CN100365153C - In-situ self-generated reinforced Ni3Al composite and method for preparing same - Google Patents
In-situ self-generated reinforced Ni3Al composite and method for preparing same Download PDFInfo
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- CN100365153C CN100365153C CNB2005100105998A CN200510010599A CN100365153C CN 100365153 C CN100365153 C CN 100365153C CN B2005100105998 A CNB2005100105998 A CN B2005100105998A CN 200510010599 A CN200510010599 A CN 200510010599A CN 100365153 C CN100365153 C CN 100365153C
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Abstract
The present invention relates to an in-situ self-generated reinforced Ni3Al composite material and a preparation method thereof, particularly to a composite material and a preparation method thereof. Aim at the defect of poor brittleness existing in existing Ni3Al-base alloy, the Ni3Al composite material of the present invention is composed of Ni, B, Ti and Al, the stoichiometric ratio of Ni and Al is 2.704 to 3: 1, the stoichiometric ratio of Ti and B is 1.04 to 1.45: 1, and TiB is 3 to 20% of the total volume of the composite material. The preparation method comprises: activating Ni-Al-Ti-B system to prepare composite powder; then using discharge plasma sintering process to generate TiB/Ni3Al composite material in situ. TiB in the TiB/Ni3Al composite material prepared by the present invention exists at the form of whiskers, and Ni3Al has the characteristics of fine crystal grains, homogeneous distribution and outstanding mechanical property.
Description
Technical field
The present invention relates to a kind of matrix material and preparation method thereof, be specifically related to a kind of in-situ self-generated TiB/Ni based on Ni-Al-Ti-B system
3Al matrix material and preparation method thereof.
Background technology
Ni
3Al base alloy is one of maximum metallic compound of research, and it has the orderly crystalline structure of L12 type.Ni
3The Al monocrystalline at room temperature is plasticity, and polycrystalline Ni
3Al shows that with fragility transgranular fracture mode failures even crystal boundary has essential fragility.Ni
3The unusual facilitation phenomenon that occurs in the Al alloy, promptly yield strength makes this alloy have competitive power under higher temperature with the phenomenon that temperature raises and increases.Ni
3The Al intermetallic compound has good in oxidation resistance, little, higher room temperature work hardening rate and the higher high temperature strength several characteristics of density, is counted as the high-temperature structural material that superalloy uses that replaces of future generation, be subjected to paying attention to widely and studying, however Ni
3The fragility of Al has limited its widespread use.Crystal grain thinning is the effective way that improves its plasticity, reports Ni
3When the grain-size of Al was reduced to nano level, its plasticity can improve a lot.The interpolation of wild phase also can improve the plasticity of intermetallic compound in addition.In order to give full play to the potentiality of intermetallic compound characteristic, many research workers are devoted to compound composite material between development of metallic, i.e. the matrix material of intermetallic compound and particle, fiber, whisker shape pottery or metallic substance.
Discharge plasma sintering is as a kind of new technology of preparing, have advantages such as heat-up rate is fast, sintering time is short, weave construction is controlled, energy-conserving and environment-protective, can be under lower sintering temperature and less forming pressure condition powder stock be sintered into and have high performance material.Discharge plasma sintering process is powder such as metal to be packed in the mould that materials such as graphite make, utilize upper and lower die head and powered electrode that specific sintering power supply and pressing pressure are put on sintered powder, finish a kind of new powder metallurgy sintered technology of producing high performance material through discharge activation, thermoplastic distortion and cooling.
The in-situ authigenic enhancement techniques obtains extensive studies owing to having very outstanding advantage, as: strengthen body and matrix and have good thermodynamic stability, survivable when in hot environment, being on active service; Strengthening body and matrix has direct atom bonded interface structure, and the interface is straight, in conjunction with firm, and the existence of reactionless thing or precipitated phase; The interface is very clean, strengthens the enhancing body that exists in produced pollution problem and the fusion-casting process and the wettability problem between matrix thereby solved the conventional particle that adds; It is more tiny to strengthen the body size, is evenly distributed, and has good mechanical property.
