CN1176240C - Granular nitride/amorphous alloy based composition - Google Patents

Granular nitride/amorphous alloy based composition Download PDF

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CN1176240C
CN1176240C CNB011140429A CN01114042A CN1176240C CN 1176240 C CN1176240 C CN 1176240C CN B011140429 A CNB011140429 A CN B011140429A CN 01114042 A CN01114042 A CN 01114042A CN 1176240 C CN1176240 C CN 1176240C
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amorphous alloy
alloy
aln
nitride
nitride particles
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CN1390970A (en
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周畅然
徐坚
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Institute of Metal Research of CAS
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Abstract

The present invention provides a composite material of nitride particles and an amorphous alloy base. The volume percentage of the nitride particles to the amorphous alloy base is AxBy, wherein x=5 to 30, y=70 to 95, x+y=100, A is any one of AlN, Si3N4, TiN, ZrN and TaN ceramic particles, and B is a polynary amorphous alloy forming the base. The size of the nitride particles is from 10 nanometers to 100 micrometers, the amorphous alloy base is characterized in that an obvious glass transformation occurs before a crystallizing transformation, and the temperature interval width (delta T) of super-cooled liquid is larger than 30 DEG C. Compared with an amorphous alloy not containing the nitride particles, the composite material with the nitride particles dispersedly distributed on the amorphous alloy base is better in thermal stability.

