CN100457934C - Method for preparing porous blocks of metallic glass by electrochemical eroding metal fibers - Google Patents

Method for preparing porous blocks of metallic glass by electrochemical eroding metal fibers Download PDF

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CN100457934C
CN100457934C CNB2007100644988A CN200710064498A CN100457934C CN 100457934 C CN100457934 C CN 100457934C CN B2007100644988 A CNB2007100644988 A CN B2007100644988A CN 200710064498 A CN200710064498 A CN 200710064498A CN 100457934 C CN100457934 C CN 100457934C
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tungsten filament
metallic glass
porous blocks
composite material
metal
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CN101050491A (en
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陈晓华
张勇
陈国良
张兴超
王美玲
惠希东
王自东
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
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Abstract

This invention relates to a method for preparing porous bulk metal glass by electrochemical etching of metal wire. The method comprises: selecting 5-10 wt.% NaOH or KOH solution as the electrolyte, utilizing W wire/ZrTiCuNiBeNb metal glass composite material as the anode, immersing 1/2 of the anode into the electrolyte vertically, utilizing a stainless steel plate as the cathode, and applying 5-20 V constant voltage as the etching voltage for electrochemical etching. During the electrochemical etching, hydrogen is released, and W wire is etched from top to bottom. Porous bulk metal glass can be obtained 4-12 h later. The method is simple, and the porous bulk metal glass has such advantages as uniform pore distribution, designable pore size and porosity, and uniform material structure and properties.

