CN117684070A - Ni (nickel) 3 Ti/WC composite material and liquid metal infiltration process preparation method thereof - Google Patents
Ni (nickel) 3 Ti/WC composite material and liquid metal infiltration process preparation method thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 302
- 238000000034 method Methods 0.000 title claims abstract description 219
- 239000002131 composite material Substances 0.000 title claims abstract description 193
- 230000008569 process Effects 0.000 title claims abstract description 188
- 230000008595 infiltration Effects 0.000 title claims abstract description 99
- 238000001764 infiltration Methods 0.000 title claims abstract description 99
- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 70
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 305
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 190
- 238000005245 sintering Methods 0.000 claims abstract description 109
- 238000000498 ball milling Methods 0.000 claims abstract description 98
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000005011 phenolic resin Substances 0.000 claims abstract description 44
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 44
- 239000011230 binding agent Substances 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 52
- 229910001000 nickel titanium Inorganic materials 0.000 claims description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 43
- 238000000465 moulding Methods 0.000 claims description 42
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 claims description 41
- 239000002245 particle Substances 0.000 claims description 40
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- 239000010439 graphite Substances 0.000 claims description 34
- 239000011812 mixed powder Substances 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 19
- 238000011049 filling Methods 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 16
- 238000005551 mechanical alloying Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
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- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000009417 prefabrication Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 8
- 239000010936 titanium Substances 0.000 description 280
- 239000000919 ceramic Substances 0.000 description 53
- 239000007791 liquid phase Substances 0.000 description 47
- 239000011159 matrix material Substances 0.000 description 33
- 239000012071 phase Substances 0.000 description 22
- 239000011148 porous material Substances 0.000 description 21
- 229910052799 carbon Inorganic materials 0.000 description 16
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- 239000011153 ceramic matrix composite Substances 0.000 description 13
- 238000002844 melting Methods 0.000 description 13
- 230000008018 melting Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 239000000956 alloy Substances 0.000 description 9
- 238000000280 densification Methods 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 238000001513 hot isostatic pressing Methods 0.000 description 7
- 239000011156 metal matrix composite Substances 0.000 description 7
- 238000002490 spark plasma sintering Methods 0.000 description 7
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 6
- 229910001069 Ti alloy Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910052774 Proactinium Inorganic materials 0.000 description 4
- 239000011195 cermet Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
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- 239000000203 mixture Substances 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
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- 239000001995 intermetallic alloy Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
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- 238000000626 liquid-phase infiltration Methods 0.000 description 1
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- 229910001092 metal group alloy Inorganic materials 0.000 description 1
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Abstract
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass: ni (Ni) 3 Ti intermetallic compound powder, WC powder, al 2 O 3 Powder, Y 2 O 3 Powder, phenolic resin binder; ni (Ni) 3 The preparation method of the Ti/WC composite material comprises the following steps: first, ni is prepared 3 Ti intermetallic compound powder; then Ni prepared 3 Mixing Ti intermetallic compound powder with WC powder and adding Al 2 O 3 Powder and Y 2 O 3 Powder sintering aid, phenolic resin binder and wet ball milling to mix and dry to prepare Ni 3 Ti/WC composite powder, preparing a strip sample blank, and carrying out a liquid metal infiltration process preparation method on the strip sample blank under vacuum conditionsA liquid metal infiltration process; preparation of Ni 3 Ti/WC composite material; the preparation method of the invention prepares Ni 3 The Ti/WC composite material block has low preparation cost and simple preparation process, and can be used for preparing Ni with complex shape 3 The Ti/WC composite material product has the advantages of higher density, higher mechanical property, excellent wear resistance and large-scale industrialized production.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and in particular relates to Ni 3 Ti/WC composite material and liquid metal infiltration process preparation method thereof, relating to a low-cost Ni preparation method 3 Preparation method of Ti/WC composite material by liquid metal infiltration process, in particular to preparation of Ni by adopting mechanical alloying process and heat treatment process 3 Ti intermetallic compound powder, and Ni 3 Preparation of Ni by mixing Ti intermetallic Compound powder with WC powder by wet ball milling and drying 3 Ti/WC composite powder and Ni is prepared by a pressure forming process 3 Ti/WC composite powder preform, according to sintering temperature higher than Ni 3 Ni is prepared by utilizing the liquid metal melting infiltration principle under the melting point condition of Ti intermetallic compound and through a liquid metal infiltration process method 3 Ti/WC composite material blocks.
