CN104561842A - Zirconium-based amorphous alloy and preparation method thereof - Google Patents

Zirconium-based amorphous alloy and preparation method thereof Download PDF

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CN104561842A
CN104561842A CN201310515657.7A CN201310515657A CN104561842A CN 104561842 A CN104561842 A CN 104561842A CN 201310515657 A CN201310515657 A CN 201310515657A CN 104561842 A CN104561842 A CN 104561842A
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zirconium
alloy
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amorphous alloy
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CN104561842B (en
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张法亮
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BYD Co Ltd
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Abstract

The invention provides a zirconium-based amorphous alloy which is characterized in that the composition of the zirconium-based amorphous alloy is ZraTibBecMdRe in which a, b, c, d and e are atomic percentages; a is greater than or equal to 25 and less than or equal to 35, b is greater than or equal to 30 and less than or equal to 40, c is greater than or equal to 10 and less than or equal to 25, d is greater than or equal to 10 and less than or equal to 20 and e is greater than 0 and less than 2; a+b+c+d+e is equal to 100; M is one or more of Co, Cu, Cr, Hf and Nb; R is one or more of Pr, Nd, Sm, Gd, Tb, Dy and Y. The zirconium-based amorphous alloy provided by the invention can be used for preparing a large critical dimension low-density zirconium-based amorphous alloy structural material by using industrial raw materials. The component is convenient to produce and control and easy for industrial production.

Description

A kind of zirconium-base amorphous alloy and preparation method thereof
Technical field
The present invention relates to non-crystaline amorphous metal and preparation method thereof, particularly a kind of Zirconium based amorphous alloy and preparation method thereof.
Background technology
Non-crystaline amorphous metal comes across the eighties of last century sixties, and conventional non-crystaline amorphous metal system has: the Y base, La base, Pr base, Nd base etc. of Zr base, Ti base, Cu base, Fe base, Pd base, Pt base, Mg base, Co base, Ca base and rare earth based.Initial non-crystaline amorphous metal can only reach micron order due to the critical size overall dimension of amorphous (formed), and is difficult to obtain practical application.Bulk amorphous alloys is because of the microtexture of its uniqueness---longrange disorder, short range order, there is the mechanical property that crystal alloy is incomparable, as high in intensity, hardness, good springiness, anti-corrosion, wear-resisting etc., in Aeronautics and Astronautics field, the industry such as IT electronics, machinery, chemical industry has wide practical use.
Wherein, zirconium-base amorphous alloy has excellent mechanical property, is the focus of current amorphous area research, and has alloy part to be applied to the production of product, as Zr-Ti-Cu-Ni-Be alloy, for the production of golf club; Zr-Cu-Al-Ni-Nb alloy, for production mobile phone component.But the density of existing zirconium-base amorphous alloy is at 6g/cm 3to 7g/cm 3, this is for the 3c product component requiring light weight, and material density is still aobvious excessive; Though zirconium-base amorphous alloy is commercial applications, usually need the starting material of high cleanliness, due to impurity pollution and also be difficult to circulation and be recycled, high cost causes cannot heavy industrialization application.
Publication number position CN101570837A patent discloses a kind of Zirconium based amorphous alloy, it consists of (Zr 1-xti x) a1eTM a2(Cu 1-yni y) b1lTM b2be cal d, wherein a1, a2, b1, b2, c, d are elemental mole ratios, and x, y are atomic percent; Wherein 0≤x≤0.4,0≤y≤1,76≤a1+a2≤85,4≤b1+b2≤23,0≤c+d≤15, and a1+a2+b1+b2+c+d=100; Described ETM is one or more in IIIB race, VB race, IVB race, group vib, group of the lanthanides and actinide elements; Described LTM is one or more in VIIB race, VIII and IB race element.This non-crystaline amorphous metal density be about 6g/cm 3-7g/cm 3material density is still aobvious excessive.
Summary of the invention
The present invention is the technical problem that density is large, critical size is little solving existing zirconium-base amorphous alloy, provides zirconium-base amorphous alloy that a kind of density is light, critical size is large and preparation method thereof.
