CN107904645B - A kind of anodized surface processing method improving metal molybdenum foil surface-active - Google Patents
A kind of anodized surface processing method improving metal molybdenum foil surface-active Download PDFInfo
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- CN107904645B CN107904645B CN201710980921.2A CN201710980921A CN107904645B CN 107904645 B CN107904645 B CN 107904645B CN 201710980921 A CN201710980921 A CN 201710980921A CN 107904645 B CN107904645 B CN 107904645B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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Abstract
The invention discloses a kind of anodized surface processing methods for improving metal molybdenum foil surface-active, pre-treatment is carried out to molybdenum foil first, surface oxide layer is removed in hydrochloric acid, the isometric mixed liquor of sulfuric acid, is then successively cleaned by ultrasonic in acetone, dehydrated alcohol, deionized water, naturally dry is hung；Using molybdenum foil as anode, platinized platinum is containing NH as cathode4F, apply certain voltage in the electrolyte of ultrapure water, ethylene glycol and carry out anodized；Naturally dry is hung after carrying out soaked in absolute ethyl alcohol, flushing to molybdenum foil later；Reduced anneal processing is finally carried out, in a hydrogen atmosphere by the molybdenum foil after anodized, 650 DEG C of held for some time is warming up to given pace and carry out reduction treatment, the metal molybdenum foil with surface porosity has been obtained after annealing.Processing method of the present invention is simple and effective, and obtained metal molybdenum foil surface-active is greatly improved, which facilitates molybdenum foil material in the application of industrial circle.
Description
Technical field
The present invention relates to a kind of processing method for improving metal molybdenum foil surface-active more particularly to a kind of raising metal molybdenum foils
The anode oxidative treatment method of surface-active.
Background technique
Metal molybdenum is due to its good elevated temperature strength and electric conductivity and lower thermal expansion coefficient, in aerospace and electricity
Son encapsulation is widely used.But since metal molybdenum is a kind of extremely strong metal of surface inertness, it is difficult to and other metals
Compound, this causes a degree of limitation to the application of molybdenum material.Nano porous metal is because have nanoscale aperture ruler
Very little, specific surface area is larger, has some unique such as physics, chemistry and mechanical property, such as high intensity, high chemical activity and electricity
Magnetic property, application prospect is very extensive, there is important application in fields such as catalysis, gas sensing and the energy.Therefore, in molybdenum
Nano porous metal layer is prepared on surface will improve the surface-active of molybdenum.The method for preparing nano porous metal at present mainly has
De- alloyage, template, oblique incidence sedimentation and metal powder sintered method etc., but these preparation process operating processes are cumbersome, system
The standby period is longer.Therefore, find it is a kind of simple and easy, short preparation period molybdenum foil surface prepare nano porous metal layer from
And the method for improving molybdenum foil surface-active is very important.
Summary of the invention
For the prior art, anodizing is first passed through the invention proposes one kind and prepares nanoporous in Mo metallic surface
Then metal oxide layer is heat-treated to obtain the processing method of nano porous metal molybdenum by hydrogen reducing.The invention improves gold
Belong to molybdenum foil surface-active, simplifies operating procedure, shorten process cycle.