Description

Granular nitride/amorphous alloy based matrix material
The present invention relates to a kind of matrix material.
Amorphous alloy has high yield strength, elastic strain limit and higher fracture toughness property at present, but shortage stretching plastic, its application is restricted, by introducing the second phase crystal grain, can suppress the germinating of partial cut band, promote the formation of multiple shear bands, thereby strengthen non-prosperous attitude alloy substrate, improve its tough, plasticity, at present, comprise following a few class with industry as strengthening the body second phase particle: refractory metals such as (1) tantalum, molybdenum, tungsten; (2) MgO, CeO, Al 2O 3, Y 2O 3Deng oxide ceramics; (3) carbide ceramics such as WC, TiC, SiC, ZrC, the particulate size is at tens to 100 microns, the method that strengthens body introducing amorphous alloy mainly comprises: (1) directly is added into the second phase particle in the alloy melt, promptly form matrix material after the melt cooling, its defective is to be difficult for realizing the uniform distribution of the second phase particle on matrix; (2) the second phase particle and amorphous alloy powder machinery is mixed, realize the uniform distribution of the second phase particle on matrix, this method is used for the oxide compound second phase particle dispersion in early days in the superalloy matrix, improve the hot strength of superalloy, its shortcoming is the impurity element that is easy to introduce from ball-milling medium and atmosphere, as iron, oxygen, carbon etc.
It is matrix with the amorphous alloy with obvious glass transition that purpose of the present invention provides a kind of, introduce nitride particles as strengthening body, form in " granular nitride/amorphous alloy based matrix material ", the introducing of an amount of nitride helps improving the thermostability and the mechanical property of single-phase amorphous alloy, simultaneously, but the introducing of nitride does not destroy the processing characteristics of matrix amorphous alloy in the supercooled liquid temperature range, nitrogenate particulate matrix material can be by melt casting, technology such as powder metallurgy are prepared into block materials, utilize its superplasticity, can realize the near clean formation type of complicated shape component in the supercooled liquid temperature range.
The matrix material that the present invention is granular nitride/amorphous alloy based, can implement material according to different service requirementss selects and design, comprise type, volume relative quantity, mean particle size, the particle shape of nitride particles and the type that constitutes the amorphous alloy of matrix, nitride particles can be selected common AlN, Si 3N 4, TiN, ZrN, TaN etc., the particulate mean particle size can be 10 nanometers (nm) to 100 microns (μ m) scopes, matrix alloy can be chosen in any in the multicomponent amorphous alloy that obvious glass transition and supercooled liquid temperature range appear before taking place in crystallization change, for example, alloys such as Al-Ni-Co-Y, Mg-Cu-Y, Mg-Nd-Y, Fe-Zr-B, Fe-Co-Ni-Nb-Zr-B, Ni-Co-Zr-Ti, Zr-Al-Ni-Cu, Zr-Ti-Nb-Ni-Cu, Cu-Ti-Ni-Zr, Pd-Ni-Cu-P, La-Al-Ni-Cu-Co.The ratio of nitride particles and matrix amorphous alloy (volume percent) is A xB y, x=5～30, y=70～95, x+y=100, A are AlN, Si 3N 4, in TiN, ZrN, the TaN ceramic particle any, B is for constituting the multicomponent amorphous alloy of body material.
The granular nitride/amorphous alloy based matrix material of the present invention contains the multicomponent alloy of element more than three kinds, or be used for obtaining by any or several compound the making in the multiple material preparation method, depend on required material forms, as powder, strip, ingot casting, plate etc., (1) can be prepared into the gram level to feather weight thin band material (30～900 microns of thickness) in batches by single roller melt-spun method, can be by ultrasonic atomizatio, in the methods such as mechanical alloying any obtains the gram level to feather weight composite material powder in batches, if as body material, can directly be prepared into block materials by conventional melt casting process with the stronger alloy of some intrinsic amorphous formation ability; (2) can adopt following method to realize the evenly mixed of nitride particles and matrix alloy; (1) nitride particles is added in the alloy melt, after (electromagnetism or machinery) stirs melt is cooled off rapidly, nitride particles is freezed in matrix, alloy melt forms amorphous alloy simultaneously; (2) nitride particles and powdered alloy (or chip, fragment) is mixed through mechanical mill, powdered alloy (or chip, fragment) can be pre-amorphous powder (or chip, fragment), after the presmelting alloying broken powder (or chip, fragment), with have the element powders mixture of the alloy phase of obvious glass transition feature with chemical composition; (3) utilize high-octane mechanical mill (being mechanical alloying) uniform distribution of the decrystallized and nitride particles of matrix alloy can be finished simultaneously, and can make initial nitride particles further broken, reach nanoscale, form " nitride nano particle/amorphous alloy base composite material ".
The present invention compares as the matrix material that strengthens body with using the micron order nitride particles, and " nitride nano particle/amorphous alloy base composite material " has better thermostability and mechanical property.
