CN109243665A - A kind of preparation method of conductive uniformly monolithic layer transition metal carbide film - Google Patents
A kind of preparation method of conductive uniformly monolithic layer transition metal carbide film Download PDFInfo
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- CN109243665A CN109243665A CN201810982522.4A CN201810982522A CN109243665A CN 109243665 A CN109243665 A CN 109243665A CN 201810982522 A CN201810982522 A CN 201810982522A CN 109243665 A CN109243665 A CN 109243665A
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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Abstract
The invention discloses a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film, this method proposes that a kind of vacuum filtration method prepares metal carbides conductive film.Specifically includes the following steps: metallic carbide titanium is made into alcohol dispersion liquid first, then titanium carbide dispersion liquid is added in dimethyl sulfoxide and is stirred, Centrifugal dispersion takes pure and turbid liquid later, upper pure and turbid liquid is ultrasonically treated in Ultrasonic cell smash, the good upper pure and turbid liquid of ultrasound is finally subjected to vacuum filtration film forming.The good conductivity of conductive monolithic layer transition metal carbide film toughness of this method preparation is high, can prepare conductive uniformly monolithic layer transition metal carbide film, this method and be simple and efficient, have broad application prospects.
Description
Technical field
The present invention relates to conductive material technical fields, and in particular to a kind of conductive uniformly monolithic layer transition metal carbide is thin
The preparation method of film.
Background technique
Currently, two-dimensional material is more and more, it is extensively studied concern since its brilliant performance causes, wherein newly
Type two-dimensional layer transition metal carbide MXene, increasingly attracts much attention.Metal carbides with layer structure
MXene is one kind novel two that Yury Gogotsi in 2011 etc. reports (Adv.Mater., 2011,23:4248-4253) first
Dimension nano material has good electric conductivity, chemical stability and mechanical property.It is filled out in energy storage, absorption, sensor, conduction
It fills the fields such as agent and shows huge potentiality.As 21 century electronic device will develop towards the directions such as light, portable, therefore
Flexible titanium carbide conductive film will have become a hot topic of research, and the leading position that gradually dominates the market.Flexible transparent conductive film
It can be applied to the fields such as flexible touch screen, flexible solar battery, flexible display.Vast application based on flexible conductive film
Prospect will also enter new deeper field for the research of flexible conductive film.
The preparation of two-dimensional layer metal carbides MXene have been relatively mature, however to the titanium carbide of single layer or few layer
The research of conductive film is also seldom.
Based on the studies above achievement and there are the problem of, the present invention proposes a kind of conductive uniformly monolithic layer transition metal carbonization
The preparation method of object film prepares conductive uniformly monolithic layer transition metal using a kind of new Ultrasonic Pulverization-vacuum filtration method
Carbide thin film.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of conductive uniformly monolithic layer transition metal carbides
The preparation method of film.Preparation process of the present invention is simple and efficient, and has good application prospect.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of conductive uniformly monolithic layer transition metal carbide film, includes the following steps:
(1) preparation of metallic carbide titanium dispersion liquid: weighing a certain amount of multilayer titanium carbide and dehydrated alcohol, by titanium carbide point
It is dispersed in dehydrated alcohol；
(2) intercalation processing is carried out to metallic carbide titanium dispersion liquid: weighs a certain amount of dimethyl sulphoxide solution in conical flask
In, titanium carbide dispersion liquid made from step (1) is transferred in conical flask, heating stirring a few hours；
(3) to metallic carbide titanium dispersion liquid carry out centrifugal treating: by titanium carbide dispersion liquid obtained in step (2) carry out from
Heart processing, outwells the supernatant containing dimethyl sulfoxide, is washed several times with dehydrated alcohol, vacuum drying treatment；
(4) titanium carbide powder obtained in step (3) preparation of titanium carbide conductive film: is dissolved in a certain amount of dehydrated alcohol
In be made into dispersion liquid, then under condition of ice bath carry out Ultrasonic Pulverization handle certain time, finally by dispersion liquid be filtered by vacuum at
Film obtains titanium carbide conductive film.
Preferably, step (1) the two-dimensional layer transition metal carbide is Ti3C2, Ti2C, Ti4C3One of or it is several
Kind, further preferably Ti3C2。
Preferably, concentration of the titanium carbide in dispersion liquid described in step (1) is 1~4mg/ml.
Preferably, the amount of multilayer titanium carbide described in step (1) is 6-24mg.
