CN102321857B - Zirconium-based amorphous composite material and preparation process thereof - Google Patents
Zirconium-based amorphous composite material and preparation process thereof Download PDFInfo
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Abstract
The invention relates to a zirconium-based amorphous composite material in the technical field of zirconium-based amorphous composite materials. The zirconium-based amorphous composite material is made from the following raw materials in percentage by weight: 70.0-75.0% of zirconium, 10.0% of aluminum, 13.3-18.7% of nickel, 0.788-2% of titanium and 0.2-0.5% of carbon; and the mole ratio of the titanium to the carbon is 1:1. The preparation process comprises the following steps of: taking titanium powder and amorphous carbon powder according to the formula, taking aluminum powder which is twice of the total weight of the titanium powder and the amorphous carbon powder, and sintering at 750 DEG C for 15-30 min to prepare an aluminum-carbon-based composite material masterbatch; mixing with the zirconium powder, the nickel powder and the residual aluminum powder, smelting and cooling. The growth of dendritic crystals in an amorphous system is promoted and the dendritic crystals are uniformly distributed in the amorphous system; the strength and the hardness of the amorphous composite material are generally increased by adding TiC ceramic grain reinforced phases, and meanwhile, a certain plastic deformation is expressed in the system and the stability is improved.
Description
Technical field
The present invention relates to the Zirconium base non-crystalline composite material technical field, particularly a kind of Zirconium base non-crystalline composite material also relates to this composite manufacture technique.
Background technology
Since the nineties in last century, material supplier author has had breakthrough progress for the research of amorphous, by the reasonable component design, can prepare a series of amorphous system by common technique.Wherein zirconium-based bulk amorphous alloy not only has good amorphous formation ability but also has good mechanical property, such as high breaking tenacity (about 2.0GPa) and elastic limit (about 2%), under the plane strain effect, have good ductility etc., make it become good structured material.But monocrystalline phase non-crystaline amorphous metal (unilateral stretching) plastix strain amount under plane stress condition is almost nil.For amorphous block general exist plasticity too low, and the problem of fragility fracture, this problem has become the bottleneck of restriction amorphous development.
Studies show that the amorphous compound phase has better mechanical property, particularly importantly can significantly improve the plasticity of amorphous block.Therefore material supplier author is making great efforts to improve by the preparation of amorphous composite these mechanical propertys of amorphous always.It is exactly the important member of amorphous composite that dentrite strengthens amorphous composite, preparation method in the past generally adopts the Amorphous Crystallization method, make noncrystally to tie up to crystallization spanning tree dendrite under the crystallization temperature, but adopt such method to exist thermal treatment temp and treatment time to be difficult to control and dentrite problem pockety.These problems have become the bottleneck that constrained tree dendrite strengthens amorphous composite.
Summary of the invention
For solve above thermal treatment temp and treatment time be difficult to control and dentrite problem pockety, the invention provides a kind of by inducing the dendrite of preparing to strengthen mutually Zirconium base non-crystalline composite material at zirconium-base amorphous middle interpolation TiC ceramic particle.The present invention has simplified the preparation process of dendrite enhancing amorphous composite, and the improvement by melting technology distributes tiny ceramic particle disperse in matrix of generation, and the combination good with matrix, thereby solve dentrite problem pockety, make the even structure of amorphous composite stable, and show good mechanical property, physicals and thermomechanical property.
The present invention also provides above-mentioned dendrite to strengthen mutually the preparation technology of Zirconium base non-crystalline composite material.
The present invention is achieved by the following measures:
A kind of Zirconium base non-crystalline composite material, made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.3-18.7%, titanium 0.788-2%, agraphitic carbon 0.2-0.5%, wherein the mol ratio of titanium and decolorizing carbon is 1:1.
Described Zirconium base non-crystalline composite material, made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.4-18.7%, titanium 1.024-1.339%, amorphous carbon powder 0.261-0.341%.
Described Zirconium base non-crystalline composite material, made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.7-18.7%, titanium 1.04%, amorphous carbon powder 0.26%.