Compare with conventional polycrystalline metal material, amorphous alloy (also claiming metallic glass) is because the long-range of structure is unordered and do not have a crystal boundary, therefore have high strength and toughness, characteristic such as corrosion-resistant and anti-oxidant, some amorphous alloy can show tangible glass transition and promptly change supercooled liquid into by amorphous solid before crystallization change takes place, the sudden change that is attended by viscosity and specific heat usually forms the supercooled liquid temperature range Δ T of broad, and (Δ T is defined as the starting temperature T that crystallization takes place amorphous alloy in continuous heat-processed xWith glass transformation temperature T gDifference, i.e. Δ T=T x-T g), have now found that, nearly tens of kinds can form amorphous alloy system and have These characteristics, Δ T value can surpass more than 30 ℃, even can surpass more than 100 ℃, as Mg-Ln-TM, Ln-Al-TM, Zr-Al-TM, Ti-Zr-TM, Zr-(Ti, Nb, Pd)-Al-TM, Zr-Ti-TM-Be, Fe-(Al, Ga)-(P, C, B, Si), Pd-Cu-Ni-P, (Fe, Co)-(Zr, Hf, Nb, Ta)-B, Ti-Ni-Cu-Sn etc. (Ln=lanthanide series metal, TM=magnesium-yttrium-transition metal), one of characteristics of this class amorphous alloy are sharply to descend in supercooled liquid temperature range viscosity, can show superplasticity, unit elongation can reach 15000%, utilizes this characteristic can realize nearly clean shape processing, non-crystaline amorphous metal is made into complex-shaped small-sized component, and the supercooled liquid temperature range Δ T and the superplasticity in Δ T temperature range of broad also make amorphous powdered alloy or strip be easy to be consolidated into block materials through powder metallurgy technology.
Advantage of the present invention: metal nitride pottery (magnesium-yttrium-transition metal nitride particularly, TMN) has high hardness, at chemical mediator, all highly stable in metal melt and the steam, high temperature is isolator down, nitride ceramics/metal composite has obtained using widely as tool material, be considered to one of Hardmetal materials of tungstenic not, good wear resistance and thermotolerance are arranged, when the cutting steel and the pig iron, can adopt higher cutting speed, because nitride has excellent preservative property and biologically inert, can use the structured material of nitride ceramics/metal composite as medicine equipment and artificial heart.
Raw materials used and preparation method is provided by following examples and accompanying drawing matrix material of the present invention.
(a) Zr that Fig. 1 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10And contain (b) 5%, (c) 7.5%, (d) 10%, (e) 20% and (f) X ray diffracting spectrum of 30%AlN composite powder respectively.
(a) Zr that Fig. 2 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10And containing (b) 5%, (c) 7.5%, (d) 10%, (e) 20% and (f) the dsc analysis result of 30% AlN composite powder (heating rate is 40K/min) respectively, arrow is designated as glass transformation temperature T g
The Zr that contains 10%AlN that Fig. 3 forms after 40 hours for mechanical mill under the scanning electron microscope of the present invention (SEM) 65Al 7.5Cu 17.5Ni 10The pattern of composite powder.
Fig. 4 is the Zr that contains 10%AlN that the present invention (a) mechanical mill formed after 40 hours 65Al 7.5Cu 17.5Ni 10The transmission electron microscope light field of composite powder is corresponding selected area electron diffraction spectrum mutually and (b).
The Zr that contains (a) 5% nanometer AlN, (c) 5% nano TiN that Fig. 5 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10Composite powder and initial state, (b) nanometer AlN, (d) nano TiN particulate X ray diffracting spectrum.
(a) Zr that Fig. 6 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10And containing the dsc analysis result (heating rate is 40K/min) of (b) 5% nanometer AlN, (c) 5% nano TiN composite powder, arrow is designated as glass transformation temperature T g
(a) Zr that Fig. 7 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10Reach and contain (b) 10%Si respectively 3N 4, (c) 10%TiN and (d) X ray diffracting spectrum of 10%TaN composite powder.
(a) Zr that Fig. 8 forms after 40 hours for mechanical mill of the present invention 65Al 7.5Cu 17.5Ni 10Reach and contain (b) 10%Si respectively 3N 4, (c) 10%TiN and (d) the dsc analysis result of 10%TaN composite powder (heating rate is 40K/min), arrow is designated as glass transformation temperature T g
(a) Zr that Fig. 9 forms after 40 hours for mechanical mill of the present invention 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3And contain (b) 10%AlN composite powder and presmelting (c) Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3The X ray diffracting spectrum of alloy.
(a) Zr that Figure 10 forms after 40 hours for mechanical mill of the present invention 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3With the dsc analysis result who contains (b) 10%AlN composite powder (heating rate is 40K/min), arrow is designated as glass transformation temperature T g
(a) La that Figure 11 forms after 80 hours for mechanical mill of the present invention 55Al 25Cu 10Ni 5Co 5And contain (b) 10%AlN composite powder and presmelting (c) La 55Al 25Cu 10Ni 5Co 5The X ray diffracting spectrum of alloy.
(a) La that Figure 12 forms after 80 hours for mechanical mill of the present invention 55Al 25Cu 10Ni 5Co 5And containing the dsc analysis result (rate of heating is 40K/min) of (b) 10%AlN composite powder, arrow is designated as glass transformation temperature T g
Embodiment 1
Select Zr 65Al 7.5Cu 17.5Ni 10(alloying constituent is an atomic percent to alloy, and at.%), the AlN particle forms AlN particle/amorphous Zr as strengthening body by mechanical alloying as matrix 65Al 7.5Cu 17.5Ni 10Alloy is the composite powder of matrix, and as parent material, purity is 99.9% with commercially available zirconium, aluminium, nickel, copper powder, and granularity is 200 or 325 orders, and being mixed with nominal composition is Zr 65Al 7.5Cu 17.5Ni 10Powdered mixture, the addition of AlN ceramic particle is 5%～30% (percent by volume, vol.%), AlN purity is 99.5%, granularity 200 orders, powdered mixture and GCr15 steel ball filled in than 15: 1 in the quenching stainless steel jar mill by ball and weight of material, fed high-purity Ar gas (99.999%) after mechanical pump vacuumizes, grind Zr at Japan system NEV-MA8 type high energy vibration formula ball mill 65Al 7.5Cu 17.5Ni 10Powdered mixture and add 5～30% AlN particulate powder mixes therein after mechanical alloying in 40 hours, the Zr of super beginning, Al, Cu, the Ni element has formed amorphous alloy completely, and X-ray diffraction spectrum and heat are analyzed (differential scanning calorimeter, DSC, down with) the results are shown in Figure 1 and Fig. 2.Glass transformation temperature (the T of alloy and matrix material g), crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T) list in table 1.