Background
The nickel-titanium intermetallic compound has higher mechanical property, good wear resistance, corrosion resistance, high-temperature oxidation resistance and the like and is widely applied in the industrial field. The nickel-titanium intermetallic compound mainly comprises Ni 3 Ti intermetallic compounds and NiTi intermetallic compounds. Due to Ni 3 Ti intermetallic compounds have many very excellent properties and are therefore widely used in engineering. Ni (Ni) 3 The Ti intermetallic compound has high strength, high toughness, high melting point, high hardness, good wear resistance, corrosion resistance and high-temperature oxidation resistance and is widely used in the engineering field. Ni (Ni) 3 The Ti intermetallic compound has unique shape memory effect and super elasticity, excellent toughness matching and excellent biocompatibility, and is widely applied in the fields of industrial equipment, bioengineering and the like. In addition to NiTi, ni is also present in the Ni-Ti binary alloy system 3 Ti、NiTi 2 Two intermetallic compounds, wherein Ni 3 Ti has a hexagonal DO 24-type crystal structure and is widely used as a precipitation-strengthened phase in cobalt-based, nickel-based, and iron-based superalloys. Recent studies have shown that Ni 3 The Ti intermetallic alloy also exhibits excellent wear resistance under dry sliding wear conditions. For several near equiatomic ratios Ni 3 The sliding wear properties of Ti alloys were studied and found to be Ni under high load 3 Although the Ti alloy is hardThe degree is obviously lower, but the wear resistance is obviously better than that of nitriding 38CrMoAl steel and Co45 cobalt-based wear-resistant alloy; its unique superelastic and high damping properties are considered to be Ni 3 Ti alloys have a major reason for their excellent wear resistance. For Ni 3 The wear resistance of Ti alloy is studied, and the shape memory effect and the super elasticity are considered to change the surface contact state, and martensite preferred orientation and stress induced martensite phase transformation have passivation effect on cracks, so that Ni is caused 3 The Ti alloy has good dry sliding abrasion resistance. Ni therefore 3 The Ti intermetallic compound has the most outstanding advantage of excellent wear resistance. Tungsten carbide ceramic materials are widely used in engineering fields due to their high strength and hardness, good wear resistance and high-temperature oxidation resistance. Tungsten carbide material belongs to hard alloy. However, tungsten carbide ceramics have a relatively high brittleness and a relatively low fracture toughness, and therefore, it is necessary to add a reinforcing and toughening phase to the WC matrix. Ni (Ni) 3 The Ti intermetallic compound can be used as a reinforcing and toughening phase of the tungsten carbide hard alloy due to higher bending strength and fracture toughness. Ni can be added to the cemented tungsten carbide 3 Formation of Ti intermetallic compound into Ni 3 The Ti/WC composite material can greatly improve the bending strength and the fracture toughness of the tungsten carbide hard alloy. Ni (Ni) 3 The compatibility of Ti intermetallic compound and WC is good, ni can be used 3 Ti intermetallic compound is added into WC matrix to form Ni through recombination 3 The Ti/WC composite material greatly improves and enhances the fracture toughness of the WC ceramic material. Thus Ni is produced 3 Ti/WC composites are the main focus and focus of research. At present, most researchers use a hot press sintering process to prepare Ni 3 Ti/WC composite material blocks. However, due to the high cost of the hot press sintering process, the preparation process is complex, and it is difficult to prepare Ni having a complex shape 3 The Ti/WC composite material products are difficult to realize industrialized production, and the industrialization is difficult to realize, which limits Ni 3 Ti/WC composite materials are widely used in the engineering field.
At present, most researchers use a hot press sintering process to prepare Ni 3 Ti/WC composite material blocks. But is composed ofThe preparation cost is high in the hot-press sintering process, the preparation process is complex, and the Ni with complex shape is difficult to prepare 3 The Ti/WC composite material products are difficult to realize industrialized production, and the industrialization is difficult to realize, which limits Ni 3 Ti/WC composite materials are widely used in the engineering field. The adoption of the normal pressure sintering process is that sintering is carried out under the condition of no pressure, so that compact Ni can not be obtained at all 3 Ti/WC composite material blocks can only obtain Ni with extremely high porosity 3 The Ti/WC composite material blocks cannot be prepared by adopting an atmospheric sintering process. Although the hot isostatic pressing sintering process can obtain compact Ni 3 The Ti/WC composite material blocks are too high in preparation cost by the hot isostatic pressing sintering process, the hot isostatic pressing equipment is expensive, and the preparation process is too complex, so that the preparation cannot be carried out by the hot isostatic pressing sintering process. Although dense Ni can be obtained by the spark plasma sintering process 3 The Ti/WC composite material blocks are too high in preparation cost by the spark plasma sintering process, and the spark plasma sintering equipment is high in price, and the preparation process is too complex, so that the spark plasma sintering process cannot be adopted for preparation. Therefore, the preparation cost is higher by adopting the powder metallurgy sintering process, the preparation process is more complex, and the Ni with complex shape is difficult to prepare 3 The Ti/WC composite material products are difficult to realize industrialized production, and the industrialization is difficult to realize, which limits Ni 3 Ti/WC composite materials are widely used in the engineering field.