The invention provides a kind of zirconium-base amorphous alloy, described zirconium-base amorphous alloy consist of Zr ati bbe cm dr e, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
Present invention also offers a kind of preparation method of zirconium-base amorphous alloy, the method comprises:
1) preparation of mother alloy ingot: under shielding gas atmosphere, after non-crystaline amorphous metal raw material is carried out melting in vacuum melting furnace, cooling forming;
2) forming method: the mother alloy ingot refuse obtained by step 1), adopts gravity casting, suction casting, spray to cast or die casting mode alloy solution to be poured into cooling in forming mould and obtains non-crystaline amorphous metal;
Wherein, the add-on that described non-crystaline amorphous metal raw material comprises Zr, Ti, Be, M and R meets general formula Zr ati bbe cm dr ethe ratio of each component represented, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
Zirconium-base amorphous alloy provided by the invention, its density is 5.5g/cm 3, significantly lower than existing zirconium-base amorphous alloy density; The critical size of non-crystaline amorphous metal of the present invention is large simultaneously.The requirement requiring high 3c product can be applicable to.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the non-crystaline amorphous metal that embodiment 1 obtains.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides a kind of zirconium-base amorphous alloy, described zirconium-base amorphous alloy consist of Zr ati bbe cm dr e, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
Zirconium-base amorphous alloy provided by the invention, has enough large amorphous formation ability, and critical size can reach more than 8mm; As everyone knows, too small amorphous formation ability, be difficult to the amorphous product of the large accessory size of shaping manufacture, can only for the production of amorphous thin slice, therefore zirconium-base amorphous alloy of the present invention is suitable for manufacturing the high-strength structure part of wall thickness at below 3mm, the inner member of such as 3C Product, housing; Miniature precision high-strength parts etc. in automobile component.In non-crystaline amorphous metal of the present invention, simultaneously not containing nickel element, the existence of nickel element can produce nickel and separate out, and is easy to the allergy causing human body, and therefore zirconium-base amorphous alloy of the present invention is easy to the structure unit as 3C Product especially.
According to zirconium-base amorphous alloy provided by the present invention, in order to make that the density of non-crystaline amorphous metal is less, critical size is larger, and preferably, described M is one or both in Co, Cu; Described R is Y element.
According to zirconium-base amorphous alloy provided by the present invention, preferably, the purity of described Zr, Ti, Be, M, R is for being greater than 97%.Also comprise the metallic impurity of 0-3% in described non-crystaline amorphous metal, described metallic impurity are one or more in transition element.Zirconium-base amorphous alloy of the present invention, low-purity industrial raw materials can be adopted to manufacture, its material purity only needs to reach more than 97% weight percent purity, so just can allow the foreign matter content having 1-3wt% in material, preferable alloy element, scrap stock, reclaimed materials and inferior industrialization starting material just can be adopted for suitability for industrialized production, this can effectively reduce the production cost of zirconium-base amorphous alloy, is conducive to non-crystaline amorphous metal recycling in process of production simultaneously.
According to zirconium-base amorphous alloy provided by the present invention, preferably, the critical size of described non-crystaline amorphous metal is more than or equal to 8mm.
Present invention also offers a kind of preparation method of zirconium-base amorphous alloy, the method comprises:
1) preparation of mother alloy ingot: under shielding gas atmosphere, after non-crystaline amorphous metal raw material is carried out melting in vacuum melting furnace, cooling forming;
2) forming method: the mother alloy ingot refuse obtained by step 1), adopts gravity casting, suction casting, spray to cast or die casting mode alloy solution to be poured into cooling in forming mould and obtains non-crystaline amorphous metal;
Wherein, the add-on that described non-crystaline amorphous metal raw material comprises Zr, Ti, Be, M and R meets general formula Zr ati bbe cm dr ethe ratio of each component represented, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
According to the preparation method of zirconium-base amorphous alloy provided by the present invention, preferably, described shielding gas is one or more in argon gas, nitrogen, helium, neon, Krypton, xenon.
According to the preparation method of zirconium-base amorphous alloy provided by the present invention, preferably, described smelting temperature is 800-1200 DEG C, and smelting time is 5-40min.
According to the preparation method of zirconium-base amorphous alloy provided by the present invention, preferably, described M is one or both in Co and Cu; Described R is Y.
According to the preparation method of zirconium-base amorphous alloy provided by the present invention, preferably, the purity of described Zr, Ti, Be, M, R is 97-100%.
