CN109967735A - The method for preparing copper fiber felt as template using graphene - Google Patents
The method for preparing copper fiber felt as template using graphene Download PDFInfo
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- CN109967735A CN109967735A CN201910374385.0A CN201910374385A CN109967735A CN 109967735 A CN109967735 A CN 109967735A CN 201910374385 A CN201910374385 A CN 201910374385A CN 109967735 A CN109967735 A CN 109967735A
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- graphene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/062—Fibrous particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention belongs to metal fiber felt technical fields, in particular to the method for preparing copper fiber felt as template using graphene, comprising: the preparation of step 1) precursor solution；2) freeze-drying process；3) high-temperature heat treatment.Preparation method of the present invention is with CuCl2For copper source, with Ar and NH3Gaseous mixture be reducing agent, NH3Gas is by CuCl2It is reduced to copper simple substance particle, copper simple substance particle is captured by graphene, is heat-treated by 950~1050 DEG C, and the copper fiber felt being made of the copper fiber that average diameter is 2~8 μm is successfully prepared.The copper fiber felt has porous structure, and large specific surface area has prospect to apply as bone implant, lithium metal battery, fuel cell, catalyst, catalyst carrier, filtering and separation material, heat exchanger and water-oil separating material etc..
Description
Technical field
The invention belongs to metal fiber felt technical fields, in particular to the side of copper fiber felt is prepared using graphene as template
Method.
Background technique
Metallic fiber (sintering) felt is made of metallic fiber, forms sintered neck and shape by the overlapped points in metallic fiber
At felt structure.The material of metallic fiber (sintering) felt includes stainless steel, carbon steel, cast iron, copper, al and ni etc..Wherein, copper fiber
(sintering) felt has the function of porous structure, certain mechanical property and physical and chemical performance and becomes a kind of novel structure/mono-
Body material has prospect as bone implant, lithium metal battery, fuel cell, catalyst, catalyst carrier, filtering and separation
Material, heat exchanger and water-oil separating material etc. and apply.The typical production process of traditional copper fiber sintering felt serving is[1–3]: (1)
Copper fiber is cut from copper rod surface using lathe (such as multiple tooth cutting tool)；(2) by obtained copper fiber according to its draw ratio into
Row classification is mixed and is spread and be dispersed in stainless steel mould, while filling Al2O3Porosity of the powder to keep its certain；(3) it installs
The upper cover of stainless steel mould, blending bolt fastening；(4) stainless steel mould is placed in atmosphere furnace, in weakly reducing atmosphere (such as H2Gas
Atmosphere), under micro-positive pressure (such as 0.3MPa) in 850~950 DEG C of 30~60min of heat preservation；(5) after furnace cooling, sample is taken out, so
After wash Al2O3Powder obtains copper fiber sintering felt serving.
There are certain deficiencies for the typical production process of copper fiber sintering felt serving: 1) complex process, higher cost；2) due to
Al2O3The use of powder, during heat treatment Al2O3And/or Al particle (Al2O3It is reduced to Al simple substance) copper fibre can be adhered to
The surface of dimension, they may weaken the physical and chemical performance of copper fiber sintering felt serving as impurity；3) in copper fiber sintering felt serving
Copper fiber is relatively large in diameter, and is typically larger than and is equal to 100 μm, thereby reduces the specific surface area of copper fiber sintering felt serving.
Bibliography
[1]Yong Tang,Wei Yuan.Minqiang Pan and Zhenping Wan,Feasibility study
of porous copper fiber sintered felt:A novel porous flow field in proton
exchange membrane fuel cells.International Journal of Hydrogen Energy 2010；
35:9661–9677.
[2] Tang Yong, Hu Jinyi, cycle, the town Zhang Xu, a kind of water-oil separating copper fiber felt of super-hydrophobic/super-oleophilic of Yuan Wei
Preparation method Chinese invention patent, 201410846141.5.
[3] Tang Yong, Li Hui, Liu Zhongshan, a kind of copper fiber felt material and its system with nano-porous surface structure of Zou Tong
Preparation Method Chinese invention patent, 201410637659.8.
Summary of the invention
Deficiency existing for typical production process for traditional copper fiber sintering felt serving, the invention discloses using graphene as mould
The method that plate prepares copper fiber felt, which simplifies, at low cost, and the copper fiber in obtained copper fiber felt is straight
Diameter is smaller, and average value is 2~8 μm.