Liquid metal infiltration techniques are the primary method of preparing metal matrix composites, cermet composites, and intermetallic/ceramic matrix composites. The infiltration method is to prepare ceramic matrix composite material by utilizing capillary pressure effect generated by intermetallic compound or metal melt with strong wettability, and spontaneously infiltrate into prefabricated member formed by ceramic powder. Ceramic powders are typically pressed under pressure to form a preform having a shape and density, and then intermetallic compounds or metal raw materials are placed on top or bottom of the preform, and the intermetallic compounds or metals melt at high temperatures to infiltrate the preform pores to form the composite material. The intermetallic compound powder and the ceramic powder can be mixed, and the mixture is subjected to pressure forming to prepare a powder preform, and the intermetallic compound is infiltrated into the ceramic preform at a high temperature, so that the liquid metal infiltration is realized to prepare the intermetallic compound/ceramic matrix composite. The liquid metal infiltration technique can be widely applied to the engineering field because of the advantage of being capable of achieving net near-dimensional forming. The intermetallic compound/ceramic matrix composite products prepared by the liquid metal infiltration technology can be various, can be made into various parts in various shapes such as strip, wafer, circular ring, cylinder, cube and the like, and can also be prepared into parts with complex shapes and complex structures according to the industrial requirements.
Infiltration is a process in which the melt spontaneously enters the porous preform of particles by capillary pressure caused by infiltration without the action of external forces. The ceramic powder can be preformed into a preform with a required shape and size by a conventional forming process, the metallic melt spontaneously infiltrates into and fills the pores in the preform, and after cooling and solidification, the composite material with uniformly distributed particles in a continuous matrix is obtained. The metal melt fusion infiltration method is that firstly, ceramic powder is made into a preform through a certain sintering process, and the metal melt or intermetallic compound melt spontaneously infiltrates into the ceramic preform at high temperature to form a sintered product. The infiltration method refers to a preparation process for forming a composite material by infiltration of a metal melt into a porous prefabricated member under the action of capillary force at high temperature, and comprises two mechanisms of physical infiltration and chemical infiltration. The principle and the technological process of physical infiltration are as follows: the ceramic is contacted with molten metal, and under certain atmosphere, alloy composition and process conditions, the wettability of the metal to the ceramic is enhanced or the molten metal reacts with trapped gas in the preform to create a vacuum, thereby allowing the metal melt to spontaneously infiltrate into the ceramic material. The principle and the technological process of chemical permeation are as follows: the component elements or the compounds of the ceramic phase are fully mixed to prepare a pressed compact, the pressed compact is placed in an alloy solution, and the pressed compact is directly reacted with the alloy solution at high temperature to generate ceramic particles which are uniformly distributed in the alloy solution to form the ceramic matrix composite or the metal matrix composite. Intermetallic/ceramic matrix composite articles may be prepared using melt infiltration of the metal. The pressureless infiltration method is to use the capillary pressure effect generated by intermetallic compound or metal melt with strong wettability to spontaneously infiltrate into the preformed member formed by ceramic powder. Ceramic powders are typically pressed under pressure to form a preform having a shape and density, and then intermetallic compounds or metal raw materials are placed on top or bottom of the preform, and the intermetallic compounds or metals melt at high temperatures to infiltrate the preform pores to form the composite material. Thus, an infiltration process may be used to prepare the intermetallic/ceramic matrix composite.
Liquid metal infiltration techniques are the primary method of preparing metal matrix composites, cermet composites, and intermetallic/ceramic matrix composites. The main process of preparing intermetallic compound/ceramic matrix composite material by molten metal infiltration method is that ceramic powder is prepared into disc porous material in advance, and then enters into molten intermetallic compound at a certain temperature, and then vacuum is pumped in furnace chamber to make the molten intermetallic compound fill up the pores to form intermetallic compound/ceramic composite material. The method has the advantages that: the process is simple, the cost is low, no special requirement is made on raw materials, particularly metal powder, no complex mechanical alloying process is needed, and large-scale production of products is realized; a near net-shape metal matrix composite can be obtained.