Below by specific embodiment, the present invention is further elaborated.
embodiment 1
According to Zr 30ti 32be 22co 6cu 9pr carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, and copper adopts the waste and old copper of 1#, purity is about 97%, and praseodymium employing purity is the praseodymium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A1 of diameter between 5mm to 30mm.
embodiment 2
According to Zr 25ti 35be 25cr 5cu 9nd carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the chromium ingot that chromium adopts purity to be greater than 99%, and copper adopts the waste and old copper of 1#, purity is about 97%, and neodymium employing purity is the neodymium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A2 of diameter between 5mm to 30mm.
embodiment 3
According to Zr 35ti 30be 24cu 10sm carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, and beryllium adopts the industrial beryllium ingot of purity 99%, and copper adopts the waste and old copper of 1#, and purity is about 97%, and samarium employing purity is the samarium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A3 of diameter between 5mm to 30mm.
embodiment 4
According to Zr 25ti 37be 17nb 20gd carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, and beryllium adopts the industrial beryllium ingot of purity 99%, and niobium adopts purity to be about the niobium bar of 99%, and gadolinium employing purity is the gadolinium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A4 of diameter between 5mm to 30mm.
embodiment 5
According to Zr 30ti 32be 22cr 6cu 9tb carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the chromium ingot that chromium adopts purity to be greater than 99%, and copper adopts the waste and old copper of 1#, purity is about 97%, and terbium adopts purity to be the terbium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A5 of diameter between 5mm to 30mm.
embodiment 6
According to Zr 35ti 40be 10co 4cu 5nb 5dy carries out alloy proportion, metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, copper adopts the waste and old copper of 1#, and purity is about 97%, niobium adopts purity to be about the niobium bar of 99%, and dysprosium employing purity is the dysprosium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A6 of diameter between 5mm to 30mm.
embodiment 7
According to Zr 30ti 32be 22co 6nb 9y carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, niobium adopts purity to be about the niobium bar of 99%, and yttrium employing purity is the yttrium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; be evacuated to 10Pa; be evacuated to 10Pa, and the argon gas being filled with 99.99% carries out atmosphere protection, carries out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A7 of diameter between 5mm to 30mm.
embodiment 8
According to Zr 30ti 32be 25co 7cu 3hf 2pr carries out alloy proportion, metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, copper adopts the waste and old copper of 1#, and purity is about 97%, hafnium adopts the hafnium metal of 98% purity, and praseodymium employing purity is the praseodymium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A8 of diameter between 5mm to 30mm.
embodiment 9
According to Zr 30ti 32be 22co 6cu 9y carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, and copper adopts the waste and old copper of 1#, purity is about 97%, and yttrium employing purity is the yttrium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A9 of diameter between 5mm to 30mm.
embodiment 10
According to Zr 35ti 29be 25co 10y carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, and beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, and yttrium employing purity is the yttrium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A10 of diameter between 5mm to 30mm.
embodiment 11
According to Zr 35ti 30be 24cu 10y carries out alloy proportion, and metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, and beryllium adopts the industrial beryllium ingot of purity 99%, and copper adopts the waste and old copper of 1#, and purity is about 97%, and yttrium employing purity is the yttrium metal of 99%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal A11 of diameter between 5mm to 30mm.
comparative example 1
According to Zr 30ti 33be 22cr 6cu 9carry out alloy proportion, metal zirconium adopts technical grade HZr-1 zirconium sponge, the technical grade titanium sponge that titanium adopts purity to be greater than 99%, and beryllium adopts the industrial beryllium ingot of purity 99%, the cobalt ingot that cobalt adopts purity to be greater than 99%, and copper adopts the waste and old copper of 1#, and purity is about 97%.
After alloy proportion completes in input vacuum melting furnace; be evacuated to 10Pa; and the argon gas being filled with 99.99% carries out atmosphere protection; carry out alloying smelting; smelting temperature is 1200 DEG C; tap to tap time is 15Min, is cast in copper mould after having smelted by alloy melt, obtains the non-crystaline amorphous metal CA1 of diameter between 5mm to 30mm.
comparative example 2
Preparing publication number according to the method for embodiment 1 is non-crystaline amorphous metal (Zr in embodiment 1 in CN101570837A 0.8ti 0.2) 78(Cu 0.667ni 0.333) 12be 10cA2.
performance test
1, XRD analysis
XRD powder diffraction analysis carries out material phase analysis to material, and to judge that whether alloy is as amorphous, this experiment carries out on the x-ray powder diffraction instrument that model is D-MAX2200PC.With copper target emanation, its incident wavelength λ=1.54060, acceleration voltage is 40KV, electric current is 20mA, and adopt step-scan, scanning step is 0.04o, the size of the present invention only non-crystaline amorphous metal A1 of testing example 1 is respectively the XRD figure of 15mm, 20mm and 25mm, and test result as shown in Figure 1.
