CN106976917B - Sheet cobalt black-two-dimensional layer carbonization titanium composite material and its two-step preparation - Google Patents
Sheet cobalt black-two-dimensional layer carbonization titanium composite material and its two-step preparation Download PDFInfo
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- CN106976917B CN106976917B CN201710124049.1A CN201710124049A CN106976917B CN 106976917 B CN106976917 B CN 106976917B CN 201710124049 A CN201710124049 A CN 201710124049A CN 106976917 B CN106976917 B CN 106976917B
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- C—CHEMISTRY; METALLURGY
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- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- 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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- H—ELECTRICITY
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- 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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Abstract
The present invention provides a kind of sheet cobalt black two-dimensional layer carbonization titanium composite material and its two-step preparation, first by Ti3C2Powder and CoCL2 6H2O are dissolved in the urea liquid that concentration is 0.03~0.3mol/L, are stirred to react 5~12h at 85~95 DEG C, are obtained reaction mixture；Solid and drying are separated after reaction mixture is washed again；Dry solid is subjected to heat treatment crystallization, obtains sheet cobalt black two-dimensional layer carbonization titanium composite material.Sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material is made by two-step method in the present invention, substantial amounts of sheet cobalt black is distributed between sheet surfaces and lamella, not only increase interlamellar spacing, improve the specific surface area of material, and stacking between layers is effectively prevented, add the chemical property of nanocomposite.
Description
【Technical field】
The invention belongs to nano-functional material preparing technical field, more particularly to a kind of sheet cobalt black-two-dimensional layer
Be carbonized titanium composite material and its two-step preparation.
【Background technology】
Two-dimensional layer titanium carbide (MXene) is to utilize Ti3AlC2The difference of interlaminar action power, by certain method by Al
Layer corrosion obtains.Due to its unique class graphene-structured, larger specific surface area, good electric conductivity etc. so that its
Absorption, photocatalysis, biosensor, lithium ion battery, ultracapacitor etc. are widely used.2015,
Zhao et al. is by by carbon nanotubes and Ti3C2TxIt is compound to have obtained the Ti of sandwich-like3C2Tx/MWCNT composite materials test table
Ti after bright load3C2Tx/MWCNT has high capacitance and the rate capability of superelevation.2016, Huang et al. was by by Cu
(CH3COO)2H2O and Ti2CTxSolvent heat treatment has obtained Cu2O/MXene nano-powders, the experimental results showed that material after load
Have greatly improved before chemical property ratio.
The oxide of cobalt is a kind of important magnetic p-type semiconductor, is a kind of important functionalization material, is mainly used in
Catalysis, electrochemistry, gas sensor, lithium ion battery etc..In transition gold when the size of cobalt black reaches nanometer range
Category field and field of nanometer technology are all widely used.Therefore, prepare the cobalt black of the nano-scale of different-shape by its
Compound and many researchers' researchs at present hot spots are carried out with other materials haveing excellent performance.2013, Zhao etc. utilized molten
Agent hot-hot decomposition method is prepared for COO/graphene nanocomposites, the results showed that the chemical property of material after load
It is significantly improved.
Sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material does not have been reported that also at present, and generally oxidation is sub-
The pattern of cobalt is inhomogenous.
【The content of the invention】
It is an object of the invention to overcome problems of the prior art, a kind of sheet cobalt black-two-dimensional layer is provided
Shape is carbonized titanium composite material and its two-step preparation, by homogeneous precipitation-heat treatment method prepare the homogeneous cobalt black of pattern/
Two-dimensional layer carbonization titanium nanometer composite material.
In order to achieve the above object, the present invention adopts the following technical scheme that：
Comprise the following steps：
(1) by Ti3C2Powder and CoCL2 6H2O are dissolved in the urea liquid that concentration is 0.03~0.3mol/L, 85~
5~12h is stirred to react at 95 DEG C, obtains reaction mixture；Solid and drying are separated after reaction mixture is washed again；
(2) dry solid is subjected to heat treatment crystallization, obtains sheet cobalt black-two-dimensional layer titanium carbide composite wood
Material.