Liquid metal infiltration techniques are the primary method of preparing metal matrix composites, cermet composites, and intermetallic/ceramic matrix composites. The metal matrix composite can be prepared by a liquid metal infiltration process, for example, ceramic powder is first made into a green body by a pressure molding process, a porous prefabricated member is prepared by a normal pressure sintering process, and the metal matrix composite is prepared by an aluminizing process. The intermetallic compound/ceramic matrix composite can be prepared by adopting a liquid metal infiltration process, ceramic powder is generally pressed into a prefabricated member with a certain shape and density under a certain pressure, then an intermetallic compound raw material is placed at the top or bottom of the prefabricated member, and the intermetallic compound is melted and infiltrated into the pores of the prefabricated member at a high temperature, so that the intermetallic compound/ceramic matrix composite is formed. For example, intermetallic compounds are melted at high temperatures and then infiltrated into a ceramic preform to form an intermetallic/ceramic matrix composite. The metal material or metal alloy material may also be infiltrated into the ceramic matrix to form a cermet composite.
Disclosure of Invention
To overcome the defects of the prior art, the invention aims to provide Ni 3 The Ti/WC composite material and the preparation method of the liquid metal infiltration process thereof overcome the problems that the operation processes of a hot pressing sintering process, a normal pressure sintering process, a hot isostatic pressing sintering process and a spark plasma sintering process are too complex, the hot pressing sintering equipment, the spark plasma sintering equipment, the hot isostatic pressing sintering equipment are complex in structure and high in price, the preparation process is high in cost, the shape and the size of the prepared product are limited, the adopted liquid metal infiltration process only needs a vacuum high-temperature sintering furnace, the vacuum high-temperature sintering furnace with the sintering temperature below 2000 ℃ can be used, and the vacuum high-temperature sintering furnace has low equipment cost because no complex pressurizing system. The liquid metal infiltration process can simplify the production process, reduce the production cost, and can be used for preparing sintered products with complex shapes, and Ni prepared by the liquid metal infiltration process 3 The Ti/WC composite material has the advantages of higher density, higher mechanical property and good wear resistance.
In order to achieve the above purpose, the invention adopts the following technical scheme:
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 10 to 60 parts of Ti intermetallic compound powder, 40 to 90 parts of WC powder and Al 2 O 3 3 to 8 parts of powder, Y 2 O 3 2 to 7 parts of powder and 5 to 10 parts of phenolic resin binder.
Ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps:
by mechanical alloyingProcess and heat treatment process for preparing Ni 3 The Ti intermetallic compound powder is ball-milled for 60 hours by adopting mechanical alloying process to prepare Ni-Ti intermetallic compound powder, wherein the mol ratio of the Ni powder to the Ti powder is 75:25, a step of selecting a specific type of material;
the prepared Ni-Ti intermetallic compound powder is subjected to a heat treatment process, wherein the heat treatment process is carried out at the temperature of 800-1200 ℃ for 1h under the vacuum condition, and Ni is prepared through the heat treatment process 3 Ti intermetallic compound powder.
The Ni 3 Intermetallic Ti compounds in Ni 3 The Ti/WC composite material comprises 10-60 parts by mass.
The Ni 3 The molar ratio of the Ni powder to the Ti powder in the Ti intermetallic compound powder was 75:25.
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
Firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 75-100 mu m; the purity of the Ti powder is 99 percent, and the granularity is 75-100 mu m;
and step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling Ni-Ti intermetallic compound powder into a graphite crucible, and then putting the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature is 800-1200 ℃, the heat preservation time is 1h, and the vacuum degree is 10 -2 The heat treatment process is carried out under the vacuum condition of Pa,preparation of Ni 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 10 to 60 parts of Ti intermetallic compound powder and 40 to 90 parts of WC powder are mixed, and Al is added into the mixed powder 2 O 3 3 to 8 parts of powder and Y 2 O 3 2-7 parts of powder of sintering aid, and 5-10 parts of phenolic resin binder are added to be mixed to obtain mixed powder; carrying out wet ball milling mixing process on the mixed powder through mechanical ball milling, loading the mixed powder into a ball milling tank, adding 100-300 ml of absolute ethyl alcohol and 30-50 agate grinding balls with the diameter of 10-15 mm into the ball milling tank, and carrying out mechanical ball milling mixing for 24 hours to prepare slurry; filling the slurry into a glass beaker, and putting the glass beaker into an oven to dry at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder; and Ni is added with 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Filling Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for a pressure molding process, wherein the molding pressure is 200MPa, the dwell time is 60s, and the dimensions of a strip-shaped sample blank obtained after the pressure molding are 50mm multiplied by 5mm multiplied by 6mm; the blank of the strip sample is put into a drying oven to be dried for 24 hours at 150 ℃ to completely solidify the phenolic resin, thus obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample prefabricated body.
Step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out at 1500-1750 deg.C for 2h and 10 deg.C under vacuum condition -2 Pa, the temperature rising speed in the sintering process is 10-35 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
In the first step and the second step, the average granularity of the Ni-Ti intermetallic compound powder is 10-15 mu m, the granularity of the powder is extremely fine, and the Ni is obtained after the heat treatment process 3 The average particle size of the Ti intermetallic compound powder is still10-15 μm and Ni 3 The Ti intermetallic compound powder has an ordered structure.