Description

A kind of method of preparing porous blocks of metallic glass by electrochemical eroding metal fibers
Technical field
The invention belongs to the non-crystaline amorphous metal field in the metal material field, particularly a kind of method of preparing porous blocks of metallic glass by electrochemical eroding metal fibers.
Background technology
Being born in nineteen nineties block metal glass (Bulk Metallic Glasses) is the developing important milestone of glassy alloy.Different with traditional amorphous ribbon material, block metal glass mainly is by design of alloy, rather than relies on quick refrigerative Technology to obtain.At present, the routine casting technology under the speed of cooling condition that can reach, up to a hundred compositions of alloy system can be prepared block metal glass surplus in the of existing ten, the maximum glassy alloy sample size that is obtained can reach 72 millimeters.The jumping of functional structure material that the appearance of block metal glass makes glassy alloy be used to the physics that integrates excellence, chemistry and mechanical property by single functional materials of past becomes possibility.
The research and development working result that has carried out in the world at present shows, compare with traditional crystal alloy material, bulk metallic glass materials has obvious advantages aspect the multinomial use properties, mainly shows: block metal glass have higher intensity (～2GPa), outstanding advantage such as big elastic limit (2%～3%), high wear resistance and good anti-corrosion.Just because of its special performance, make block metal glass obtained in fields such as sports goods, electronics, medical science and national defence application more and more widely (document 1, MarkTelford, Materials Today, Vol.3,2004, PP36).
Porous material is the material that a class is made up of continuous solid phase skeleton and hole.Porous material especially metal polyporous material has higher specific tenacity and specific surface area, plays various effects such as support structure, damping, buffering, separating and filtering, catalytic carrier and biomedical implant.Especially when metallic glass is made porous material, can also greatly improve its temperature-room type plasticity, because hole can limit the expansion of shear zone, can hinder, shift even start new shear zone, thereby change the distribution of shear zone, impel and form a plurality of shear zones, correspondingly improved whole plasticity, to improve whole plasticity be the same reason (document 2, H.Choi-Yim, W.L.Johnson for metal or ceramic enhancement phase in its mechanism and the metallic glass based composites, Appl.Phys.Lett., Vol.71,1997, PP3808).The porous blocks of metallic glass that has high specific strength and wear resistant corrosion resistant concurrently has very tempting application prospect, for example, as bio-medical material, be used for artificial bone, may become the strong rival of crystalline state titanium alloy porous material (document 3, A.H.Brothers, D.C.Dunand, Scripta Mater., Vol.54,2006, PP513-20).
Mostly the preparation of porous blocks of metallic glass at present is to use for reference the preparation method of common metal porous material.Such as, people such as Schroers J utilize hydration B 2O 3Particle is at Pd 43Cu 27Ni 10P 20Decomposition in the melt produces water vapor bubbles and prepares density 1.4g/cm 3, obturator-type porous blocks of metallic glass (document 4, J.Schroers, C.Veazey, W.L.Johnson, Appl.Phys.Lett., Vol.82,2003, PP370); Inoue A seminar then quenches jointly by glass melt and NaCl particle, dissolves NaCl then in water, obtain porous blocks of metallic glass (document 5, T.Wada, A.Inoue, Mater.Trans., Vol.44,2003, PP2228).Other inject high pressure hydrogen method (document 6, T.Wada, A.Inoue, Mater.Trans. in addition, Vol.45,2004, PP2761), be molded into hollow carbon microballoon method (document 7, A.H.Brothers, D.C Dunand.Appl.Phys.Lett., Vol.84,2004, PP1108) etc.The porous blocks of metallic glass hole of these method preparations is obturator-type more, and pore size and hole 1 rate are all wayward, particularly serious is, glass melt easily and gas or particle react, thereby influenced glass forming ability, the novel method of therefore inquiring into the preparation porous blocks of metallic glass is very necessary.
Summary of the invention
The object of the invention is to develop a kind of novel method of preparing porous blocks of metallic glass by electrochemical eroding metal fibers.This method is easy to simply realize that porous blocks of metallic glass void distribution state, pore size and the porosity of preparation all can design that the structure and the performance of material are even.
A kind of method of preparing porous blocks of metallic glass by electrochemical eroding metal fibers, it is characterized in that: with purity greater than 99% Zr, Ti, Cu, Ni, Be and Nb arc melting in the argon gas atmosphere of titanium absorption, make it to mix, cooling obtains ingot casting, and the weight percent of each composition is in the ingot casting: Zr:40-48%, Ti:12-14%, Cu:11-13%, Ni:9-11%, Be16-23%, Nb:0-3%.Select for use through the tungsten filament behind the aligning and in 40%HF, soak, remove surface film oxide, in acetone and alcohol, clean respectively with ultrasonic wave then.Tungsten filament after the processing is loaded in the silica tube together with the ingot casting of pulverizing, heat tracing under vacuum state, make molten metal fully penetrate in the tungsten filament, rapid quenching in saturated brine subsequently, prepare tungsten filament/ZrTiCuNiBeNb metal glass composite material, the volume fraction of tungsten filament is 20-80% in tungsten filament/ZrTiCuNiBeNb metal glass composite material.Cut into chunks perpendicular to fiber direction in tungsten filament/ZrTiCuNiBeNb metal glass composite material sample edge.Selecting the NaOH or the KOH solution of 5%-10% massfraction for use is electrolytic solution, with tungsten filament/metal glass composite material as anode, vertically about three/part immerses in the electrolytic solution, Stainless Steel Disc is as negative electrode, add the 5-20V constant voltage for corrosion voltage, carry out galvanic corrosion, reaction hydrogen is constantly overflowed, tungsten filament constantly is corroded from bottom to top, can obtain the porous blocks of metallic glass of through hole type after 4-12 hour.
The present invention has following advantage:
1, can prepare the porous blocks of metallic glass that distribution wiry, diameter and volume fraction in wire/metal glass composite material process prepare different aperture distribution, pore size and porosity by control seepage flow casting.Because the wire position in the wire/metal glass composite material of the complete corresponding seepage flow casting preparation in the position of the final porous blocks of metallic glass mesopore that obtains.This method can be prepared at an easy rate and align cellular through hole type porous blocks of metallic glass.