Further, Ti in step (1)3C2The ratio of powder, CoCL2 6H2O and urea liquid is (50~200) mg：(0.1
~1.0) g：(50~100) mL.
Further, reaction mixture deionized water and absolute ethyl alcohol centrifuge washing in step (1).
Further, the solid isolated in step (1) is dried in vacuo 12~48h at 40~100 DEG C.
Further, in the heat treatment crystallization of step (2), heating rate is 1~4 DEG C/min.
Further, the heat treatment crystallization of step (2) carries out in nitrogen or argon gas atmosphere.
Further, it is to keep the temperature 1~3h at 300~450 DEG C in the heat treatment crystallization of step (2).
It is a kind of to utilize sheet cobalt black made from two-step preparation as described above-two-dimensional layer carbonization titanium composite material.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention is by homogeneous precipitation-heat treatment two-step method, by Ti3C2With the urea water of CoCL2 6H2O and various concentration
Solution mix and then is heat-treated at a certain temperature, cobalt ions and Ti3C2With reference to urea is in aqueous solution under certain temperature
The presoma that generation basic cobaltous carbonate and titanium carbide are combined with cobalt ions is decomposed, is calcined by protective atmosphere, basic cobaltous carbonate point
Solution generation cobalt black.And obtain a kind of sheet cobalt protoxide/two-dimensional layer carbonization titanium nanometer composite material.Substantial amounts of sheet one
Cobalt oxide is distributed between sheet surfaces and lamella, not only increases interlamellar spacing, improves the specific surface area of material, and effectively
Stacking between layers is prevented, the chemical property of material is improved by the synergistic effect of two kinds of materials.And this hair
It is bright to have preparation process simple, controllably, the features such as obtained cobalt black novel in shape.
The obtained composite material pattern of the present invention is homogeneous, is sheet, and sheet produced by the present invention cobalt black/two-dimensional layer
Titanium carbide can be used in high performance electrode material, with Ti3C2It compares, COO-Ti3C2The chemical property of composite material has centainly
Raising, charging and discharging currents be 100mA when, Ti3C2Specific capacity be 98mAh/g, C after loadOO-Ti3C2Specific capacity improve
To 220mAh/g.
【Description of the drawings】
Fig. 1 is the SEM figures of sheet cobalt black/two-dimensional nano carbonization titanium composite material.
Fig. 2 is the charge and discharge cycles figure of sheet cobalt black/two-dimensional nano carbonization titanium composite material.
【Specific embodiment】
The present invention is described in further details with embodiment below in conjunction with the accompanying drawings.
The present invention is first by Ti3AlC2Chemical etching is carried out in HF acid, Al is made selectively to be etched away, obtains one kind
Two-dimensional layer Ti3C2Nano material utilizes the Ti3C2Nano material prepares sheet cobalt black-two-dimensional layer titanium carbide composite wood
Material.Preparation method of the present invention specifically includes：
(1) ternary Ti3AlC2The preparation of ceramic powder：Ternary layers are prepared according to the method for patent ZL201310497696.9
Shape Ti3AlC2Ceramic powder；It is more than 97% ternary layered Ti using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling item
Part：The mass ratio of ballstone, batch mixing and ball-milling medium (absolute ethyl alcohol) is 10:1:1, rotational speed of ball-mill 400r/min, high-energy ball milling
Time is 4h, then dries gained solid-liquid batch mixing at 50 DEG C, obtains the Ti that grain size is about 8 μm3AlC2Ceramic powder；
(2) two-dimensional layer Ti3C2The preparation of nano material：Two-dimensional layer is synthesized according to the method for patent 201410812056.7
Shape Ti3C2Nano material；Secondly, by gained Ti in step (1)3AlC2Ceramic powder is immersed in HF acid solutions, wherein 5g