In the third step, the granularity of WC powder is 5-8 mu m, ni 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder is 10-60 parts by mass.
The beneficial effects of the invention are as follows:
compared with the prior art, the invention firstly adopts a mechanical alloying process and a heat treatment process to prepare Ni 3 Ti intermetallic compound powder, and Ni 3 Preparation of Ni by mixing Ti intermetallic compound powder with WC powder 3 Ti/WC composite powder, preparing a strip-shaped sample blank by pressure forming, and preparing Ni by a liquid metal infiltration process method 3 Ti/WC composite material blocks. The invention adopts the liquid metal infiltration process with lower cost and simple preparation process, and can prepare Ni with complex shape 3 The Ti/WC composite material product is suitable for industrial production and is beneficial to realizing industrialization. The invention utilizes the sintering temperature higher than Ni 3 Ni under the condition of Ti intermetallic compound melting point 3 The Ti intermetallic compound is melted to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase particles and WC particles can be sintered into compact Ni 3 Ti/WC composite material blocks.
The invention provides a method for preparing Ni by adopting a liquid metal infiltration process 3 Ti/WC composite material blocks. The traditional hot-pressing sintering process method has higher cost, the preparation process is complex, the shape and the size of the prepared product are limited, and the large-scale production and the industrialization are difficult to realize. The liquid metal infiltration process is adopted to prepare the green body which is subjected to pressure forming, the liquid metal infiltration process is only required to sinter, the preparation cost is low, the preparation process is simple, the sintered product with complex shape can be prepared, the industrial production is easy, and the industrialization is facilitated. At the same time due to Ni 3 The sintering process of the Ti/WC composite material is higher than Ni 3 Ni under the condition of the melting point of Ti intermetallic compound 3 The melting point of Ti intermetallic compound is 1380 deg.C, sintering temperature is 1500 deg.C-1750 deg.C, at this temperatureNi under degree 3 The Ti intermetallic compound has melted to form a liquid phase, the formed liquid phase fills the pores in the WC matrix, and Ni 3 The Ti intermetallic compound liquid phase is bonded with WC particles through a liquid metal infiltration process preparation method to form a compact sintered block. The preparation method of the liquid metal infiltration process can obtain a sintered product with higher density and uniform and compact microstructure, and the sintered product also has higher mechanical property. Wherein 10 parts by weight of Al is added 2 O 3 Powder and Y 2 O 3 The function of the powder sintering aid is to contain Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix, plays a role in filling pores, and improves the mechanical property of the ceramic composite material. The phenolic resin binder with the mass portion of 10 parts is added into the composite powder to improve the strength and the hardness of the strip-shaped sample blank after the pressure molding, prevent the sample from being broken and destroyed when the sample is taken and put into a graphite crucible, ensure the integrity of the strip-shaped sample blank, decompose into gas at high temperature in the sintering process to volatilize, only contain a small amount of residual carbon, and the residual carbon is mixed in the sintered sample, so that the final product is not affected. Therefore, the Ni prepared by adopting the liquid metal infiltration process preparation method of the invention 3 The Ti/WC composite material block has the advantages of low cost and high performance, and parts with complex shapes can be prepared according to engineering requirements, so that the method has important significance and practical value.
Drawings
FIG. 1 shows Ni prepared by the method provided by the invention 3 X-ray diffraction pattern of Ti/WC composite material blocks.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, wherein the molar ratio of the Ni powder to the Ti powder is 75:25, a step of selecting a specific type of material;
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 75 mu m; the purity of the Ti powder is 99 percent, and the granularity is 75 mu m;
And step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling Ni-Ti intermetallic compound powder into a graphite crucible, and then putting the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature of the heat treatment process is 800 ℃, the heat preservation time is 1h, and the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa, ni is prepared by a heat treatment process 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 10 parts of Ti intermetallic compound powder and 90 parts of WC powder were mixed, and Al was added to the mixed powder 2 O 3 8 parts of powder and Y 2 O 3 2 parts of powder of sintering aid, and adding 5 parts of phenolic resin binder for mixing to obtain mixed powder; wet ball milling the mixed powder through mechanical ball milling, loading the obtained mixed powder into a ball milling tank, adding 100 milliliters of absolute ethyl alcohol and 30 agate grinding balls with the diameter of 10mm into the ball milling tank, carrying out mechanical ball milling and mixing for 24 hours to prepare slurry, loading the slurry into a glass beaker, placing the glass beaker into a baking oven, and drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder; ni is added with 3 Ti/WC composite powderForming into strip sample by overpressure, and mixing Ni with 3 The Ti/WC composite powder is put into a steel mold, the steel mold is placed into a molding press for pressure molding, the molding pressure is 200MPa, the dwell time is 60s, and the dimensions of a strip-shaped sample blank obtained after pressure molding are 50mm multiplied by 5mm multiplied by 6mm. The strip-shaped sample blank is put into a drying box and dried for 24 hours at 150 ℃ to completely solidify the phenolic resin, thus obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample preform, wherein Ni 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder comprises 10 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out by sintering at 1500 deg.C for 2h and vacuum degree of 10 -2 Pa, wherein the temperature rising speed in the sintering process is 10 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of the Ti intermetallic compound is 1380 ℃, and Ni is sintered at 1500 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 The Ti intermetallic compound liquid phase particles and WC particles have good wettability, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 YAG phase, forming liquid phase to promote densification of ceramic composite material matrix and improve mechanical property of ceramic composite materialPerformance. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. Therefore, ni with higher density and higher mechanical property can be prepared by the liquid metal infiltration process preparation method 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material comprises 10 parts by mass.