Scanning electron microscopic observation confirms that the AlN/ amorphous Zr alloy-base composite material particle size that mechanical alloying forms is 20～50 μ m (Fig. 3), and transmission electron microscope (TEM) is observed and confirmed that the erose AlN second phase particle dispersion is distributed in amorphous Zr 65Al 7.5Cu 17.5Ni 10(Fig. 4) is of a size of 20～200nm on the alloy substrate.
Embodiment 2
Press embodiment 1, at Zr 65Al 7.5Cu 17.5Ni 105～10% AlN and the TiN nano particle that add in the alloy, with commercially available AlN and TiN nanometer powder is parent material, and granularity is 10～100nm, and purity is 99.9%, form " nitride nano particle/amorphous alloy base composite material " through mechanical alloying, at Zr 65Al 7.5Cu 17.5Ni 10In 5～10% the nanometer AlN that adds and TiN particulate powder mixture after mechanical alloying in 40 hours, initial Zr, Al, Cu, the Ni element has formed amorphous alloy completely, the X-ray diffraction spectrum of different composite material and heat are analyzed (DSC) result respectively as shown in Figure 5 and Figure 6, the glass transformation temperature (T of matrix material g), crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T) list in table 1.The pattern of composite powder and nanometer AlN and the distribution of TiN particle in the non-crystaline amorphous metal matrix are similar to Example 1.
Embodiment 3
Press embodiment 1, at Zr 65Al 7.5Cu 17.5Ni 1010% the Si that adds in the alloy 3N 4, TiN and TaN ceramic particle, form " nitride particles/amorphous alloy base composite material ", Zr behind the ball milling 65Al 7.5Cu 17.5Ni 10In 10% the Si that adds 3N 4, TiN and TaN ceramic particle powder mixture after mechanical alloying in 40 hours, initial Zr, Al, Cu, the Ni element is completed into amorphous alloy, and X-ray diffraction spectrum and heat are analyzed (DSC) result respectively as shown in Figure 7 and Figure 8, the glass transformation temperature (T of matrix material g), crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T) list in table 1.The pattern of composite powder and Si 3N 4, TiN and the distribution of TaN particle in the non-crystaline amorphous metal matrix be similar to Example 1.
Embodiment 4
Select Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3(atomic ratio) alloy is as matrices of composite material, and common AlN particle selects for use commercially available high pure metal bulk (plate, ingot, bar) as parent material for strengthening body, and purity is 99.99% (weight ratio), presses composition Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3Alloyage through the vacuum arc fumace melt back, forms the uniform alloy pig of chemical ingredients, and alloy structure is the miscellany of compound phase between crystalline metal.The alloy pig Mechanical Crushing of presmelting is powdered, and particle size is less than 0.5mm.Press embodiment 1,10% percent by volume AlN ceramic particle of interpolation forms " AlN nano particle/amorphous Zr alloy-base composite material " powder after the mechanical alloying.At Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3In the powdered mixture of 10% the AlN ceramic particle that adds after mechanical alloying in 40 hours, initial structure is crystalline Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3Mother alloy is completed into amorphous alloy.X-ray diffraction spectrum and heat are analyzed (DSC) result respectively as Fig. 9 and shown in Figure 10, the glass transformation temperature (T of matrix material g), crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T) list in table 1.The pattern of composite powder and Si 3N 4, TiN and the distribution of TaN particle in the non-crystaline amorphous metal matrix be similar to Example 1.
Embodiment 5
Select La 55Al 25Cu 10Ni 5Co 5(atomic ratio) alloy is as matrices of composite material, and common AlN particle selects for use commercially available high pure metal bulk (plate, ingot, bar) as parent material for strengthening body, and purity is 99.99% (weight ratio), presses composition La 55Al 25Cu 10Ni 5Co 5Alloyage through the vacuum arc fumace melt back, forms the uniform alloy pig of composition, and alloy structure is the miscellany of compound phase between crystalline metal.The alloy pig Mechanical Crushing of presmelting is powdered, and particle size is less than 0.5mm.The 10% percent by volume AlN ceramic particle that adds forms " AlN nano particle/non-crystalline state La alloy-base composite material " powder after the mechanical alloying.At La 55Al 25Cu 10Ni 5Co 5In the powdered mixture of 10% the AlN ceramic particle that adds after mechanical alloying in 80 hours, initial structure is crystalline La 55Al 25Cu 10Ni 5Co 5Mother alloy is completed into amorphous alloy.The X-ray diffraction spectrum of different composite material and heat are analyzed (DSC) structure respectively as Figure 11 and shown in Figure 12.Glass transformation temperature (the T of alloy and matrix material thereof g), crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T) list in table 1.The pattern of composite powder and the distribution of AlN particle in the non-crystaline amorphous metal matrix are similar to Example 1.
Glass transformation temperature (the T of various materials among the embodiment 1～5 that table 1 is determined by the heat analysis g),
Crystallization starting temperature (T x) and supercooled liquid temperature province width (Δ T x).
(heating rate is 40K/min)
Embodiment Material T g(K) T x(K) ΔT x(K)
1 Zr 65Al 7.5Cu 17.5Ni 10 Zr 65Alloy+10%AlN 669 668 729 738 60 70
2 Zr 65Alloy+5% nanometer AlN Zr 65Alloy+5% nano TiN 670 679 748 753 78 74
3 Zr 65Alloy+10%Si 3N 4 Zr 65Alloy+10%TiN 668 672 737 738 69 66
4 Zr 58.5Nb 2.8Cu 15.6Ni 12.8Al 10.3 Zr 58.5Alloy+10%AlN 685 668 764 767 79 99
5 La 55Al 25Cu 10Ni 5Co 5 La 55Alloy+10%AlN 451 450 492 499 41 49