Summary of the invention
At existing Ni
3There is the defective of fragility difference in Al base alloy, and the present invention is intended to adopt the discharge plasma sintering process original position to generate the tiny TiB/Ni of crystal grain by adopting high-energy ball milling method mechanical activation Ni-Al-Ti-B powder
3The Al matrix material, the material of this method preparation improves its toughness when improving material hardness.
In-situ self-generated reinforced Ni of the present invention
3The Al matrix material is grouped into by Ni, B, four kinds of one-tenth of Ti, Al, and wherein the stoichiometric ratio of each composition is Ni: Al=2.704～3: 1, and Ti: B=1.04～1.45: 1, TiB account for 3～20% of total composite volume.
In-situ self-generated reinforced Ni
3The preparation method of Al matrix material realizes as follows: one, high-energy ball milling machinery activation Ni-Al-Ti-B powder: by stoichiometric ratio is Ni: Al=2.704～3: 1, Ti: B=1.04～1.45: 1,3～20% the ratio that TiB accounts for total composite volume takes by weighing the Ni-Al-Ti-B element powders and steel ball is together put into ball grinder, charge into argon gas atmosphere after vacuumizing, the control ratio of grinding media to material is 5～20: 1, vibrational frequency is 100～300 times/minute, ball milling 30～50 hours obtains composite powder; Two, discharge plasma sintering: in the stone mill mould of earlier composite powder behind the mechanical activation being packed into, subsequently mould is put into the discharge plasma sintering stove, by upper and lower pressure head composite powder is exerted pressure, control pressure is 10～85MPa, is evacuated to 5～15Pa then, is heated to 800～1100 ℃ with the heat-up rate of 80～120 ℃/min, insulation 5～15min, impose the pressure of 65～95MPa simultaneously, be cooled to room temperature with 40～100 ℃/min then, obtain TiB/Ni
3The Al matrix material.
The present invention is a kind of employing discharge plasma sintering in-situ self-generated TiB/Ni
3The Design Theory of Al matrix material and preparation technology.Through calculation of thermodynamics, in the Ni-Al-Ti-B system following reaction can take place:
3Ni+Al→Ni
3Al (1)
Ti+2B→TiB
2 (2)
Ti+TiB
2→TiB (3)
More than Fan Ying Enthalpies of Formation is negative value, illustrates that these three reactions all can take place on thermodynamics.Wherein, Ti and B at first form TiB
2, the 3rd reaction can take place when Ti is excessive.Because the special crystalline structure (B27) of TiB makes that B is easy to make that along the specific direction diffusion speed of growth on this direction is greater than other directions, therefore the TiB that generates can exist with the pattern of whisker and matrix Ni
3Among the Al.In addition in mechanical milling process, because the collision of high-frequency ball-material-ball, make original powder repeated deformation, in this process, four kinds of element powders are evenly distributed each other, introduce a large amount of defectives such as hole, dislocation etc. simultaneously.
In the discharge plasma sintering process, the power supply of alternation produces the plasma discharge process between powder, and this process makes particle surface activate, and has accelerated the diffusion between the material, makes the particle viscous deformation improve, and shortens sintering time.After being incubated,, obtain evenly tiny grain structure because the speed of cooling of this technology is very big.
Ni
3Al is that the form with nanocrystal exists, and this makes material deformation even, reduces the stress concentration in the deformation process.The existence of the TiB phase of whisker shape can effectively hinder and the deflection crackle in addition, also can improve the plasticity of material.
According to above-mentioned reaction, adopt high-energy ball milling machinery activation Ni-Al-Ti-B system to make composite powder.Adopt appropriate parameters then, applying charge plasma sintering technology original position generation volume fraction is 3～20% TiB/Ni
3The Al matrix material.Because sintering mechanism that discharge plasma sintering process is special and big speed of cooling, so Ni
3The Al matrix grain is of a size of nano level, and test result is 40 ± 10nm.The special crystal structure of TiB (B27) makes the TiB that generates grow with the whisker shape.For prepared enhancing body volume fraction is 10% matrix material, and the matrix material density is very high, reaches 99.8% of theoretical value, and the hardness value of material is 1170Hv.