Technical scheme is as follows:
The method for preparing copper fiber felt as template using graphene comprising following steps:
1) preparation of precursor solution:
(1) by CuCl2·2H2O is dissolved in deionized water or distilled water, obtains CuCl2Solution；
(2) to CuCl2Dehydrated alcohol and graphene powder are added in solution, obtains graphene suspension I；
(3) graphene suspension I is successively ultrasonically treated, be vacuum-treated, be ultrasonically treated, until graphene is totally submerged
CuCl2Solution obtains graphene suspension II；
2) freeze-drying process: the graphene suspension II in step 1) is freeze-dried 24~36h, is loaded
CuCl2Graphene powder；
3) high-temperature heat treatment:
(1) powder obtained in step 2) is placed in the porcelain boat or quartz boat of about two make-ups；
(2) the two porcelain boats or quartz boat are placed in tube furnace；
(3) in Ar gas atmosphere, tube furnace is warming up to 550~650 DEG C；
(4) Ar air to close is closed, opens simultaneously Ar and NH3Gaseous mixture, NH in gaseous mixture3Gas content is 30~60%, will be managed
Formula furnace is in 550~650 DEG C of 15~25min of heat preservation；
(5) by Ar and NH3Gaseous mixture close, open simultaneously Ar gas, tube furnace be warming up to 950~1050 DEG C, and protect
30~60min of temperature；
(6) in Ar gas atmosphere, tube furnace is cooled to room temperature, obtains the copper fiber felt.
Graphene, CuCl in the step 1)2·2H2O, the mass ratio of deionized water or distilled water, dehydrated alcohol is
1:28~56:400~1700:100~200.
The ultrasonic treatment condition is that 200~2500W is ultrasonically treated 5~30min.
The vacuum processing conditions are that 0.0001~0.01MPa is vacuum-treated 3~10min.
The inlet end of two porcelain boats or quartz boat in the step 3) retains 5~40mm2Gap.
Ar gas, Ar and the NH3Gaseous mixture flow velocity be 5~40mL/min.
The heating rate of the tube furnace is 5~40 DEG C/min.
We have discovered that in the present invention when heat treatment temperature is 550~650 DEG C, CuCl2By NH3Gas is reduced to copper
Simple substance particle, copper simple substance particle are captured under the driving of carrier gas by graphene, and captured copper simple substance particle will be used as it is secondary
Template further captures the copper simple substance particle of floating, and then becomes copper fiber at 950~1050 DEG C, and in the overlapped points of copper fiber
Sintered neck is formed, copper fiber felt is formed.Meanwhile graphene is gradually removed to outside tube furnace under the driving of carrier gas.
Compared with prior art, the advantages and positive effects of the present invention are:
(1) present invention reports the method for preparing copper fiber felt as template using graphene, burns relative to traditional copper fiber
The preparation process of felt is tied, the method and process that the present invention reports is simple.
(2) preparation method that the present invention reports is without using Al2O3Powder, therefore Al will not be introduced on the surface of copper fiber2O3
And/or Al granule foreign.
(3) relative to traditional copper fiber sintering felt serving, the diameter for the copper fiber in copper fiber felt that the present invention reports is smaller,
Its average value is 2~8 μm, therefore the large specific surface area of copper fiber felt, is conducive to the exposure of its active site.
(4) in the high-temperature heat treatment process for the preparation method that the present invention reports, heating rate is fast, the energy saving and time.
Detailed description of the invention
Fig. 1 is the XRD spectrum of copper fiber felt prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM picture of the surface topography of copper fiber felt prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention is further explained and is illustrated below with reference to embodiment, but the present invention is not limited in any way.With
Raw material used in lower embodiment is commercially available analysis pure raw material.
Embodiment 1
1) preparation of precursor solution:
(1) by 14g CuCl2·2H2O is dissolved in 425g deionized water, obtains CuCl2Solution；
(2) to CuCl250g dehydrated alcohol and 0.25g graphene powder are added in solution, obtains graphene suspension I；
(3) by graphene suspension I, successively 2000W ultrasonic treatment 15min, 0.001MPa vacuum processing 7min, 1500W surpasses
Sonication 15min, until graphene is totally submerged CuCl2Solution obtains graphene suspension II.Graphene in precursor solution,
CuCl2·2H2O, distilled water, dehydrated alcohol mass ratio be 1:56:1700:200.
2) freeze-drying process: the graphene suspension II in step 1) is freeze-dried 36h, obtains CuCl2's
Graphene powder.