Claims (3)

1. granular nitride/amorphous alloy based matrix material is characterized in that: the ratio (volume percent) of nitride particles and matrix amorphous alloy is A xB y, x=5～30, y=70～95, x+y=100, A are AlN, Si 3N 4, in TiN, ZrN, the TaN ceramic particle any, B is for constituting the multicomponent amorphous alloy of body material.
2. according to the described matrix material of claim 1, it is characterized in that: AlN, Si 3N 4, TiN, ZrN, TaN ceramic particle size range be 10 nanometers (nm) to 100 microns (μ m), disperse is distributed on the amorphous alloy matrix.
3. according to the described matrix material of claim 1, it is characterized in that: the amorphous alloy as matrices of composite material should have following feature: the multicomponent alloy that 1) contains element more than three kinds; 2) can adopt in melt-spun, ultrasonic atomizatio, melt casting, the mechanical alloying method any to be prepared into amorphous alloy; 3) obvious glass transition appearred in amorphous alloy before crystallization change takes place, and the width in supercooled liquid interval (Δ T) is greater than 30 ℃.
CNB011140429A 2001-06-07 2001-06-07 Granular nitride/amorphous alloy based composition Expired - Fee Related CN1176240C (en)

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CN100569984C (en) * 2007-01-12 2009-12-16 中国科学院金属研究所 Crystalline state alloy spherical particle/amorphous alloy base composite material and preparation method thereof
CN100560775C (en) * 2007-01-12 2009-11-18 中国科学院金属研究所 Amorphous alloy spherical particle/crystal alloy based composites and preparation method thereof
CN100560776C (en) * 2007-01-12 2009-11-18 中国科学院金属研究所 Amorphous alloy spherical particle/amorphous alloy base composite material and preparation method
CN106636985B (en) * 2016-11-16 2018-06-22 南京工程学院 A kind of metal glass composite material and preparation method thereof
CN114686724A (en) * 2022-03-11 2022-07-01 华南理工大学 Composite material with shape memory function and SLM (Selective laser melting) preparation method thereof

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