Described Zirconium base non-crystalline composite material, the granularity of used titanium≤75 μ m, decolorizing carbon granularity≤15 μ m, aluminium particle size≤75 μ m.
The preparation technology of described Zirconium base non-crystalline composite material may further comprise the steps:
(1) contain the preparation of the aluminum matrix composite masterbatch of TiC ceramic particle:
Take by weighing titanium valve and amorphous carbon powder by formula ratio, and according to titanium valve and amorphous carbon powder weight and twice take by weighing aluminium powder, mix, dry, be pressed into prefabricated section, 750 ℃ of sintering 15-30min make the aluminum matrix composite masterbatch in the resistance furnace that has shielding gas to exist;
(2) preparation of Zirconium base non-crystalline composite material:
Take by weighing zirconium powder, nickel powder and remaining aluminium powder by formula ratio; mixed with the aluminum matrix composite masterbatch that step (1) makes; melting in the arc-melting furnace that has shielding gas to exist, rate of cooling is that 200-400 ℃/s is cooled to 5-20 ℃, has both got Zirconium base non-crystalline composite material.
Use ball mill that titanium valve, amorphous carbon powder and aluminium powder are mixed in the step (1).
It is 500A that arc-melting furnace is stablized after-current, and voltage is 40V.
The operation steps of melting is: 10-15 raw material second fusing after arc-melting furnace is stable, continue induction stirring melting 2-3 minute, and repeat this step 6 time.
The column amorphous block is cast in the Zirconium base non-crystalline composite material suction.
The present invention provides nucleation site revulsive crystallization spanning tree dendrite by add generated in-situ TiC ceramic particle in amorphous block, and the improvement by melting technology before amorphous preparation, in matrix, generate the tiny ceramic particle that disperse distributes, make it be evenly distributed in the matrix and then can better prepare the uniform Zirconium base non-crystalline composite material of distribution of dendritic.The invention solves dendrite and strengthen that dendrite generates unmanageable problem in the amorphous composite, the dendrite that can prepare different dendrite content by the content that changes particle strengthens amorphous composite.Simultaneously by control that ceramic particle is distributed can efficient solution the problem of distribution of dendritic inequality in the crystal composite material by no means.Analyze after deliberation that the dendrite that generates is the same crystalline phase in the preparation, so just guaranteed that this technique prepares the amorphous composite of stable performance in the future production.
And prove through repetition test: TiC ceramic particle quality mark during in 1.3% left and right sides dendrite to strengthen pine-tree structure in the amorphous composite complete and be evenly distributed.Simultaneously under other granule contents, also system has been played certain enhancement.
Beneficial effect of the present invention:
(1) introduced the TiC ceramic particle reinforced phase nucleation site of crystallization in the amorphous is provided, and then promoted the dendritic growth in the amorphous system, simultaneously owing to the distribution of having controlled the TiC particle in the system, thereby the dendrite in the system is evenly distributed mutually;
(2) the general raising of the adding of TiC ceramic particle reinforced phase intensity and the hardness of amorphous composite, simultaneously also so that diagram of system reveals certain plastic deformation, adding along with the TiC ceramic particle reinforced phase, the pure amorphous of the strength ratio of system improves about 20%, reach 1200MPa, Vickers' hardness is brought up to 6.5-7.5GPa, show simultaneously contain the TiC ceramic particle reinforced phase the system plastic deformation ability greater than 1.0%, and abrasion loss is also lower in wear-resisting wiping test;
(3) add the TiC ceramic particle reinforced phase, also played positive effect aspect stable improving.
