |
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