In order to solve the above-mentioned technical problem, a kind of anodic oxidation table improving metal molybdenum foil surface-active proposed by the present invention
Surface treatment method, steps are as follows:
Step 1: the pre-treatment of molybdenum platinum: molybdenum foil being impregnated 5min in hydrochloric acid, sulfuric acid mixture liquid, removes surface nature oxygen
Change layer；Then, successively molybdenum foil is cleaned by ultrasonic with acetone, dehydrated alcohol and deionized water, nature is hung after the completion of cleaning
It dries, it is spare；
Step 2: preparing electrolyte: the ingredient of electrolyte includes ammonium fluoride, ethylene glycol and ultrapure water, wherein ammonium fluoride
Molar concentration is 0.2~0.5M, and the volume ratio of ethylene glycol and ultrapure water is 6~19:1；The preparation of the electrolyte: first with container amount
Take ultrapure water, then, ammonium fluoride be added into the container, using magnetic stirrer it is uniform after add ethylene glycol, continue
It stirs evenly, obtains electrolyte；
Step 3: anodized: as anode, platinized platinum is immersed into the molybdenum foil after step 1 is cleaned as cathode
In the electrolyte of step 2 preparation, add the DC voltage of 5~35V in cathode and anode both ends, under room temperature lasting 20min；
Step 4: being cleaned and dried: the molybdenum foil after anodic oxidation being immersed in 5~10min in dehydrated alcohol, is taken out with anhydrous
Ethyl alcohol is rinsed again, and the molybdenum foil after rinsing well hangs naturally dry；
Step 5: hydrogen reducing is annealed: molybdenum foil of the step 4 after dry being put and is placed in tube furnace on a ceramic substrate, is led to
Enter hydrogen atmosphere, is warming up to 650 DEG C with the heating rate of 5~8 DEG C/min, keeps the temperature 3~5 hours, then cool to 25 with the furnace~
35 DEG C, obtain the molybdenum foil of porous surface.
Preferably, in step 2, the molar concentration of ammonium fluoride is 0.4M, and the volume ratio of ethylene glycol and ultrapure water is 19:1.
In step 3, the spacing of anode and cathode is 2~3cm.
In step 5, heating and insulating process are: being first warming up to 250 DEG C with the heating rate of 5 DEG C/min, heat preservation
Then 10min is warming up to 650 DEG C with the heating rate of 8 DEG C/min, keep the temperature 4 hours；The temperature that furnace cooling is arrived is 25 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
The molybdenum foil surface-active with nano surface porous metallic layers being prepared through the invention has obtained very big
It improves.The present invention, in molybdenum foil Surface Creation nanoporous oxide layer, is then annealed by hydrogen reducing by anodic oxidation first
Processing obtains the porous molybdenum foil of nano surface, simplifies operating procedure, shortens manufacturing cycle, is conducive to produce in enormous quantities.
Detailed description of the invention
Fig. 1 is to carry out hydrogen reducing annealing to the porous surface oxide layer molybdenum foil after the completion of anodic oxidation in embodiment 1
Temperature variation curve；
Fig. 2 is the electron scanning micrograph of nano surface porous oxide coatings molybdenum foil in embodiment 1；
Fig. 3 is that hydrogen reducing handles rear surface nanoporous molybdenum foil electron scanning micrograph in embodiment 1；
Fig. 4 is the liberation of hydrogen polarization curve of the porous molybdenum foil of nano surface and pure molybdenum foil obtained in embodiment 1；
Fig. 5 is the Tafel slope of nano surface porous molybdenum foil and pure molybdenum foil obtained in embodiment 1；
Fig. 6 is the stability test figure of the porous molybdenum foil of nano surface obtained in embodiment 1；
Fig. 7 is that hydrogen reducing handles rear surface nanoporous molybdenum foil electron scanning micrograph in embodiment 2；
Fig. 8 is that hydrogen reducing handles rear surface nanoporous molybdenum foil electron scanning micrograph in embodiment 3；
Fig. 9 is that hydrogen reducing handles rear surface nanoporous molybdenum foil electron scanning micrograph in embodiment 4；
Figure 10 is that hydrogen reducing handles rear surface nanoporous molybdenum foil electron scanning micrograph in embodiment 5.
Specific embodiment
Technical solution of the present invention is described in further detail in the following with reference to the drawings and specific embodiments, it is described specific
Embodiment is only explained the present invention, is not intended to limit the invention.
A kind of method improving molybdenum foil surface-active proposed by the present invention, main thought is with molybdenum foil anodized
The nanoporous oxide layer obtained afterwards is presoma, then handles to obtain by hydrogen atmosphere thermal reduction porous with nano surface
The molybdenum foil of metal layer.
Embodiment 1: the anodized surface processing method of metal molybdenum foil surface-active is improved, comprising the following steps:
Step 1: the pre-treatment of molybdenum platinum, including oxide layer and cleaning.