Description of drawings
Accompanying drawing 1 is the granule-morphology on the aluminum matrix composite masterbatch surface of embodiment 2 preparations,
A figure is the SEM pattern of the Zr-Al-Ni non-crystaline amorphous metal of comparative example's 1 preparation in the accompanying drawing 2,
B figure is the surface topography of the Zirconium base non-crystalline composite material of embodiment 2 preparations in the accompanying drawing 2,
Accompanying drawing 3 is the compressive stress strain curve of Zirconium base non-crystalline composite material when compression speed 0.5mm/min of different Ti C granule content,
Accompanying drawing 4 be the matrix material of embodiment 2 preparation at the sem test figure of incompressible test rupture cross section,
Accompanying drawing 5 is the thermal analysis curve figure of matrix material under 10 ℃/min of temperature rise rate, 15 ℃/min, 20 ℃/min and 25 ℃/min condition of embodiment 2 preparation,
Accompanying drawing 6 is the thermal analysis curve figure of Zr-Al-Ni non-crystaline amorphous metal under 10 ℃/min of temperature rise rate, 15 ℃/min, 20 ℃/min and 25 ℃/min condition of comparative example 1 preparation.
Embodiment
Listed the raw materials used weight percent hundred of embodiment 1-4 in the table 1.Raw materials used: Ti Powder Particle Size≤75 μ m, decolorizing carbon Powder Particle Size≤15 μ m, Al Powder Particle Size≤75 μ m.
The raw materials used amount cartogram of table 1 embodiment 1-4 (wt%)
Embodiment 1:
(1) contain the preparation of the aluminum matrix composite masterbatch of TiC ceramic particle:
Take by weighing titanium valve 1.339g and amorphous carbon powder 0.341g, and according to titanium valve and amorphous carbon powder weight and twice take by weighing aluminium powder, mix, use ball mill that three kinds of powder are mixed, do at argon gas that 750 ℃ of sintering 15-30min make the aluminum matrix composite masterbatch in the resistance furnace of protection gas;
(2) dendrite strengthens the preparation of Zirconium base non-crystalline composite material:
Take by weighing zirconium powder, nickel powder and remaining aluminium powder in the ratio among the embodiment in the table 11, and zirconium powder, aluminium powder and nickel powder mixed with the aluminum matrix composite masterbatch, melting in the argon arc smelting furnace, and use induction stirring that each component is mixed, rate of cooling is that 200-400 ℃/s is cooled to 5-20 ℃; Then inhale and cast the column amorphous block that the 4mm diameter is about 80mm.The operating voltage of arc-melting furnace is 380V, 50Hz, and three-phase alternating current, the 5A electric current is used in the starting the arc, and stable after-current is 500A, voltage 40V, stable rear 10-15 melts second, continues afterwards the induction stirring melting 2-3 minute, and melt back is 6 times like this.
The Theoretical Mass mark of the TiC particle of this moment is 1.7% as calculated.
The Vickers' hardness that records matrix material is brought up to more than the 6.8GPa, and incompressible intensity greater than 1.6%, is seen accompanying drawing 3 greater than 1200MPa, plastix strain value.The Vickers' hardness of this matrix material and the pure amorphous block of incompressible strength ratio are significantly improved.
Embodiment 2
Take by weighing each starting material in the ratio among the embodiment in the table 12, make dendrite according to the technique of embodiment 1 and strengthen Zirconium base non-crystalline composite material, the massfraction of the TiC particle of this moment is 1.3% as calculated.
The Vickers' hardness of matrix material is greater than 7.0GPa, and incompressible intensity more than the 1250MPa, the plastix strain value about 1.3%, see accompanying drawing 3.The Vickers' hardness of this matrix material and incompressible intensity are significantly improved than pure amorphous block equally.
Embodiment 3
Take by weighing each starting material in the ratio among the embodiment in the table 13, make dendrite according to the technique of embodiment 1 and strengthen Zirconium base non-crystalline composite material, the massfraction of the TiC particle of this moment is 1.0% as calculated.
The Vickers' hardness of material 2 samples is greater than 6.5GPa, and incompressible intensity more than the 1200MPa, the plastix strain value about 1.1%, see accompanying drawing 3.The Vickers' hardness of this matrix material and incompressible intensity are significantly improved than pure amorphous block equally.