2, multiple non-crystaline amorphous metal system with strong glass forming ability can adopt this method to prepare porous blocks of metallic glass, and the glass forming ability of alloy influenced by wire less, be suitable for preparing larger sized porous blocks of metallic glass.
Amorphous phase in the porous blocks of metallic glass can verify by several different methods, and wherein X-ray diffraction method is the most frequently used.The X ray diffracting spectrum of amorphous structure only demonstrates the diffuse scattering peak of the disperse of a broad fully.Fig. 1 is the X-ray diffractogram of the porous blocks of metallic glass cross section of two kinds of different-alloy compositions of the present invention, as can be seen from the figure, in the effective resolution of X-ray diffractometer, do not observe any crystallization peak, illustrate that prepared porous material substrate still keeps original amorphous structure.In metallic glass, contain the crystallization phase time, will observe the Bragg diffraction peak of sharp-pointed relatively representative crystallization phase.
Pore size can determine that porosity can be measured by force microscopy by microscopically section method of direct observation in the porous blocks of metallic glass.Examine under a microscope out cross section total area S o(cm 2) and the interstitial surface area S that wherein comprises p(cm 2), again by following formula calculate porous insert porosity (document 9, Liu Peisheng, Ma Xiaoming. the porous material detection method, Beijing: metallurgical industry press, 2006, PP14):
θ＝(S p/S o)×100％
Description of drawings:
Fig. 1 is the X-ray diffractogram of the porous blocks of metallic glass cross section of two kinds of different-alloy compositions of the present invention.
Fig. 2 is the Zr of about 80% porosity of the present invention 47Ti 13Cu 11Ni 10Be 16Nb 3Porous blocks of metallic glass exterior appearance picture.
Fig. 3 is the Zr of about 20% porosity of the present invention 47Ti 13Cu 11Ni 10Be 16Nb 3The scanning electron microscopy in porous blocks of metallic glass cross section (SEM) image.
Fig. 4 is the Zr of about 60% porosity of the present invention 47Ti 13Cu 11Ni 10Be 16Nb 3The scanning electron microscopy in porous blocks of metallic glass cross section (SEM) image.
Fig. 5 is the Zr of about 80% porosity of the present invention 47Ti 13Cu 11Ni 10Be 16Nb 3The scanning electron microscopy in porous blocks of metallic glass cross section (SEM) image.
Fig. 6 is the Zr of about 80% porosity of the present invention 41.2Ti 13.8Cu 12.5Ni 10.0Be 22.5The scanning electron microscopy in porous blocks of metallic glass cross section (SEM) image.
Embodiment
Embodiment 1:
Purity is pressed nominal composition proportioning arc melting in the argon atmospher of titanium absorption greater than 99.99% Zr, Ti, Cu, Ni, Be and Nb, make it to mix, cooling obtains ingot casting.Diameter is that the tungsten filament of 250 μ m is long through being cut into 5em after aligning, and soaks in 40%HF, removes surface film oxide, cleans in acetone and alcohol respectively with ultrasonic wave then.Tungsten filament after the processing is loaded in the silica tube together with the ingot casting of pulverizing, the silica tube diameter 4mm of setting-out product place, heat tracing under vacuum state makes molten metal fully penetrate in the tungsten filament, rapid quenching in saturated brine is prepared the tungsten filament/Zr that contains 20% volume fraction approximately subsequently 47Ti 13Cu 11Ni 10Be 16Nb 3Metal glass composite material.Sample after compound edge is cut into the segment of 8mm perpendicular to fiber direction.The NaOH solution of preparing 5% massfraction is as electrolytic solution, tungsten filament/metal glass composite material is as anode, vertically about three/part immerses in the electrolytic solution, Stainless Steel Disc is as negative electrode, and institute's making alive is the 5V constant voltage, carries out galvanic corrosion, reaction is acutely carried out, have hydrogen constantly to overflow, tungsten filament constantly is corroded from bottom to top, can obtain the porous blocks of metallic glass of through hole type after 6 hours.Crystallization does not take place in the X ray diffracting spectrum in cross section as shown in Figure 1.The scanning electron microscopy picture of material section as shown in Figure 3.The hole of the about 250 μ m of diameter is evenly distributed in the metallic glass, and the interstitial surface area by aforementioned force microscopy determines the cross section total area and wherein comprises can be regarded as out porosity about 20%.
Embodiment 2:
Technical scheme such as embodiment 1, electrolytic solution select the KOH solution of 5% massfraction, the tungsten filament/Zr for preparing for use 47Ti 13Cu 11Ni 10Be 16Nb 3Metal glass composite material contains the tungsten filament of 60% volume fraction approximately, and the porosity in the final porous blocks of metallic glass that obtains is about 60%.The scanning electron microscopy picture of material section as shown in Figure 4.After testing, crystallization does not take place in the porous blocks of metallic glass that is obtained.
Embodiment 3:
Technical scheme such as embodiment 1, the tungsten filament/Zr for preparing 47Ti 13Cu 11Ni 10Be 16Nb 3Metal glass composite material contains the tungsten filament of 80% volume fraction approximately, and the porosity in the final porous blocks of metallic glass that obtains is about 80%.Material appearance pattern picture as shown in Figure 2 because the wire volume fraction is bigger, metal glass surface also is corroded and portals to come, and can obviously observe the through hole pattern.The scanning electron microscopy picture of material section as shown in Figure 5.After testing, crystallization does not take place in the porous blocks of metallic glass that is obtained.
Embodiment 4:
Technical scheme such as embodiment 1, alloying constituent is selected Zr for use 41.2Ti 13.8Cu 12.5Ni 10.0Be 22.5, tungsten filament/metal glass composite material of preparing contains the tungsten filament of 80% volume fraction approximately, and the final porous blocks of metallic glass porosity that obtains is about 80%.The scanning electron microscopy picture of material section as shown in Figure 6.Crystallization does not take place in the X ray diffracting spectrum in cross section as shown in Figure 1.
Embodiment 5:
Technical scheme such as embodiment 1, the tungsten filament/Zr for preparing 47Ti 13Cu 11Ni 10Be 16Nb 3Metal glass composite material contains the tungsten filament of 20% volume fraction approximately, and the final porous blocks of metallic glass porosity that obtains is about 20%.Institute's making alive is 15V, and the increase of voltage has obviously strengthened corrosion current, reacts more violent, has accelerated corrosion speed.After testing, crystallization does not take place in the porous blocks of metallic glass that is obtained.