Ti3AlC2Powder, which is immersed in 100mL mass concentration 40wt%HF acid solutions, to react for 24 hours；Magnetic agitation, to ternary layered
Ti3AlC2It is 5~6 with deionized water eccentric cleaning to pH after powder carries out corrosion treatment, by obtained solid sample drying at room temperature,
Obtain two-dimensional layer Ti3C2Nano material；
(3) Ti is taken3C250~200mg of powder, 0.1~1.0g of CoCL2 6H2O be dissolved in 50~100mL concentration for 0.03~
5~12h is stirred in the urea liquid of 0.3mol/L at 85~95 DEG C.Then, it will react mixed with deionized water and absolute ethyl alcohol
It closes solution centrifuge washing for several times, then centrifuges solid, 40~100 DEG C of 12~48h of vacuum drying.Finally, with 1~4 DEG C/min
Heating rate 1~3h kept the temperature in 300~450 DEG C of nitrogen or argon gas atmosphere carry out heat treatment crystallization to get to one oxygen of sheet
Change cobalt/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 1
Take Ti3C2Powder 50mg, CoCL2 6H2O 0.1g are dissolved in the urea liquid that 50mL concentration is 0.03mol/L 95
5h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 40 DEG C of vacuum drying 48h.Finally, 3h is kept the temperature in 300 DEG C of nitrogen atmospheres with the heating rate of 1 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 2
Take Ti3C2Powder 200mg, CoCL2 6H2O 1.0g are dissolved in the urea liquid that 100mL concentration is 0.03mol/L
8h is stirred at 95 DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 100 DEG C of vacuum drying 12h.Finally, 1h is kept the temperature in 450 DEG C of nitrogen atmospheres with the heating rate of 4 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 3
Take Ti3C2Powder 150mg, CoCL2 6H2O 1.0g are dissolved in the urea liquid that 80mL concentration is 0.3mol/L 85
12h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 60 DEG C of vacuum drying 12h.Finally, 2h is kept the temperature in 400 DEG C of nitrogen atmospheres with the heating rate of 3 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 4
Take Ti3C2Powder 200mg, CoCL2 6H2O 0.5g are dissolved in the urea liquid that 75mL concentration is 0.1mol/L 90
10h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 80 DEG C of vacuum drying 12h.Finally, 3h is kept the temperature in 450 DEG C of nitrogen atmospheres with the heating rate of 4 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 5
Take Ti3C2Powder 200mg, CoCL2 6H2O 0.1g are dissolved in the urea liquid that 100mL concentration is 0.2mol/L 95
5h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 40 DEG C of vacuum drying 12h.Finally, 3h is kept the temperature in 400 DEG C of nitrogen atmospheres with the heating rate of 1 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 6
Take Ti3C2Powder 200mg, CoCL2 6H2O 1.0g are dissolved in the urea liquid that 50mL concentration is 0.3mol/L 85
8h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 100 DEG C of vacuum drying 48h.Finally, 1h is kept the temperature in 350 DEG C of nitrogen atmospheres with the heating rate of 4 DEG C/min to be heat-treated
Crystallization is to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
Embodiment 7
Take Ti3C2Powder 120mg, CoCL2 6H2O 0.8g are dissolved in the urea liquid that 60mL concentration is 0.15mol/L 92
6h is stirred at DEG C.Then, with deionized water and absolute ethyl alcohol by reaction mixture centrifuge washing for several times, then centrifuge solid
Body, 50 DEG C of vacuum drying are for 24 hours.Finally, 1.5h is kept the temperature in 380 DEG C of nitrogen atmospheres with the heating rate of 2 DEG C/min and carries out hot place
Crystallization is managed to get to sheet cobalt black/two-dimensional layer carbonization titanium nanometer composite material.
As shown in Figure 1, COO-Ti3C2Composite material is with clearly layer structure, sheet cobalt oxide are evenly coated at Ti3C2
Sheet surfaces.
As seen from Figure 2, with Ti3C2It compares, COO-Ti3C2The chemical property of composite material improves.