Prepare concentrated hydrochloric acid and concentrated sulfuric acid mixed liquor: the concentrated sulfuric acid for first measuring 80mL mass fraction 98% is poured into equipped with 500mL
In the beaker of ultrapure water, the concentrated hydrochloric acid that the mass fraction for then measuring equivalent again is 37% is added in beaker, is finally settled to 1L,
It stirs evenly.
Oxide layer: cutting the molybdenum foil of 20mm × 20mm (with a thickness of 17 μm) with scalpel, which is put into above-mentioned salt
5min is impregnated in sour sulfuric acid mixture liquid, removes surface natural oxidizing layer；
Cleaning: the molybdenum foil after removing natural oxidizing layer is sequentially placed into and is respectively provided with acetone, dehydrated alcohol and deionized water
Beaker in be cleaned by ultrasonic, it may be assumed that molybdenum foil is immersed in acetone cleaning agent, supersonic frequency be 40kHz under clean
10min；Then 10min is cleaned with 40kHz supersonic frequency in the beaker equipped with dehydrated alcohol；Deionized water finally is being housed
10min is cleaned with 40kHz supersonic frequency in beaker.After the completion of cleaning, molybdenum foil is hung up into naturally dry, after being cleaned
Molybdenum foil.
Step 2: preparing electrolyte: first by the ammonium fluoride (NH of 5.92g4F it) is added in 40mL ultrapure water, utilizes magnetic
Power blender stirs evenly, and then adds the ethylene glycol (i.e. the volume ratio of ethylene glycol and ultrapure water is 9:1) of 360mL, continues
It stirs evenly, obtains the ammonium fluoride (NH of 0.4M4F) electrolyte.
Step 3: anodized: as anode, platinized platinum is immersed in the molybdenum foil after step 1 is cleaned as cathode
In the beaker of electrolyte equipped with step 2 preparation, the spacing of anode and cathode is 3cm, adds 20V's in cathode and anode both ends
DC voltage, persistently 20min, completion anodized surface are handled under room temperature.
Step 4: being cleaned and dried: anodized surface, treated that molybdenum foil is put into dehydrated alcohol impregnates 10min, takes
It is rinsed with dehydrated alcohol to the clean free from admixture in surface and is depended on after out, the molybdenum foil after rinsing well hangs naturally dry, obtains
To the molybdenum foil with nano surface porous oxide coatings.
Step 5: hydrogen reducing makes annealing treatment: being obtained using the atmosphere protection tube furnace of model OTL-1200X to step 4
The molybdenum foil with nano surface porous oxide coatings arrived carries out hydrogen reducing processing, i.e., has nano surface for what step 4 obtained
The molybdenum foil of porous oxide coatings is put to be placed in tube furnace on a ceramic substrate, is passed through hydrogen atmosphere, as shown in Figure 1, first with 5 DEG C/min
Heating rate be warming up to 250 DEG C, keep the temperature 10min；Then 650 DEG C are warming up to the heating rate of 8 DEG C/min, keep the temperature 4 hours；
Last furnace cooling takes out sample to room temperature, obtains with the porous molybdenum foil of nano surface.
The sample prepared to embodiment 1 is tested and is characterized:
(1) SEM is tested: the molybdenum foil with nano surface porous oxide layer that 1 step 4 of the present embodiment is prepared
Carry out SEM test.The electron scanning micrograph of 100000 times of amplification is as shown in Fig. 2, by Fig. 2 it can be concluded that through anodic oxygen
Nanoporous oxide layer structure is formd on molybdenum foil surface after change.Fig. 3 has to be obtained after step 5 hydrogen reduction processing
The molybdenum foil of nano surface porous structure amplifies 100000 times of electron scanning micrograph, and Fig. 3 shows after hydrogen reduction,
Molybdenum foil surface obtains nano porous metal layer structure.