The present invention is applicable to that discharge plasma sintering TiB whisker strengthens nanometer crystalline Ni
3The Al matrix material.The prepared material of discharge plasma sintering process has that crystal grain is tiny, homogeneous microstructure, density advantages of higher.Owing to adopt the in-situ authigenic reaction method to prepare material, enhancing body and matrix have good thermodynamic stability in the gained material in addition, and be survivable when being on active service in hot environment; Strengthening body and matrix has direct atom bonded interface structure, and the interface is straight, in conjunction with firm, and the existence of reactionless thing or precipitated phase; The interface is very clean, strengthens the enhancing body that exists in produced pollution problem and the fusion-casting process and the wettability problem between matrix thereby solved the conventional particle that adds; It is more tiny to strengthen the body size, is evenly distributed, and has good mechanical property etc.
Embodiment
Embodiment one: the in-situ self-generated reinforced Ni of present embodiment
3The Al matrix material is grouped into by Ni, B, four kinds of one-tenth of Ti, Al, and wherein the stoichiometric ratio of each composition is Ni: Al=2.704～3: 1; Ti: B=1.04～1.45: 1, TiB account for 3～20% of total composite volume.
Nickel powder described in the present embodiment (Ni) particle size range is 10 μ m, and about aluminium powder (Al) average particle size particle size 3 μ m, titanium valve (Ti) particle size is 10 μ m, and boron powder (B) particle size is 3 μ m.
Embodiment two: what present embodiment and embodiment one were different is that the stoichiometric ratio of each composition is Ni: Al=3: 1, and B: Ti=1: 1.2, TiB accounts for 5% of total composite volume.
Embodiment three: what present embodiment and embodiment one were different is that the stoichiometric ratio of each composition is Ni: Al=3: 1, and B: Ti=1: 1.446, TiB accounts for 10% of total composite volume.
Embodiment four: what present embodiment and embodiment one were different is that the stoichiometric ratio of each composition is Ni: Al=3: 1, and B: Ti=1: 1.25, TiB accounts for 15% of total composite volume.
Embodiment five: what present embodiment and embodiment one were different is that the stoichiometric ratio of each composition is Ni: Al=2.8: 1, and B: Ti=1: 1.05, TiB accounts for 18% of total composite volume.
Embodiment six: what present embodiment and embodiment one were different is that the stoichiometric ratio of each composition is Ni: Al=2.9: 1, and B: Ti=1: 1.35, TiB accounts for 8% of total composite volume.
Embodiment seven: present embodiment prepares TiB/Ni as follows
3The Al matrix material:
One, high-energy ball milling machinery activation Ni-Al-Ti-B powder: for preparing 3～20vol%TiB/Ni
3The Al matrix material, in stoichiometric ratio is that the ratio of Ni: Al=2.704～3: 1, Ti: B=1.04～1.45: 1 takes by weighing the Ni-Al-Ti-B element powders and steel ball is together put into ball grinder, charge into argon gas atmosphere after vacuumizing, control ball material (quality) is than being 5～20: 1, vibrational frequency is 100～300 times/minute, ball milling 30～50 hours has the water quench ball grinder in this process, prevent that the temperature in the mechanical milling process from raising.In mechanical milling process, element powders is impacted by the steel ball of rapid movement, repeated deformation, thus make element powders be evenly distributed, obtain composite powder.
Two, discharge plasma sintering: the composite powder behind the mechanical activation is packed in the stone mill mould, put into the discharge plasma sintering stove, by upper and lower pressure head composite powder is imposed certain pressure (10～85MPa), be evacuated to 5～15Pa then, heat-up rate with 80～120 ℃/min is heated to 800 1100 ℃, is incubated 5～15min, imposes the pressure of 65～95MPa in the time of insulation, be cooled to room temperature with 20～60 ℃/min then, obtain TiB/Ni
3The Al matrix material.