Embodiment 4
Take by weighing each starting material in the ratio among the embodiment in the table 14, make dendrite according to the technique of embodiment 1 and strengthen Zirconium base non-crystalline composite material, the massfraction of the TiC particle of this moment is 2.3% as calculated.
The Vickers' hardness of material 2 samples is greater than 6.8GPa, and incompressible intensity more than the 1100MPa, the plastix strain value about 1.8%, see accompanying drawing 3.The Vickers' hardness of this matrix material and incompressible intensity are significantly improved than pure amorphous block equally.
The comparative example 1
Mix according to the part by weight weighing of Zr, Al, three kinds of raw materials of Ni among the embodiment 2, melting and use induction stirring that each component is mixed in the argon arc smelting furnace, rate of cooling is that 200-400 ℃/s is cooled to 5-20 ℃; Then inhale and cast the column amorphous block that the 4mm diameter is about 80mm, obtain the Zr-Al-Ni alloy.The operating voltage of arc-melting furnace is 380V, 50Hz, and three-phase alternating current, the 5A electric current is used in the starting the arc, and stable after-current is 500A, voltage 40V, stable rear 10-15 melts second, continues afterwards the induction stirring melting 2-3 minute, melt back 6 times.
Performance test
Surface topography
Use scanning electron microscope to detect the granule-morphology on the aluminum matrix composite masterbatch surface of embodiment 2 preparations, see and to find out that the TiC particle is the most tiny shown in the accompanying drawing 1 that spherical in shape, median size is at 1～2 μ m.Detect the surface topography of the Zirconium base non-crystalline composite material of embodiment 2 preparations, shown in b figure in the accompanying drawing 2, a is the SEM pattern of the Zr-Al-Ni non-crystaline amorphous metal of comparative example's 1 preparation in the accompanying drawing 2, there is not crystal boundary among a figure, weave construction is fine and close, be amorphous structure completely, can be clearly seen that among the b figure to be evenly distributed and the dendrite of structural integrity.
Incompressible test
Preparing the TiC granule content with reference to embodiment 1-4 is 0.0%, 0.2%, 0.7% Zirconium base non-crystalline composite material, accompanying drawing 3 is 0.0%, 0.2%, 0.7%, 1.3%, 1.7%, 2.0%, 2.3% the compressive stress strain curve of Zirconium base non-crystalline composite material when compression speed is 0.5mm/min for the TiC granule content, as can be seen from the figure, ceramic particle TiC is as strongthener, effectively raise the intensity of matrix, simultaneously as the sclerosis phase, so that structure hardening appears in matrix, thereby the Vickers' hardness that contains the system of particle generally improves.Aspect viscous deformation, division, thereby occurs or concentrates, so the expansion complicated of shear zone effectively raises plasticity so that shear zone is obstructed when extending as the introducing of second-phase in particle; Moreover owing to exist a small amount of crystalline phase (dendrite) in the matrix, when compression set, also played the effect of certain raising plasticity.Comprehensively, these factors are so that granule content is to behave oneself best on the over-all properties of sample of 1.3wt%, thereby as the primary study object, carry out thermodynamics, the analysis and research of terms of mechanics.
Matrix material to embodiment 2 preparations carries out the scanning electron microscope sweep test at incompressible test rupture cross section, as shown in Figure 4, obvious multiplex has occured in shear zone in figure right side central position, a lot of shear zones has been subject to inhibition herein simultaneously, stop to continue expansion, show as concentrating of shear zone on the microcosmic, and the plastic deformation that shows as on the macroscopic view in the incompressible test of sample improves.
The characteristic temperature test
(1) Zirconium base non-crystalline composite material of embodiment 2 preparations is done the thermodynamics test, understand its thermostability
Thermal analysis curve figure under 10 ℃/min of temperature rise rate, 15 ℃/min, 20 ℃/min and 25 ℃/min condition sees Fig. 5, and the characteristic temperature cartogram sees the following form 2.