Preferably, the amount of dehydrated alcohol described in step (1) is 4-8ml, further preferably 6ml.
Preferably, the amount of dimethyl sulphoxide solution described in step (2) is 60-100ml, further preferably 80ml.
Preferably, mixing speed described in step (2) is 200-400rpm, further preferably 300rpm.
Preferably, whipping temp described in step (2) is 50-70 DEG C, further preferably 60 DEG C.
Preferably, mixing time described in step (2) is 3-5h, further preferably 4h.
Preferably, centrifugal rotational speed described in step (3) is 1000-2000rpm, further preferably 1500rpm.
Preferably, centrifugation number described in step (3) is 2-4 times, further preferably 3 times.
Preferably, vacuum drying temperature described in step (3) is 50-70 °, further preferably 60 DEG C；Drying time is
6-18h, further preferably 12h.
Preferably, the amount of dehydrated alcohol described in step (4) is 4-8ml, further preferably 6ml.
Preferably, concentration of the titanium carbide in dispersion liquid described in step (4) is 1~4mg/ml.
Preferably, the Ultrasonic Pulverization time of titanium carbide dispersion liquid described in step (4) is 1-3h, further preferably 2h.
Compared with the existing technology, the present invention has the advantage that:
Method of the invention can prepare conductive uniformly monolithic layer transition metal carbide film, improve traditional handicraft system
The bad disadvantage of the standby too thick conductive effect of stratiform titanium carbide lamella, and preparation process of the present invention is simple and efficient, and is had and is answered well
Use prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of 1 gained monolithic layer titanium carbide of embodiment.
Fig. 2 is the scanning electron microscopic picture of multi-slice titanium carbide.
Fig. 3 is the X-ray diffraction spectrogram of monolithic layer titanium carbide and multi-slice titanium carbide.
Fig. 4 is the uniform monolithic layer transition gold of conduction that 4 embodiments are prepared with various concentration monolithic layer titanium carbide dispersion liquid
Belong to the variation relation figure of carbide thin film sheet resistance.
Fig. 5 is the uniform monolithic layer transition gold of conduction that 4 embodiments are prepared with various concentration monolithic layer titanium carbide dispersion liquid
Belong to variation relation figure of the carbide thin film through differently curved number rear surface resistance.
Specific embodiment
Specific implementation of the invention is further described below in conjunction with example and attached drawing, but embodiments of the present invention
It is without being limited thereto.
Embodiment 1
(1) the multilayer titanium carbide (Ti of 6mg is weighed3C2) and 6ml dehydrated alcohol, titanium carbide is dispersed in dehydrated alcohol；
(2) dimethyl sulfoxide of 80ml is weighed in conical flask, and titanium carbide dispersion liquid made from step (1) is transferred to cone
In shape bottle, heating stirring 4 hours at 60 DEG C；
(3) titanium carbide dispersion liquid obtained in step (2) is centrifuged 3 times under 1500rpm revolving speed, sub- containing dimethyl
The supernatant of sulfone is outwelled, and is washed 3 times with dehydrated alcohol, is dried in vacuo 12h at 60 DEG C；
(4) preparation of titanium carbide conductive film: titanium carbide powder obtained in step (3) is dissolved in the dehydrated alcohol of 6ml
Being made into concentration is 1mg/ml dispersion liquid, then carries out Ultrasonic Pulverization under condition of ice bath and handles 2h, finally takes out dispersion liquid vacuum
Filter film forming, obtains titanium carbide conductive film.
The performance of conductive film prepared by the present embodiment is shown in Table 1.
Table 1
From the scanning electron microscopic picture of Fig. 1 monolithic layer titanium carbide: multi-slice titanium carbide occurs obviously after Ultrasonic Pulverization
Monolithic layer structure, and monolithic layer structure is more.
From the scanning electron microscopic picture of Fig. 2 multi-slice titanium carbide: being mostly more without the processed titanium carbide of Ultrasonic Pulverization
Lamellar structure, and it is not completely separable between lamella.
From the X-ray diffraction spectrogram of Fig. 3 monolithic layer titanium carbide and multi-slice titanium carbide: handling to obtain through Ultrasonic Pulverization
Highest peak of the monolithic titanium carbide in 39 ° of highest peak compared to the multi-slice titanium carbide that is handled without Ultrasonic Pulverization at 39 °
It is basic to disappear, and the peak at 10 ° and 20 ° is wider, peak intensity is weaker, illustrates to have obtained effective monolithic after Ultrasonic Pulverization is handled
Layer titanium carbide, and interlamellar spacing is larger.