Embodiment six: present embodiment prepares TiB/Ni as follows
3The Al matrix material:
One, high-energy ball milling machinery activation Ni-Al-Ti-B powder: be preparation 10vol%TiB/Ni
3The Al matrix material is Ni: Al=12.78 in stoichiometric ratio: 4.26, B: Ti=1: 1.4 ratio takes by weighing the Ni-Al-Ti-B element powders and steel ball is together put into ball grinder, vacuumizes (10
-2Pa) charge into argon gas atmosphere after.The control ratio of grinding media to material is 10: 1, and vibrational frequency is 200 times/minute, and ball milling 40 hours has the water quench ball grinder to prevent that the temperature in the mechanical milling process from raising in this process.In mechanical milling process, element powders is impacted by the steel ball of rapid movement, repeated deformation, thus make element powders be evenly distributed, obtain composite powder.
Two, discharge plasma sintering: the composite powder behind the mechanical activation is packed in the stone mill mould, put into the discharge plasma sintering stove and impose certain pressure (10～80MPa), be evacuated to 10Pa then, heat-up rate with 100 ℃/min is heated to temperature shown in the table 1, under this temperature, be incubated 5mn, impose the pressure of 80MPa simultaneously, be cooled to room temperature with 40 ℃/min then, obtain TiB/Ni
3The Al matrix material.This matrix material density is very high, reaches 99.8% of theoretical value, and the performance perameter of material sees Table 1.
Table 1
| Material | Sintering temperature (℃) | Hardness (Hv) | Fracture toughness property (MPam 1/2) | s(MPa) |
| Ni 3Al | 950 | 813 | 20 | 727.8 |
| 10vol.％TiB/Ni 3Al | 900 | 926 | 20.67 | 988 |
| 10vol.％TiB/Ni 3Al | 950 | 1170 | 21.29 | 1178 |
| 10vol.％TiB/Ni 3Al | 1000 | 989 | 22.89 | 1320 |
| 10vol.％TiB/Ni 3Al | 1050 | 794 | 22.64 | 1583 |
Institute's column data is the hardness and the fracture toughness property value of the material of employing the inventive method preparation in the table 1, and wherein yield strength is the three point bending test gained.
Claims (2)
1. in-situ self-generated reinforced Ni
3The preparation method of Al matrix material is characterized in that described Ni
3The Al matrix material is prepared as follows: one, high-energy ball milling machinery activation Ni-Al-Ti-B powder: in stoichiometric ratio is that 3～20% ratio that Ni: Al=2.704～3: 1, Ti: B=1.04～1.45: 1, TiB account for total composite volume takes by weighing the Ni-Al-Ti-B element powders and steel ball is together put into ball grinder, charge into argon gas atmosphere after vacuumizing, the control ratio of grinding media to material is 5～20: 1, vibrational frequency is 100～300 times/minute, ball milling 30～50 hours obtains composite powder; Two, discharge plasma sintering: in the stone mill mould of earlier composite powder behind the mechanical activation being packed into, subsequently mould is put into the discharge plasma sintering stove, by upper and lower pressure head composite powder is exerted pressure, control pressure is 10～85MPa, is evacuated to 5～15Pa then, is heated to 800～1100 ℃ with the heat-up rate of 80～120 ℃/min, insulation 5～15min, impose the pressure of 65～95MPa simultaneously, be cooled to room temperature with 40～100 ℃/min then, obtain TiB/Ni
3The Al matrix material.
2. according to the described in-situ self-generated reinforced Ni of claim 1
3The preparation method of Al matrix material is characterized in that described TiB/Ni
3In the Al matrix material, TiB accounts for 10% of total composite volume, and the stoichiometric ratio of each composition is Ni: Al=3: 1, and B: Ti=1: 14.
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| CN102189337B (en) * | 2011-02-14 | 2014-04-30 | 北京工业大学 | Laser crack-free fusion welding repair method for Ni3Al-based alloy casting |
| CN110492094B (en) * | 2019-07-12 | 2021-05-25 | 广东工业大学 | Normal-temperature plastic deformation-rapid consolidation magnesium alloy anode material and preparation method and application thereof |
| CN111471896B (en) * | 2020-05-14 | 2021-05-04 | 哈尔滨工业大学 | Preparation method of nano hafnium oxide reinforced NiAl composite material |
| CN114232035A (en) * | 2021-12-21 | 2022-03-25 | 贵州省新材料研究开发基地 | Modified anode for hydrometallurgy and preparation method thereof |
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