3) high-temperature heat treatment:
(1) powder obtained in step 2) is placed in the quartz boat of about two make-ups, the air inlet of the two quartz boats
End retains 20mm2Gap；
(2) the two quartz boats are placed in microwave tube type oven；
(3) in the Ar gas atmosphere that flow velocity is 5mL/min, microwave tube type oven is warming up to 600 with the rate of 35 DEG C/min
℃；
(4) Ar gas is closed, Ar and NH are opened simultaneously3Gaseous mixture, NH in gaseous mixture3The content of gas is 50%, gaseous mixture
Flow velocity is 10mL/min, by microwave tube type oven in 600 DEG C of heat preservation 25min；
(5) Ar and NH is closed3Gaseous mixture, open simultaneously Ar gas, the flow velocity of Ar gas is 15mL/min, by microwave tube type oven
1000 DEG C are warming up to the rate of 40 DEG C/min, and keeps the temperature 60min；
(6) continue in the Ar gas atmosphere that flow velocity is 25mL/min, microwave tube type oven is cooled to room temperature, copper fiber is obtained
Felt.
The XRD spectrum of prepared copper fiber felt is as shown in Figure 1, diffraction maximum all in map belongs to elemental copper
(JCPDS04-0836), illustrate that copper fiber felt is made of elemental copper.The SEM picture of the surface topography of copper fiber felt is as shown in Fig. 2, copper
Contain a large amount of micron order holes in fibrofelt, and the diameter of copper fiber is 5.4 ± 2.1 μm.
Embodiment 2
1) preparation of precursor solution:
(1) by 10.5g CuCl2·2H2O is dissolved in 250g distilled water, obtains CuCl2Solution；
(2) to CuCl237.5g dehydrated alcohol and 0.25g graphene powder are added in solution, obtains graphene suspension I；
(3) by graphene suspension I, successively 2500W is ultrasonically treated 10min, 0.0001MPa vacuum processing 3min, 1000W
It is ultrasonically treated 25min, until graphene is totally submerged CuCl2Solution obtains graphene suspension II；Graphite in precursor solution
Alkene, CuCl2·2H2O, deionized water, dehydrated alcohol mass ratio be 1:42:1000:150.
2) freeze-drying process: the graphene suspension II in step 1) is freeze-dried 30h, obtains CuCl2's
Graphene powder.
3) high-temperature heat treatment:
(1) powder obtained in step 2) is placed in the quartz boat of about two make-ups, the air inlet of the two quartz boats
End retains 5mm2Gap；
(2) the two quartz boats are placed in microwave tube type oven；
(3) in the Ar gas atmosphere that flow velocity is 10mL/min, microwave tube type oven is warming up to 550 with the rate of 25 DEG C/min
℃；
(4) Ar gas is closed, Ar and NH are opened simultaneously3Gaseous mixture, NH in gaseous mixture3The content of gas is 30%, gaseous mixture
Flow velocity is 20mL/min, by microwave tube type oven in 550 DEG C of heat preservation 20min；
(5) Ar and NH is closed3Gaseous mixture, open simultaneously Ar gas, the flow velocity of Ar gas is 30mL/min, by microwave tube type oven
950 DEG C are warming up to the rate of 30 DEG C/min, and keeps the temperature 45min；
(6) continue in the Ar gas atmosphere that flow velocity is 15mL/min, microwave tube type oven is cooled to room temperature, copper fiber is obtained
Felt.
The XRD spectrum of prepared copper fiber felt illustrates that copper fiber felt is made of elemental copper.The surface topography of copper fiber felt
SEM picture show copper fiber felt in contain a large amount of micron order holes, and the diameter of copper fiber be 5.0 ± 2.6 μm.
Embodiment 3
1) preparation of precursor solution:
(1) by 28g CuCl2·2H2O is dissolved in 400g distilled water, obtains CuCl2Solution；
(2) to CuCl2100g dehydrated alcohol and 1g graphene powder are added in solution, obtains graphene suspension I；
(3) by graphene suspension, successively 200W is ultrasonically treated 30min, 0.01MPa vacuum processing 10min, 800W ultrasound
5min is handled, until graphene is totally submerged CuCl2Solution obtains graphene suspension II；Graphene in precursor solution,
CuCl2·2H2O, distilled water, dehydrated alcohol mass ratio be 1:28:400:100.
2) freeze-drying process: for 24 hours by the graphene suspension II freeze-drying in step 1), CuCl is obtained2's
Graphene powder.