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 4 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to the variation relation figure of sheet resistance: with the increase of titanium carbide dispersion liquid concentration, the resistance of titanium carbide conductive film first subtracts
It is gradually increased again after small.
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 5 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to variation relation figure through differently curved number rear surface resistance: when the concentration of titanium carbide dispersion is 1mg/ml, with curved
The resistance variations of the increase of bent number, titanium carbide films are very small, illustrate that the toughness of titanium carbide films is fine, sheet resistance base
This not influence of number by bending.
Embodiment 2
(1) the multilayer titanium carbide (Ti of 12mg is weighed3C2) and 6ml dehydrated alcohol, titanium carbide is dispersed in dehydrated alcohol；
(2) dimethyl sulphoxide solution of 80ml is weighed in conical flask, and titanium carbide dispersion liquid made from step (1) is shifted
In middle conical flask, heating stirring 4 hours at 60 DEG C；
(3) titanium carbide dispersion liquid obtained in step (2) is centrifuged 3 times under 1500rpm revolving speed, sub- containing dimethyl
The supernatant of sulfone is outwelled, and is washed 3 times with dehydrated alcohol, is dried in vacuo 12h at 60 DEG C；
(4) preparation of titanium carbide conductive film: titanium carbide powder obtained in step (3) is dissolved in the dehydrated alcohol of 6ml
Being made into concentration is 2mg/ml dispersion liquid, then carries out Ultrasonic Pulverization under condition of ice bath and handles 2h, finally takes out dispersion liquid vacuum
Filter film forming, obtains titanium carbide conductive film.
The performance of conductive film prepared by the present embodiment is shown in Table 2.
Table 2
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 4 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to the variation relation figure of sheet resistance: with the increase of titanium carbide dispersion liquid concentration, the resistance of titanium carbide conductive film first subtracts
It is gradually increased again after small, and when dispersion liquid concentration is 2mg/ml, the resistance of conductive film is minimum, and electric conductivity is best.
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 5 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to variation relation figure through differently curved number rear surface resistance: when the concentration of titanium carbide dispersion is 2mg/ml, with curved
The resistance variations of the increase of bent number, titanium carbide films are very small, illustrate that the toughness of titanium carbide films is fine, sheet resistance base
This not influence of number by bending.
Embodiment 3
(1) the multilayer titanium carbide (Ti of 18mg is weighed3C2) and 6ml dehydrated alcohol, titanium carbide is dispersed in dehydrated alcohol；
(2) dimethyl sulphoxide solution of 80ml is weighed in conical flask, and titanium carbide dispersion liquid made from step (1) is shifted
In middle conical flask, 60 DEG C heating stirring 4 hours；
(3) titanium carbide dispersion liquid obtained in step (2) is centrifuged 3 times under 1500rpm revolving speed, sub- containing dimethyl
The supernatant of sulfone is outwelled, and is washed 3 times with dehydrated alcohol, is dried in vacuo 12h at 60 DEG C；
(4) titanium carbide powder obtained in step (3) is dissolved in the dehydrated alcohol of 6ml and is made into concentration as 3mg/ml dispersion
Then liquid carries out Ultrasonic Pulverization under condition of ice bath and handles 2h, finally dispersion liquid is filtered by vacuum and forms a film, obtain titanium carbide conduction
Film.
The performance of conductive film prepared by the present embodiment is shown in Table 3.
Table 3
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 4 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to the variation relation figure of sheet resistance: with the increase of titanium carbide dispersion liquid concentration, the resistance of titanium carbide conductive film first subtracts
It is gradually increased again after small.
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 5 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to variation relation figure through differently curved number rear surface resistance: when the concentration of titanium carbide dispersion is 3mg/ml, with curved
The resistance variations of the increase of bent number, titanium carbide films are very small, illustrate that the toughness of titanium carbide films is fine, sheet resistance base
This not influence of number by bending.
Embodiment 4
(1) the multilayer titanium carbide (Ti of 24mg is weighed3C2) and 6ml dehydrated alcohol, titanium carbide is dispersed in dehydrated alcohol；
(2) dimethyl sulphoxide solution of 80ml is weighed in conical flask, and titanium carbide dispersion liquid made from step (1) is shifted
In middle conical flask, heating stirring 4 hours at 60 DEG C；
(3) titanium carbide dispersion liquid obtained in step (2) is centrifuged 3 times under 1500rpm revolving speed, sub- containing dimethyl
The supernatant of sulfone is outwelled, and is washed 3 times with dehydrated alcohol, is dried in vacuo 12h at 60 DEG C；
(4) titanium carbide powder obtained in step (3) is dissolved in the dehydrated alcohol of 6ml and is made into concentration as 4mg/ml dispersion
Then liquid carries out Ultrasonic Pulverization under condition of ice bath and handles 2h, finally dispersion liquid is filtered by vacuum and forms a film, obtain titanium carbide conduction
Film.
