CN109652853A - The method of matte surface is prepared on a kind of Zr base large amorphous alloy - Google Patents

The method of matte surface is prepared on a kind of Zr base large amorphous alloy Download PDF

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Publication number
CN109652853A
CN109652853A CN201910150899.8A CN201910150899A CN109652853A CN 109652853 A CN109652853 A CN 109652853A CN 201910150899 A CN201910150899 A CN 201910150899A CN 109652853 A CN109652853 A CN 109652853A
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amorphous alloy
base
zirconium
matte
electrolyte
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CN109652853B (en
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何世伟
田荣荣
孙利
曹祚君
陈汉森
申曦
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CHANGZHOU SHIJING LIQUID METAL Co.,Ltd.
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Anhui University of Technology AHUT
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • C25F3/08Etching of refractory metals

Abstract

The invention discloses a kind of methods that matte surface is prepared on Zr base large amorphous alloy, belong to amorphous alloy technical field of surface.Method particularly includes: zirconium-base amorphous alloy is placed in the electrolytic cell for filling electrolyte, using zirconium-base amorphous alloy as anode, using graphite plate or platinized platinum as cathode, galvano-cautery is carried out under constant current conditions;Wherein, fluoride salt is contained in the electrolyte, the content > 50% of Zr element in the zirconium-base amorphous alloy, 3~4 kinds in other elements Cu, Ni, Ti, Al, Be.The present invention by way of galvano-cautery, can be prepared on zirconium-base amorphous alloy compact structure, frosted uniformly, in grayish frosted oxidation film.