3) high-temperature heat treatment:
(1) powder obtained in step 2) is placed in the porcelain boat of about two make-ups, the inlet ends of the two porcelain boats it
Between retain 40mm2Gap；
(2) the two porcelain boats are placed in common (heating wire) tube furnace；
(3) in the Ar gas atmosphere that flow velocity is 35mL/min, common tube furnace is warming up to 650 with the rate of 5 DEG C/min
℃；
(4) Ar gas is closed, Ar and NH are opened simultaneously3Gaseous mixture, NH in gaseous mixture3The content of gas is 60%, gaseous mixture
Flow velocity is 40mL/min, by common tube furnace in 650 DEG C of heat preservation 15min；
(5) Ar and NH is closed3Gaseous mixture, open simultaneously Ar gas, the flow velocity of Ar gas is 38mL/min, by common tube furnace
1050 DEG C are warming up to the rate of 10 DEG C/min, and keeps the temperature 30min；
(6) continue in the Ar gas atmosphere that flow velocity is 30mL/min, common tube furnace is cooled to room temperature, copper fiber is obtained
Felt.
The XRD spectrum of prepared copper fiber felt illustrates that copper fiber felt is made of elemental copper.The surface topography of copper fiber felt
SEM picture show copper fiber felt in contain a large amount of micron order holes, and the diameter of copper fiber be 4.2 ± 1.7 μm.
The method for preparing copper fiber felt as template using graphene that the present invention is disclosed and proposed, those skilled in the art can lead to
Cross reference present disclosure, the appropriate links such as condition route that change are realized, although method and technology of preparing of the invention by compared with
Good examples of implementation are described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to herein
The methods and techniques route is modified or reconfigures, to realize final technology of preparing.In particular, it should be pointed out that
All similar replacements and change are apparent to those skilled in the art, they are considered as being included in this hair
In bright spirit, range and content.
Claims (7)
1. the method for preparing copper fiber felt as template using graphene, it is characterised in that the following steps are included:
1) preparation of precursor solution:
(1) by CuCl2·2H2O is dissolved in deionized water or distilled water, obtains CuCl2Solution；
(2) to CuCl2Dehydrated alcohol and graphene powder are added in solution, obtains graphene suspension I；
(3) graphene suspension I is successively ultrasonically treated, be vacuum-treated, be ultrasonically treated, until graphene is totally submerged CuCl2It is molten
Liquid obtains graphene suspension II；
2) freeze-drying process: the graphene suspension II in step 1) is freeze-dried 24~36h, obtains CuCl2Stone
Black alkene powder；
3) high-temperature heat treatment:
(1) powder obtained in step 2) is placed in the porcelain boat or quartz boat of about two make-ups；
(2) the two porcelain boats or quartz boat are placed in tube furnace；
(3) in Ar gas atmosphere, tube furnace is warming up to 550~650 DEG C；
(4) Ar air to close is closed, opens simultaneously Ar and NH3Gaseous mixture, NH in gaseous mixture3Gas content is 30~60%, by tube furnace
In 550~650 DEG C of 15~25min of heat preservation；
(5) by Ar and NH3Gaseous mixture close, open simultaneously Ar gas, tube furnace be warming up to 950~1050 DEG C, and keep the temperature 30~
60min；
(6) in Ar gas atmosphere, tube furnace is cooled to room temperature, obtains the copper fiber felt.
2. the method as described in claim 1, it is characterized in that graphene, CuCl in the step 1)2·2H2O, deionization
The mass ratio of water or distilled water, dehydrated alcohol is 1:28~56:400~1700:100~200.
3. the method as described in claim 1, it is characterized in that ultrasonic treatment condition is that 200~2500W is ultrasonically treated 5~30min.
4. the method as described in claim 1, it is characterized in that vacuum processing conditions be 0.0001~0.01MPa be vacuum-treated 3~
10min。
5. the method as described in claim 1, it is characterized in that the inlet end of two porcelain boats or quartz boat in the step 3)
Retain 5~40mm2Gap.
6. the method as described in claim 1, it is characterized in that Ar gas, Ar and NH3Gaseous mixture flow velocity be 5~40mL/min.
7. the method as described in claim 1, it is characterized in that in the step 3) heating rate of tube furnace be 5~40 DEG C/
min。
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| US6346136B1 (en) * | 2000-03-31 | 2002-02-12 | Ping Chen | Process for forming metal nanoparticles and fibers |
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