(2) electro-chemical test: Fig. 4 is pure molybdenum foil and has the molybdenum foil of nano surface porous metallic layers as obtained by embodiment 1
Liberation of hydrogen polarization curve, as can be seen from Figure 4 the liberation of hydrogen take-off potential of pure molybdenum foil is higher, and about -0.552V receives with surface
The liberation of hydrogen take-off potential of meter Duo Kong molybdenum foil is lower, about -0.443V, represents its surface-active since liberation of hydrogen take-off potential is smaller and gets over
Height, this shows that method proposed by the present invention improves the surface-active of metal molybdenum foil really.
Fig. 5 is the Tafel slope of pure molybdenum foil and the molybdenum foil as obtained by embodiment 1 with nano surface porous metallic layers, should
Slope is that Tafel slope is smaller to show its surface-active by measuring what polarization curve was handled to linear sweep voltammetry
It is higher.It is 173mV/dec, the Tafel slope of the porous molybdenum foil of nano surface by the Tafel slope of the available pure molybdenum foil of Fig. 5
For 83mV/dec, this shows that method proposed by the present invention improves the surface-active of metal molybdenum foil really.
Fig. 6 is to have nano surface porous metallic layers molybdenum foil in 0.5mol/L sulfuric acid electrolyte after 500 circulations
In stability test figure, stability test figure can determine the stability of molybdenum foil nano surface porous metallic layers.Sweep interval
- 1V, sweep speed 100mV/s are arrived for -0.2V.Fig. 6 shows that after 500 circulations, polarization curve is surveyed with first time
Curve deviation is unobvious, illustrates that it has good stability in 0.5mol/L sulfuric acid electrolyte.
Embodiment 2: the anodized surface processing method of metal molybdenum foil surface-active, the side of step and embodiment 1 are improved
Method is essentially identical, and difference is only, in the electrolyte that step 2 is prepared, ammonium fluoride (NH4F molar concentration) is 0.2M, ethylene glycol
Volume ratio with ultrapure water is 6:1；The finally obtained electron scanning micrograph with the porous molybdenum foil of nano surface is such as
Shown in Fig. 7.
Embodiment 3: the anodized surface processing method of metal molybdenum foil surface-active, the side of step and embodiment 1 are improved
Method is essentially identical, and difference is only, in the electrolyte that step 2 is prepared, ammonium fluoride (NH4F molar concentration) is 0.3M, ethylene glycol
Volume ratio with ultrapure water is 19:1；The finally obtained electron scanning micrograph with the porous molybdenum foil of nano surface is such as
Shown in Fig. 8.
Embodiment 4: the anode oxidative treatment method of metal molybdenum foil surface-active, the method base of step and embodiment 1 are improved
This is identical, and difference is only, in the electrolyte that step 2 is prepared, ammonium fluoride (NH4F molar concentration) is 0.4M, ethylene glycol and super
The volume ratio of pure water is 19:1；Finally obtained electron scanning micrograph such as Fig. 9 with the porous molybdenum foil of nano surface
It is shown.
Embodiment 5: the anode oxidative treatment method of metal molybdenum foil surface-active, the method base of step and embodiment 1 are improved
This is identical, and difference is only, in the electrolyte that step 2 is prepared, ammonium fluoride (NH4F molar concentration) is 0.5M, ethylene glycol and super
The volume ratio of pure water is 9:1；Finally obtain electron scanning micrograph such as Figure 10 institute with the porous molybdenum foil of nano surface
Show.
By above-mentioned multiple embodiments it can be concluded that, different ammonium fluoride (NH4F) concentration, ethylene glycol and ultrapure water volume ratio
The nanoporous molybdenum foil finally obtained is influenced most important.Water content is higher, and surface oxide layer is finer and close, obtains after annealing
Molybdenum foil surface is also comparatively dense, water content it is too low it will cause oxide on surface generate it is less, nano-porous structure can not be formed；
Ammonium fluoride (NH4F) molar concentration is bigger, and " erosion " effect of surface oxide layer is more obvious, and obtained nano-porous structure is more
Uniformly, but a large amount of appearance that are excessively high and will cause crackle, therefore suitable technological parameter is selected to have to nanoporous molybdenum foil is obtained
Significance.