Description

The method of matte surface is prepared on a kind of Zr base large amorphous alloy
Technical field
The invention belongs to amorphous alloy technical field of surface, specifically, being related to a kind of Zr base large amorphous alloy On prepare the method for matte surface.
Background technique
Amorphous alloy is also known as glassy metal, be made by high cooling velocity alloy material atom do not have enough time into There is not a kind of material in metastable state state for crystallizing and being formed in rearrangement.Its atom is in topological disorder in three-dimensional space Arrangement, has the structure of unique longrange disorder, shortrange order, thus shows excellent physics, chemistry and mechanical property.? In amorphous alloy, there is powerful glass forming ability (GFA) and roomy mistake by the zirconium-base amorphous alloy of essential element of Zr Cold liquid phase region, can use less complicated equipment be relatively easy to prepare have excellent performance, the block that size is larger, easy to form Body amorphous alloy.Therefore, zirconium-base amorphous alloy has been always the emphasis and hot spot of AMORPHOUS ALLOY since being found, in aviation The fields such as space flight, military project, electronic device, biological medicine, sports goods receive significant attention.
But the process for treating surface development time of zirconium-base amorphous alloy is shorter, being currently known by way of sandblasting can So that zirconium-base amorphous alloy obtains matte surface structure, for example, Chinese Patent Application No. are as follows: 201110421437.9, publication date For the patent document on May 2nd, 2012, a kind of amorphous alloy surface treatment process is disclosed, which utilizes metal Grain and non-metallic particle carry out spray treatment to amorphous alloy surface;Wherein, metallic particles is shot, in shot, steel sand, iron sand One or more, non-metallic particle is one of ceramics, the pellet of glass or sand material or a variety of.The amorphous that this method obtains closes Gold surface has certain roughness, but relaxation crystallization phenomenon occurs in the part that the technique easily leads to amorphous alloy, while can draw Enter impurity element.
Therefore, the new method in zirconium-base amorphous alloy surface building frosted structure is developed to be of great significance.Through retrieving, Chinese Patent Application No. are as follows: 201110179302.6, publication date are as follows: the patent document on January 2nd, 2013 discloses a kind of zirconium Base non-crystalline alloy compound material, which includes zirconium-base amorphous alloy matrix, and is attached to the zirconium-base amorphous alloy Ceramic film on matrix surface, the ceramic film fill electrolyte (containing sulphur by the way that zirconium-base amorphous alloy matrix to be placed in One of hydrochlorate, nitrate, oxalates or a variety of aqueous solutions, pH value be 6~7) electrolytic cell in, with zirconium-base amorphous alloy Matrix is anode, using stainless steel plate as cathode, is formed under conditions of plasma oxidation, the ceramic film contains ZrO2。 The hardness of the ceramic film is high, corrosion resistance and wear-resisting property are good and good with the adhesive force of zirconium-base amorphous alloy matrix, still The technique using plasma method for oxidation, energy consumption is higher, and this method is only capable of obtaining the ceramic membrane of common densification, can not obtain Obtain frosted layer.
Summary of the invention
1. to solve the problems, such as
It is easy to cause amorphous alloy relaxation occur for the existing method for preparing matte surface layer on zirconium-base amorphous alloy Crystallization phenomenon destroys substrate performance, and the problem of may introduce impurity, and the present invention is provided on a kind of Zr base large amorphous alloy The method for preparing matte surface, this method can prepare compact structure, mill by way of galvano-cautery on zirconium-base amorphous alloy Sand is uniform, is in grayish frosted oxidation film.
2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of method that matte surface is prepared on Zr base large amorphous alloy, zirconium-base amorphous alloy is placed in and fills electrolyte Electrolytic cell in, using zirconium-base amorphous alloy as anode, using graphite plate or platinized platinum as cathode, galvano-cautery is carried out under constant current conditions; Wherein, contain fluoride salt in the electrolyte;The content > 50% of Zr element, other elements in the zirconium-base amorphous alloy For 3~4 kinds in Cu, Ni, Ti, Al, Be.
Preferably, the electrolyte is NH4F and Na2SO4Aqueous solution, wherein Na2SO4It is main as supporting electrolyte Play the role of increasing the conductivity of electrolyte.
Preferably, F in the electrolyte-Concentration be 0.4~0.6mol/L, NH4F and Na2SO4Molar ratio is (2~3): 10。
Preferably, the operating temperature of the electrolyte are as follows: 20~25 DEG C.
Preferably, the current density of constant current anodic oxidation is 8~14mA/cm2, the time is 25~30min.
Preferably, the cathode area is 1~1.5 times of annode area, to reduce the point discharge of anode sample.
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) F in electrolyte used in the method for matte surface is prepared on Zr base large amorphous alloy of the present invention-For zirconium base Amorphous alloy has unique corrasion, can react with Zr under lower current potential and generate ZrF6 2-Ion, thus zirconium Base noncrystal alloy is in F-Corrosion under form hole, tri- kinds of valve-type metals of Zr, Ti, Al, which are then passivated, in another aspect matrix forms oxygen Change film, in the case where corroding the synergistic effect with oxidation filming, matte surface can be constructed by electrochemical anodic oxidation, and be prepared into The surface film oxide compact structure that arrives, frosted uniformly, gray, the corrosion resistance of amorphous alloy is also improved;
(2) the method F of matte surface is prepared on Zr base large amorphous alloy of the present invention-Excessive concentration will lead to corrosion speed Rate is excessive, can not form oxidation film;F-Concentration it is too low then can corrosion rate it is inadequate, oxidation film can be formed but be difficult to form frosted Surface;And current density is excessive can form oxidation film, but is difficult to form matte surface, current density is too small, then is difficult to be formed Oxidation film;Inventor obtains F by largely testing and analyzing-Concentration preferably 0.4~0.6mol/L, current density preferably 8 ~14mA/cm2When, the synergistic effect of corrosion and oxidation filming is preferable, so as to form matte surface;
(3) anode oxidation process involved in the method for matte surface is prepared on Zr base large amorphous alloy of the present invention, It can be completed under room temperature, synthesis temperature is low, and noncrystal substrate will not be made to generate crystallization or relaxation phenomena and lead to amorphous alloy performance It is destroyed;And anodic oxidation is to be in the parent metal on surface directly with the anionic reactive in selected media, is allowed to be formed The product of itself conversion, actually controlled corrosion of metal process, in-situ construction binding force is strong, favorable reproducibility.
Detailed description of the invention
Fig. 1 is the flow chart that the method for matte surface is prepared on Zr base large amorphous alloy of the present invention;
Fig. 2 is the zirconium-base amorphous alloy piece before preparing matte surface layer;
Fig. 3 is the zirconium-base amorphous alloy piece after preparing matte surface layer;
Fig. 4 is the stereoscan photograph of the zirconium-base amorphous alloy piece before preparing matte surface layer;
Fig. 5 is the stereoscan photograph of the zirconium-base amorphous alloy piece after preparing matte surface layer;
Fig. 6 is the XRD spectrum of zirconium-base amorphous alloy piece before and after preparing matte surface layer.
Specific embodiment
The present invention is further described below combined with specific embodiments below.
Embodiment 1
As shown in Figure 1, zirconium-base amorphous alloy piece after pre-treatment is (as shown in Figure 2) to be used as anode, cathode is platinized platinum, Anode and cathode is placed in electrolyte, temperature be 20 DEG C, current density 14mA/cm2, electrolysis time be 30 minutes under conditions of Anodic oxidation is carried out, anode alloy piece naturally dry after ethyl alcohol cleans is taken out, frosted table can be prepared on zirconium-base amorphous alloy Face (as shown in Figure 3).Wherein, platinized platinum cathode area is 1.5 times of alloy sheet annode area, and electrolyte used is by NH4F and Na2SO4It is dissolved in the water obtained, NH4F and Na2SO4Dissolved molar ratio is 2:10, F-Concentration be 0.4mol/L.
The zirconium-base amorphous alloy surface that the present embodiment is prepared is in frosted structure, and oxidation film layer compact structure, frosted Uniformly, surface is in light gray.It is observed under scanning electron microscope, there is a large amount of crystal grain in anodic oxidation rear surface, and crystal grain is uniformly distributed, And compact crystallization.It can be seen that from XRD spectrum, crystalline state ZrO occurs in zirconium-base amorphous alloy surface after anodic oxidation2And Al2O3Spread out Penetrate peak.
Embodiment 2
As shown in Figure 1, the zirconium-base amorphous alloy piece after pre-treatment is as anode, cathode is graphite plate, by anode and cathode Be placed in electrolyte, temperature be 25 DEG C, current density 14mA/cm2, electrolysis time be 30 minutes under conditions of carry out anode Oxidation takes out anode alloy piece naturally dry after ethyl alcohol cleans, matte surface can be prepared on zirconium-base amorphous alloy.Wherein, Graphite cathode area is equal with alloy sheet annode area, and electrolyte used is by NH4F and Na2SO4It is dissolved in the water obtained, NH4F with Na2SO4Dissolved molar ratio is 2:10, F-Concentration be 0.5mol/L.
The zirconium-base amorphous alloy surface that the present embodiment is prepared is in frosted structure, and oxidation film layer compact structure, frosted Uniformly, surface is in light gray.
Embodiment 3
As shown in Figure 1, the zirconium-base amorphous alloy piece after pre-treatment is as anode, cathode is platinized platinum, and anode and cathode is set In electrolyte, temperature be 20 DEG C, current density 8mA/cm2, electrolysis time be 25 minutes under conditions of carry out anodic oxygen Change, takes out anode alloy piece naturally dry after ethyl alcohol cleans, matte surface can be prepared on zirconium-base amorphous alloy.Wherein, platinum Piece cathode area is 1.5 times of alloy sheet annode area, and electrolyte used is by NH4F and Na2SO4It is dissolved in the water obtained, NH4F With Na2SO4Dissolved molar ratio is 3:10, F-Concentration be 0.6mol/L.
The zirconium-base amorphous alloy surface that the present embodiment is prepared is in frosted structure, and oxidation film layer compact structure, frosted Uniformly, surface is in light gray.
Embodiment 4
As shown in Figure 1, the zirconium-base amorphous alloy piece after pre-treatment is as anode, cathode is graphite plate, by anode and cathode Be placed in electrolyte, temperature be 20 DEG C, current density 8mA/cm2, electrolysis time be 30 minutes under conditions of carry out anode Oxidation takes out anode alloy piece naturally dry after ethyl alcohol cleans, matte surface can be prepared on zirconium-base amorphous alloy.Wherein, Graphite cathode area is equal with alloy sheet annode area, and electrolyte used is by NH4F and Na2SO4It is dissolved in the water obtained, NH4F with Na2SO4Dissolved molar ratio is 3:10, F-Concentration be 0.6mol/L.
The zirconium-base amorphous alloy surface that the present embodiment is prepared is in frosted structure, and oxidation film layer compact structure, frosted Uniformly, surface is in light gray.
Embodiment 5
As shown in Figure 1, the zirconium-base amorphous alloy piece after pre-treatment is as anode, cathode is platinized platinum, and anode and cathode is set In electrolyte, temperature be 25 DEG C, current density 14mA/cm2, electrolysis time be 25 minutes under conditions of carry out anodic oxygen Change, takes out anode alloy piece naturally dry after ethyl alcohol cleans, matte surface can be prepared on zirconium-base amorphous alloy.Wherein, platinum Piece cathode area is 1.5 times of alloy sheet annode area, and electrolyte used is by NH4F and Na2SO4It is dissolved in the water obtained, NH4F With Na2SO4Dissolved molar ratio is 3:10, F-Concentration be 0.5mol/L.
The zirconium-base amorphous alloy surface that the present embodiment is prepared is in frosted structure, and oxidation film layer compact structure, frosted Uniformly, surface is in light gray.