The characteristic temperature cartogram of the matrix material of table 2 embodiment 2 preparations
| Temperature rise rate ℃/min | T g/℃ | T x/℃ | T p1/℃ | T p2/℃ |
| 10 | 491.5 | 527.2 | 544.8 | 619.2 |
| 15 | 493.6 | 530.5 | 549.7 | 621.4 |
| 20 | 495.0 | 538.4 | 552.8 | 622.8 |
| 25 | 498.1 | 545.1 | 554.2 | 628.7 |
By characteristic temperature as can be known: the architectural feature temperature raises greatly with the temperature rise rate change, illustrates that the glass transition behavior of bulk amorphous composite materials is relevant with temperature rise rate, shows as certain crystallization kinetics.
With the intensity of activation that the Kissinger method calculates, see the following form 3,
Data communication device is crossed A, B value and the intensity of activation data sheet that the match of Kissinger method obtains in table 3 table 2
| Parameter | T g | T x | T p1 | T p2 |
| The A=C(constant) | 93.895 | 25.788 | 64.978 | 66.958 |
| B=-E C/R（K） | -80229.39 | -29439.36 | -62329.66 | -69750.69 |
| Degree of confidence R2 | 0.9348 | 0.9189 | 0.9861 | 0.8218 |
| E C (J/mol) | 666706.23 | 244641.08 | 517959.47 | 579628.23 |
With the intensity of activation that the Ozawa method calculates, see the following form 4,
Data communication device is crossed A, B value and the intensity of activation data sheet that the match of Ozawa method obtains in table 4 table 2
| Parameter | Tg | Tx | Tp1 | Tp2 |
| A=C (constant) | 47.4177 | 17.8853 | 34.9200 | 35.8549 |
| B=-0.4567E C/R(K) | -35510.4 | -13488.9 | -27785.2 | -31072.5 |
| Degree of confidence R 2 | 0.9371 | 0.9266 | 0.9868 | 0.8292 |
| E C(J/mol) | 646139.2 | 245440.1 | 505573.2 | 565387.0 |
(2) the Zr-Al-Ni non-crystaline amorphous metal of comparative example 1 preparation carried out the thermodynamics test, the thermal analysis curve figure under 10 ℃/min of temperature rise rate, 15 ℃/min, 20 ℃/min and the 25 ℃/min condition sees Fig. 6, and characteristic temperature sees the following form 5,
Table 5
Zr-Al
-The characteristic temperature of-Ni non-crystaline amorphous metal system under different temperature rise rates
| Temperature rise rate ℃/min | T g/℃ | T x/℃ | T p1/℃ | T p2/℃ |
| 10 | 491.7 | 525.6 | 546.5 | 624.1 |
| 15 | 494.1 | 529.2 | 551.4 | 629.7 |
| 20 | 495.6 | 537.7 | 554.7 | 635.9 |
| 25 | 498.8 | 544.8 | 557.5 | 640.1 |
With the intensity of activation that the Kissinger method calculates, see the following form 6,
Data communication device is crossed A, B value and the intensity of activation data sheet that the match of Kissinger method obtains in table 6 table 5
| Parameter | T g | T x | T p1 | T p2 |
| The A=C(constant) | 87.177 | 23.156 | 56.348 | 37.963 |
| B=-E C/R（K） | -75015.5 | -27238.2 | -55293.7 | -44164.9 |
| Degree of confidence R 2 | 0.9464 | 0.9208 | 0.9998 | 0.9900 |
| E C (J/mol) | 623379 | 226350 | 459490 | 367011 |
Variation according to intensity of activation can be found out at glass transformation temperature (T
g) time intensity of activation be 623379 J/mol to the maximum, illustrate glass transition this moment to begin the energy that need to consume maximum.And begin temperature (T in crystallization
x) time intensity of activation minimum, beginning of this explanation crystallization does not need too many energy.