Example 2:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 80 mu m; the purity of the Ti powder is 99 percent, and the granularity is 80 mu m;
and step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling Ni-Ti intermetallic compound powder into a graphite crucible, and then putting the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature of the heat treatment process is 900 ℃, the heat preservation time is 1h, and the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa, ni is prepared by a heat treatment process 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 20 parts of Ti intermetallic compound powder and 80 parts of WC powder were mixed, and after mixingAdding Al to the powder of (2) 2 O 3 Powder 7 parts and Y 2 O 3 3 parts of powder of sintering aid, and adding 6 parts of phenolic resin binder for mixing to obtain mixed powder; wet ball milling mixing process is carried out on the mixed powder through mechanical ball milling, the obtained mixed powder is filled into a ball milling tank, 150 milliliters of anhydrous ethanol and 35 agate grinding balls with the diameter of 11mm are added into the ball milling tank for mechanical ball milling and mixing for 24 hours to prepare slurry, the slurry is filled into a glass beaker, and the glass beaker is put into an oven for drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder, ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Placing Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for pressure molding under the molding pressure of 200MPa and the pressure maintaining time of 60s, obtaining a strip-shaped sample blank with the size of 50mm multiplied by 5mm multiplied by 6mm after pressure molding, placing the strip-shaped sample blank into a drying box, and drying at 150 ℃ for 24 hours to completely cure phenolic resin, thereby obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample prefabricated body. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder comprises 20 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out at 1550 deg.C for 2h and 10 deg.C under vacuum condition -2 Pa, wherein the heating speed in the sintering process is 15 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of Ti intermetallic compound is 1380 ℃, ni when sintered at 1550 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 Intermetallic Ti compoundsThe wettability of the liquid-phase particles and WC particles is good, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. Therefore, ni with higher density and higher mechanical property can be prepared by the liquid metal infiltration process preparation method 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material comprises 20 parts by mass.
Example 3:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
preparing Ni-Ti intermetallic compound powder, wherein the mole ratio of Ni powder to Ti powder is 75:25, loading Ni powder and Ti powder into a ball milling tank of a QM-1SP2 planetary ball mill, wherein the molar ratio of the Ni powder to the Ti powder is 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 85 mu m; the purity of the Ti powder is 99 percent, and the granularity is 85 mu m;
And step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling the obtained Ni-Ti intermetallic compound powder into a graphite crucible, and then placing the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature of the heat treatment process is 1000 ℃, the heat preservation time is 1h, and the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa, ni is prepared by a heat treatment process 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 30 parts of Ti intermetallic compound powder and 70 parts of WC powder were mixed, and Al was added to the mixed powder 2 O 3 6 parts of powder and Y 2 O 3 4 parts of powder of sintering aid, and adding 7 parts of phenolic resin binder for mixing to obtain mixed powder; wet ball milling mixing process is carried out on the mixed powder through mechanical ball milling, the obtained mixed powder is filled into a ball milling tank, 200 milliliters of absolute ethyl alcohol and 40 agate grinding balls with the diameter of 12mm are added into the ball milling tank for mechanical ball milling and mixing for 24 hours to prepare slurry, the slurry is filled into a glass beaker, and the glass beaker is put into an oven for drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder and Ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Placing Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for pressure molding under the molding pressure of 200MPa and the pressure maintaining time of 60s, obtaining a strip-shaped sample blank with the size of 50mm multiplied by 5mm multiplied by 6mm after pressure molding, placing the strip-shaped sample blank into a drying box, and drying at 150 ℃ for 24 hours to completely cure phenolic resin, thereby obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample preform, wherein Ni 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder comprises 30 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; infiltration of liquid metalThe preparation method comprises sintering at 1600 deg.C for 2h, and vacuum infiltration with vacuum degree of 10 -2 Pa, wherein the temperature rising speed in the sintering process is 20 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of Ti intermetallic compound is 1380 ℃, ni when sintering is carried out at 1600 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 The Ti intermetallic compound liquid phase particles and WC particles have good wettability, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. Therefore, ni with higher density and higher mechanical property can be prepared by the liquid metal infiltration process preparation method 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material is 30 parts by mass.