2, critical dimension measurement
Non-crystaline amorphous metal sample A1-A11 and CA1-CA2 is cut, then by the sample section of cutting by the D/Max2500PC XRD diffractometer of Rigaku Co., Ltd. is tested, angle of diffraction is that 2theta is between 20 ° ~ 80 °, sweep velocity is 20 °/min, sweep voltage is 40Kv, and electric current is 200mA.The results are shown in Table 1.
3, density
By the density of Archimedes method test non-crystaline amorphous metal sample A1-A11 and CA1-CA2.The results are shown in Table 1.
Table 1
。
As can be seen from Table 1, adopt alloying constituent of the present invention, can adopt the raw metal of low-purity, both can obtain the critical size more than more than 8mm, wherein implementation column 8 can obtain the non-crystaline amorphous metal of critical size up to 30mm.The density of non-crystaline amorphous metal of the present invention only has 5.5g/cm simultaneously 3, therefore substantially increase the specific tenacity of alloy.And comparative example is not owing to adding rare earth element, causes the foreign gas element in alloy and some oxide compound to remove, then can greatly fall low-alloyed critical size.
As can be seen from Figure 1, any crystallization peak do not observed by the sample that embodiment 1 obtains in the effective resolution of X-ray diffractometer, illustrates that the alloy that embodiment 1 prepares is non-crystaline amorphous metal, illustrates that alloy prepared by the present invention is non-crystaline amorphous metal simultaneously yet.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. a zirconium-base amorphous alloy, is characterized in that, described zirconium-base amorphous alloy consist of Zr ati bbe cm dr e, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
2. zirconium-base amorphous alloy according to claim 1, is characterized in that, described M is one or both in Co and Cu; Described R is Y.
3. zirconium-base amorphous alloy according to claim 1, is characterized in that, the purity of described Zr, Ti, Be, M, R is 97-100%.
4. zirconium-base amorphous alloy according to claim 1, is characterized in that, also comprises the metallic impurity of 0-3% in described non-crystaline amorphous metal, and described metallic impurity are one or more in transition element.
5. zirconium-base amorphous alloy according to claim 1, is characterized in that, the critical size of described non-crystaline amorphous metal is more than or equal to 8mm.
6. a preparation method for zirconium-base amorphous alloy, is characterized in that, the method comprises:
1) preparation of mother alloy ingot: under shielding gas atmosphere, after non-crystaline amorphous metal raw material is carried out melting in vacuum melting furnace, cooling forming;
2) forming method: the mother alloy ingot refuse obtained by step 1), adopts gravity casting, suction casting, spray to cast or die casting mode alloy solution to be poured into cooling in forming mould and obtains non-crystaline amorphous metal;
Wherein, the add-on that described non-crystaline amorphous metal raw material comprises Zr, Ti, Be, M and R meets general formula Zr ati bbe cm dr ethe ratio of each component represented, wherein a, b, c, d, e are atomic percent; 25≤a≤35,30≤b≤40,10≤c≤25,10≤d≤20,0<e<2, and a+b+c+d+e=100; Described M is one or more in Co, Cu, Cr, Hf and Nb; Described R is one or more in Pr, Nd, Sm, Gd, Tb, Dy and Y.
7. preparation method according to claim 6, is characterized in that, described shielding gas is one or more in argon gas, nitrogen, helium, neon, Krypton, xenon.
8. preparation method according to claim 6, is characterized in that, described smelting temperature is 800-1200 DEG C, and smelting time is 5-40min.
9. preparation method according to claim 6, is characterized in that, described M is one or both in Co and Cu; Described R is Y.
10. preparation method according to claim 6, is characterized in that, the purity of described Zr, Ti, Be, M, R is 97-100%.
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