With the intensity of activation that the Ozawa method calculates, see the following form 7,
Data communication device is crossed A, B value and the intensity of activation data sheet that the match of Ozawa method obtains in table 7 table 5
| Parameter | T g | T x | T p1 | T p2 |
| The A=C(constant) | 44.503 | 16.740 | 31.174 | 23.269 |
| B=-0.4567E C/R（K） | -33248 | -12531 | -24731 | -19966 |
| Degree of confidence R 2 | 0.948 | 0.929 | 0.999 | 0.991 |
| E C（J/mol） | 604972.4 | 228012.1 | 449999.1 | 363296.4 |
Alloy system is when crystallization, the energy that the atom of generation crystallization will obtain to add just can form active cluster, such additional energy generally can obtain by collision, so intensity of activation also can be understood to alloy system atom required additional energy when forming active cluster.So the size of intensity of activation can reflect the size of the required potential barrier that overcomes in the crystallization process, if intensity of activation is higher, the required potential barrier that overcomes of alloy atom is just larger, and then non-crystaline amorphous metal is just more stable, and namely thermostability is just higher.By E in table 3 and table 6 and table 4 and the table 7
CValue can be found out, no matter is to use Kissinger method or Ozawa method, and the intensity of activation of the Zirconium base non-crystalline composite material that contains TiC particle 1.3% of embodiment 2 preparations is at glass transformation temperature (T
g), crystallization begins temperature (T
x) and crystallization peak temperature (T
Pi) intensity of activation all compared than the Zr-Al-Ni non-crystaline amorphous metal of embodiment 1 preparation improves, this explanation is added a certain amount of TiC particle and has been played positive effect aspect stable improving.
Claims (8)
1. Zirconium base non-crystalline composite material is characterized in that being made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.3-18.7%, titanium 0.788-2%, agraphitic carbon 0.2-0.5%, wherein the mol ratio of titanium and decolorizing carbon is 1:1;
Obtain by following steps:
(1) contain the preparation of the aluminum matrix composite masterbatch of TiC ceramic particle:
Take by weighing titanium valve and amorphous carbon powder by formula ratio, and according to titanium valve and amorphous carbon powder weight and twice take by weighing aluminium powder, mix, dry, be pressed into prefabricated section, 750 ℃ of sintering 15-30min make the aluminum matrix composite masterbatch in the resistance furnace that has shielding gas to exist;
(2) preparation of Zirconium base non-crystalline composite material:
Take by weighing zirconium powder, nickel powder and remaining aluminium powder by formula ratio; mixed with the aluminum matrix composite masterbatch that step (1) makes; melting in the arc-melting furnace that has shielding gas to exist, rate of cooling is that 200-400 ℃/s is cooled to 5-20 ℃, namely gets Zirconium base non-crystalline composite material.
2. Zirconium base non-crystalline composite material according to claim 1 is characterized in that being made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.4-18.7%, titanium 1.024-1.339%, amorphous carbon powder 0.261-0.341%.
3. Zirconium base non-crystalline composite material according to claim 1 is characterized in that being made by the raw material of following weight percent:
Zirconium 70.0-75.0%, aluminium 10.0%, nickel 13.7-18.7%, titanium 1.04%, amorphous carbon powder 0.26%.
4. Zirconium base non-crystalline composite material according to claim 1 is characterized in that the granularity of titanium≤75 μ m, decolorizing carbon granularity≤15 μ m, aluminium particle size≤75 μ m.
5. Zirconium base non-crystalline composite material according to claim 1 is characterized in that using ball mill that titanium valve, amorphous carbon powder and aluminium powder are mixed.
6. Zirconium base non-crystalline composite material according to claim 1 is characterized in that it is 500A that arc-melting furnace is stablized after-current, and voltage is 40V.
7. Zirconium base non-crystalline composite material according to claim 6 is characterized in that the operation steps of melting is: 10-15 raw material second fusing after arc-melting furnace is stable, continue induction stirring melting 2-3 minute, and repeat this step 6 time.
8. Zirconium base non-crystalline composite material according to claim 1 is characterized in that the column amorphous block is cast in the Zirconium base non-crystalline composite material suction.
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