Example 4:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 90 mu m; the purity of the Ti powder is 99 percent, and the granularity is 90 mu m;
and step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling the obtained Ni-Ti intermetallic compound powder into a graphite crucible, and then placing the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature of the heat treatment process is 1100 ℃, the heat preservation time is 1h, and the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa. Ni is prepared through a heat treatment process 3 Ti intermetallic compound powder.
Step three, ni prepared in the step two is processed 3 40 parts of Ti intermetallic compound powder and 60 parts of WC powder were mixed, and Al was added to the mixed powder 2 O 3 5 parts of powder and Y 2 O 3 5 parts of powder of sintering aid, and adding 8 parts of phenolic resin binder for mixing to obtain mixed powder; wet ball milling mixing process is carried out on the mixed powder through mechanical ball milling, the obtained mixed powder is filled into a ball milling tank, 250 milliliters of anhydrous ethanol and 45 agate grinding balls with the diameter of 13mm are added into the ball milling tank for mechanical ball milling and mixing for 24 hours to prepare slurry, the slurry is filled into a glass beaker, and the glass beaker is put into an oven for drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder and Ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Filling Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for pressure molding, wherein the molding pressure is 200MPa, the dwell time is 60s, and the steel mold is formed byThe bar-shaped sample blank with the size of 50mm multiplied by 5mm multiplied by 6mm is obtained after the overpressure forming, the bar-shaped sample blank is put into a drying box and dried for 24 hours at 150 ℃ to completely solidify the phenolic resin, and the Ni containing the phenolic resin binder with certain strength is obtained 3 Ti/WC composite powder strip-shaped sample prefabricated body. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder is 40 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out by sintering at 1650 deg.C for 2h, vacuum preserving for 10 -2 Pa, wherein the temperature rising speed in the sintering process is 25 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of Ti intermetallic compound is 1380 ℃, ni when sintering is carried out at 1650 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 The Ti intermetallic compound liquid phase particles and WC particles have good wettability, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. So that the preparation method can be realized through the liquid metal infiltration processTo prepare Ni with higher density and higher mechanical property 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material is 40 parts by mass.
Example 5:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 95 mu m; the purity of the Ti powder is 99 percent, and the granularity is 95 mu m;
And step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling the obtained Ni-Ti intermetallic compound powder into a graphite crucible, and then placing the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature of the heat treatment process is 1150 ℃, the heat preservation time is 1h, and the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa. Ni is prepared through a heat treatment process 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 50 parts of Ti intermetallic compound powder and 50 parts of WC powder were mixed, and Al was added to the mixed powder 2 O 3 4 parts of powder and Y 2 O 3 6 parts of powder of sintering aid, and adding 9 parts of phenolic resin binder for mixing to obtain mixed powder; passing the mixed powder through a machineWet ball milling mixing process, loading the obtained mixed powder into a ball milling tank, adding 300 ml of absolute ethanol and 50 agate grinding balls with the diameter of 14mm into the ball milling tank, carrying out mechanical ball milling mixing for 24 hours to prepare slurry, loading the slurry into a glass beaker, placing the glass beaker into a baking oven, and drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder and Ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Placing Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for pressure molding under the molding pressure of 200MPa and the pressure maintaining time of 60s, obtaining a strip-shaped sample blank with the size of 50mm multiplied by 5mm multiplied by 6mm after pressure molding, placing the strip-shaped sample blank into a drying box, and drying at 150 ℃ for 24 hours to completely cure phenolic resin, thereby obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample preform, wherein Ni 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder comprises 50 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out by sintering at 1700 deg.C for 2h and vacuum degree of 10 -2 Pa, wherein the temperature rising speed in the sintering process is 30 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of Ti intermetallic compound is 1380 ℃, ni when sintering is carried out at 1700 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 The Ti intermetallic compound liquid phase particles and WC particles have good wettability, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. Therefore, ni with higher density and higher mechanical property can be prepared by the liquid metal infiltration process preparation method 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material is 50 parts by mass.