The foregoing is merely the preferable specific embodiments of the present invention, but scope of protection of the present invention is not limited thereto,
Any person skilled in the art is in the technical scope that the present invention is shown, according to the technical scheme of the invention and its inventive conception
What is converted on an equal basis should be covered by the protection scope of the present invention.
Claims (4)
1. it is a kind of improve metal molybdenum foil surface-active anodized surface processing method, it is characterised in that: this method according to
Lower step carries out:
Step 1: the pre-treatment of molybdenum foil: molybdenum foil being impregnated 5min in hydrochloric acid, sulfuric acid mixture liquid, removes surface natural oxidizing layer；
Then, successively molybdenum foil is cleaned by ultrasonic with acetone, dehydrated alcohol and deionized water, naturally dry is hung after the completion of cleaning,
It is spare；
Step 2: preparing electrolyte: the ingredient of electrolyte includes ammonium fluoride, ethylene glycol and ultrapure water, wherein mole of ammonium fluoride
Concentration is 0.2 ~ 0.5 M, and the volume ratio of ethylene glycol and ultrapure water is 6 ~ 19:1；The preparation of the electrolyte: it is first measured with container super
Then ammonium fluoride is added into the container in pure water, using magnetic stirrer it is uniform after add ethylene glycol, continue to stir
Uniformly, electrolyte is obtained；
Step 3: anodized: for the molybdenum foil after step 1 is cleaned as anode, platinized platinum is immersed into step as cathode
In the electrolyte of two preparations, add the DC voltage of 5 ~ 35 V in cathode and anode both ends, under room temperature lasting 20min；
Step 4: being cleaned and dried: the molybdenum foil after anodic oxidation being immersed in 5 ~ 10min in dehydrated alcohol, dehydrated alcohol is used in taking-up
It is rinsed again, the molybdenum foil after rinsing well hangs naturally dry；
Step 5: hydrogen reducing is annealed: molybdenum foil of the step 4 after dry being put and is placed in tube furnace on a ceramic substrate, hydrogen is passed through
Gas atmosphere is warming up to 650 DEG C with the heating rate of 5 ~ 8 DEG C/min, keeps the temperature 3 ~ 5 hours, then cool to 25 ~ 35 DEG C with the furnace,
Obtain the molybdenum foil of porous surface.
2. improving the anodized surface processing method of metal molybdenum foil surface-active according to claim 1, it is characterised in that:
In step 2, the molar concentration of ammonium fluoride is 0.4 M, and the volume ratio of ethylene glycol and ultrapure water is 19:1.
3. improving the anodized surface processing method of metal molybdenum foil surface-active according to claim 1, it is characterised in that:
In step 3, the spacing of anode and cathode is 2 ~ 3 cm.
4. improving the anodized surface processing method of metal molybdenum foil surface-active according to claim 1, it is characterised in that:
In step 5, heating and insulating process are: be first warming up to 250 DEG C with the heating rate of 5 DEG C/min, keep the temperature 10min, then with
The heating rate of 8 DEG C/min is warming up to 650 DEG C, keeps the temperature 4 hours；The temperature that furnace cooling is arrived is 25 DEG C.
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| CN108950615A (en) * | 2018-07-04 | 2018-12-07 | 天津大学 | A kind of molybdenum/platinum based on surface anodization nanoporous molybdenum/silver layer shape composite material and preparation method thereof |
| CN110684990A (en) * | 2018-07-04 | 2020-01-14 | 国家纳米科学中心 | Molybdenum phosphide nano material and preparation method and application thereof |
| CN111472032A (en) * | 2020-04-29 | 2020-07-31 | 南方科技大学 | Nano porous structure metal material and preparation method thereof |
| CN113355716B (en) * | 2021-06-15 | 2022-10-04 | 北京化工大学 | Preparation of mesoporous MoO by electrochemical anodic oxidation method 2 Method (2) |
| CN116282165A (en) * | 2022-09-07 | 2023-06-23 | 北京化工大学 | Novel magnesium metal mixed ion positive electrode material and preparation method and application thereof |
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