Claims (1)

1. the method for a preparing porous blocks of metallic glass by electrochemical eroding metal fibers, it is characterized in that: with purity greater than 99% Zr, Ti, Cu, Ni, Be and Nb arc melting in the argon gas atmosphere of titanium absorption, make it to mix, cooling obtains ingot casting, and the weight percent of each composition is in the ingot casting: Zr:40-48%, Ti:12-14%, Cu:11-13%, Ni:9-11%, Be16-23%, Nb:0-3%; Select for use through the tungsten filament behind the aligning and in 40%HF, soak, remove surface film oxide, in acetone and alcohol, clean respectively with ultrasonic wave then; Tungsten filament after the processing is loaded in the silica tube together with the ingot casting of pulverizing, heat tracing under vacuum state, make molten metal fully penetrate in the tungsten filament, rapid quenching in saturated brine subsequently, prepare tungsten filament/ZrTiCuNiBeNb metal glass composite material, the volume fraction of tungsten filament is 20-80% in tungsten filament/ZrTiCuNiBeNb metal glass composite material; Cut into chunks perpendicular to fiber direction in tungsten filament/ZrTiCuNiBeNb metal glass composite material sample edge, selecting the NaOH or the KOH solution of 5%-10% massfraction for use is electrolytic solution, with tungsten filament/ZrTiCuNiBeNb metal glass composite material as anode, vertical three/part immerses in the electrolytic solution, Stainless Steel Disc is as negative electrode, add the 5-20V constant voltage and be corrosion voltage, carry out galvanic corrosion, reaction hydrogen is constantly overflowed, tungsten filament constantly is corroded from bottom to top, can obtain porous blocks of metallic glass after 4-12 hour.
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