The performance of conductive film prepared by the present embodiment is shown in Table 4.
Table 4
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 4 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to the variation relation figure of sheet resistance: with the increase of titanium carbide dispersion liquid concentration, the resistance of titanium carbide conductive film first subtracts
It is gradually increased again after small.
By the uniform monolithic layer transition metal carbide film of the conduction of Fig. 5 various concentration monolithic layer titanium carbide dispersion liquid preparation
Known to variation relation figure through differently curved number rear surface resistance: when the concentration of titanium carbide dispersion is 4mg/ml, with curved
The resistance variations of the increase of bent number, titanium carbide films are very small, illustrate that the toughness of titanium carbide films is fine, sheet resistance base
This not influence of number by bending.
Claims (10)
1. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film, which comprises the steps of:
(1) preparation of metallic carbide titanium dispersion liquid: multilayer titanium carbide is dispersed in dehydrated alcohol, obtains the dispersion of metallic carbide titanium
Liquid；
(2) intercalation processing is carried out to metallic carbide titanium dispersion liquid: diformazan is added in metallic carbide titanium dispersion liquid made from step (1)
In base sulfoxide, heating stirring；
(3) centrifugal treating is carried out to metallic carbide titanium dispersion liquid: titanium carbide dispersion liquid obtained in step (2) is carried out at centrifugation
Reason, outwells the supernatant containing dimethyl sulfoxide, is washed with dehydrated alcohol, vacuum drying treatment；
(4) preparation of titanium carbide conductive film: titanium carbide powder obtained in step (3) is dissolved in dehydrated alcohol and is made into dispersion
Then liquid carries out Ultrasonic Pulverization processing under condition of ice bath, finally dispersion liquid is filtered by vacuum and forms a film, and obtains conductive uniform monolithic
Layer transition metal carbide film.
2. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that step (1) titanium carbide is Ti3C2, Ti2C, Ti4C3One or more of.
3. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that concentration of step (1) titanium carbide in metallic carbide titanium dispersion liquid is 1 ~ 4mg/ml.
4. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that the speed of step (2) described stirring is 200-400rpm.
5. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that the temperature of step (2) described stirring is 50-70 DEG C.
6. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that the time of step (2) described stirring is 3-5h.
7. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that the revolving speed of step (3) described centrifugation is 1000-2000rpm；The number of the centrifugation is 2-4 times.
8. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that step (3) the vacuum drying temperature is 50-70 DEG C, time 6-18h.
9. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that concentration of step (4) the described titanium carbide in dispersion liquid is 1 ~ 4mg/ml.
10. a kind of preparation method of conductive uniformly monolithic layer transition metal carbide film according to claim 1, special
Sign is that the time of step (4) described Ultrasonic Pulverization is 1-3h.
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| CN111137895A (en) * | 2020-01-03 | 2020-05-12 | 南昌航空大学 | Preparation method of two-dimensional layered nano material MXene quantum dots |
| CN111341497A (en) * | 2020-03-13 | 2020-06-26 | 浙江大学 | Preparation method of silver nanowire-MXene composite transparent conductive film |
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| CN112795209A (en) * | 2019-11-14 | 2021-05-14 | 清华大学 | Two-dimensional titanium carbide film with stable environment and excellent conductivity and mechanical property, and preparation method and application thereof |
| CN112992402A (en) * | 2021-04-16 | 2021-06-18 | 西安宏星电子浆料科技股份有限公司 | Silver and two-dimensional MXene mixed system conductor slurry for chip resistor and preparation method thereof |
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| CN112795209A (en) * | 2019-11-14 | 2021-05-14 | 清华大学 | Two-dimensional titanium carbide film with stable environment and excellent conductivity and mechanical property, and preparation method and application thereof |
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| CN112992402A (en) * | 2021-04-16 | 2021-06-18 | 西安宏星电子浆料科技股份有限公司 | Silver and two-dimensional MXene mixed system conductor slurry for chip resistor and preparation method thereof |
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