Claims (6)

1. preparing the method for matte surface on a kind of Zr base large amorphous alloy, it is characterised in that: zirconium-base amorphous alloy to be placed in Fill in the electrolytic cell of electrolyte, using zirconium-base amorphous alloy as anode, using graphite plate or platinized platinum as cathode, under constant current conditions into Row galvano-cautery;Wherein, fluoride salt is contained in the electrolyte, the content > of Zr element in the zirconium-base amorphous alloy 50%, 3~4 kinds in other elements Cu, Ni, Ti, Al, Be.
2. preparing the method for matte surface on a kind of Zr base large amorphous alloy according to claim 1, it is characterised in that: The electrolyte is NH4F and Na2SO4Aqueous solution.
3. preparing the method for matte surface on a kind of Zr base large amorphous alloy according to claim 2, it is characterised in that: F in the electrolyte-Concentration be 0.4~0.6mol/L, NH4F and Na2SO4Molar ratio is (2~3): 10.
4. preparing the method for matte surface on a kind of Zr base large amorphous alloy according to claim 3, it is characterised in that: The operating temperature of the electrolyte are as follows: 20~25 DEG C.
5. preparing the method for matte surface on a kind of Zr base large amorphous alloy according to claim 1, it is characterised in that: The current density of constant current anodic oxidation is 8~14mA/cm2, the time is 25~30min.
6. preparing the method for matte surface on a kind of Zr base large amorphous alloy according to claim 1, it is characterised in that: The cathode area is 1~1.5 times of annode area.
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CN111058076B (en) * 2019-12-30 2020-11-20 安徽工业大学 Zr-based high-entropy alloy material and method for synthesizing porous spherical structure on surface of Zr-based high-entropy alloy

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