When charging and discharging currents are 100mA, Ti3C2Specific capacity be 98mAh/g, C after loadOO-Ti3C2Specific capacity be increased to
220mAh/g。
Claims (6)
1. the preparation method of sheet cobalt black-two-dimensional layer carbonization titanium composite material, which is characterized in that comprise the following steps：
(1) ternary Ti3AlC2The preparation of ceramic powder：It is more than 97% ternary layered Ti using high-energy ball milling refinement purity3AlC2
Ceramic powder, ball milling condition：The mass ratio of ballstone, batch mixing and ball-milling medium is 10:1:1, rotational speed of ball-mill 400r/min, high energy
Ball-milling Time is 4h, then dries gained solid-liquid batch mixing at 50 DEG C, obtains the Ti that grain size is 8 μm3AlC2Ceramic powder；
(2) two-dimensional layer Ti3C2The preparation of nano material：By gained Ti in step (1)3AlC2Ceramic powder is immersed in HF acid solutions
In, wherein 5g Ti3AlC2Ceramic powder, which is immersed in 100mL mass concentration 40wt%HF acid solutions, to react for 24 hours；Magnetic agitation,
To ternary layered Ti3AlC2After ceramic powder carries out corrosion treatment, it is 5~6 with deionized water eccentric cleaning to pH, gained is consolidated
Body sample drying at room temperature, obtains two-dimensional layer Ti3C2Nano material；
(3) by two-dimensional layer Ti3C2Nano material and CoCL2 6H2O are dissolved in the urea liquid that concentration is 0.03~0.3mol/L
In, 5~12h is stirred to react at 85~95 DEG C, obtains reaction mixture；Solid is separated after reaction mixture is washed again
It is and dry；
(4) dry solid is kept the temperature into 1~3h in 300~450 DEG C of nitrogen or argon gas atmosphere and carries out heat treatment crystallization, obtain piece
Shape cobalt black-two-dimensional layer carbonization titanium composite material.
2. the preparation method of sheet cobalt black according to claim 1-two-dimensional layer carbonization titanium composite material, feature
It is, Ti in step (3)3C2The ratio of powder, CoCL2 6H2O and urea liquid is (50~200) mg：(0.1~1.0) g：(50
~100) mL.
3. the preparation method of sheet cobalt black according to claim 1-two-dimensional layer carbonization titanium composite material, feature
It is, reaction mixture deionized water and absolute ethyl alcohol centrifuge washing in step (3).
4. the preparation method of sheet cobalt black according to claim 1-two-dimensional layer carbonization titanium composite material, feature
It is, the solid isolated in step (3) is dried in vacuo 12~48h at 40~100 DEG C.
5. the preparation method of sheet cobalt black according to claim 1-two-dimensional layer carbonization titanium composite material, feature
It is, in the heat treatment crystallization of step (4), heating rate is 1~4 DEG C/min.
6. a kind of utilize sheet cobalt black made from preparation method described in claim 1-two-dimensional layer carbonization titanium composite material.
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| CN107934965B (en) * | 2017-12-15 | 2021-02-02 | 陕西科技大学 | Ti3C2-Co(OH)(CO3)0.5Process for preparing nano composite material |
| CN108417406A (en) * | 2018-01-30 | 2018-08-17 | 哈尔滨工业大学 | A kind of Ti3C2MXene-Co composite material and preparation methods |
| CN109211985B (en) * | 2018-09-01 | 2020-12-04 | 哈尔滨工程大学 | Flexible alkaline gas sensing chip and preparation method thereof |
| CN109941997B (en) * | 2019-03-29 | 2022-07-15 | 陕西科技大学 | Hemoglobin-like Co3O4/Ti3C2Preparation method and application of nano composite material |
| CN113176305B (en) * | 2021-04-20 | 2024-01-12 | 西安交通大学 | Composite gas-sensitive material and preparation method thereof, ethanol gas sensor and preparation method thereof |
| CN114736680B (en) * | 2022-04-22 | 2023-10-27 | 东南大学 | Preparation method of titanium carbide quantum dot based on multi-metal ion synergistic coordination modification |
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