Example 6:
ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process comprises the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 100 mu m; the purity of the Ti powder is 99 percent, and the granularity is 100 mu m;
and step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
the obtained Ni-Ti intermetallic compound powder is put into a graphite crucible, and then the graphite crucible is put into a vacuum furnaceIn a furnace, the heat treatment temperature of the heat treatment process is 1200 ℃, the heat preservation time is 1h, the heat treatment process is carried out under the vacuum condition, and the vacuum degree is 10 -2 Pa, ni is prepared by a heat treatment process 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 60 parts of Ti intermetallic compound powder and 40 parts of WC powder were mixed, and Al was added to the mixed powder 2 O 3 3 parts of powder and Y 2 O 3 7 parts of powder of sintering aid, and adding 10 parts of phenolic resin binder for mixing to obtain mixed powder; wet ball milling mixing process is carried out on the mixed powder through mechanical ball milling, the obtained mixed powder is filled into a ball milling tank, 300 milliliters of absolute ethyl alcohol and 50 agate grinding balls with the diameter of 15mm are added into the ball milling tank for mechanical ball milling and mixing for 24 hours to prepare slurry, the slurry is filled into a glass beaker, and the glass beaker is put into an oven for drying at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder and Ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Placing Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for pressure molding under the molding pressure of 200MPa and the pressure maintaining time of 60s, obtaining a strip-shaped sample blank with the size of 50mm multiplied by 5mm multiplied by 6mm after pressure molding, placing the strip-shaped sample blank into a drying box, and drying at 150 ℃ for 24 hours to completely cure phenolic resin, thereby obtaining Ni with certain strength and containing phenolic resin binder 3 Ti/WC composite powder strip-shaped sample prefabricated body. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder comprises 60 parts by mass;
step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out by sintering at 1750 deg.C for 2h and vacuum degree of 10 -2 Pa, wherein the temperature rising speed in the sintering process is 35 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
Wherein Ni is 3 The melting point of Ti intermetallic compound is 1380 ℃, ni when sintered at 1750 DEG C 3 The Ti intermetallic compound particles melt to form a liquid phase, ni 3 The Ti intermetallic compound liquid phase infiltrates into the middle of WC particles through the pores in the WC matrix, so that the molten Ni 3 The Ti intermetallic compound liquid phase fills the pores in the WC ceramic matrix due to Ni 3 The Ti intermetallic compound liquid phase particles and WC particles have good wettability, ni 3 The Ti intermetallic compound can be well bonded with WC particles to form compact Ni 3 The Ti/WC composite material is sintered into a block. And Ni 3 The higher the Ti intermetallic compound content, ni 3 The Ti/WC composite is more dense. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. And a small amount of phenolic resin binder is decomposed into gas at high temperature to volatilize, and only a small amount of residual carbon is mixed in the sintered sample. Therefore, ni with higher density and higher mechanical property can be prepared by the liquid metal infiltration process preparation method 3 Ti/WC composite material blocks. Therefore, ni is prepared by the liquid metal infiltration process 3 Ti/WC composite material blocks. Wherein Ni is 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite material comprises 60 parts by mass.
Example 7
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 60 parts of Ti intermetallic compound powder, 40 parts of WC matrix powder and sintering aid Al 2 O 3 3 parts of powder and Y 2 O 3 7 parts of powder and 10 parts of phenolic resin binder.
Example 8
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 50 parts of Ti intermetallic compound powder, 50 parts of WC matrix powder and sintering aid Al 2 O 3 4 parts of powder and Y 2 O 3 6 parts of powder and 9 parts of phenolic resin binder.
Example 9
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 40 parts of Ti intermetallic compound powder, 60 parts of WC matrix powder and sintering aid Al 2 O 3 5 parts of powder and Y 2 O 3 5 parts of powder and 8 parts of phenolic resin binder.
Example 10
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 30 parts of Ti intermetallic compound powder, 70 parts of WC matrix powder and sintering aid Al 2 O 3 6 parts of powder and Y 2 O 3 4 parts of powder and 7 parts of phenolic resin binder.
Example 11
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 20 parts of Ti intermetallic compound powder, 80 parts of WC matrix powder and sintering aid Al 2 O 3 Powder 7 parts and Y 2 O 3 3 parts of powder and 6 parts of phenolic resin binder.
Example 12
Ni (nickel) 3 The Ti/WC composite material comprises the following components in parts by mass:
Ni 3 10 parts of Ti intermetallic compound powder, 90 parts of WC matrix powder and sintering aid Al 2 O 3 8 parts of powder and Y 2 O 3 2 parts of powder and 5 parts of phenolic resin binder.
As can be seen from examples 1-6, the liquid metal infiltration process adopted in examples 1-6 is simple in preparation process and low in cost, and does not need to use complicated and expensive hot-pressing sintering equipment, spark plasma sintering equipment and hot isostatic pressing sintering equipment. The adopted liquid metal infiltration process only needs a vacuum high-temperature sintering furnace, and the vacuum high-temperature sintering furnace with the sintering temperature below 2000 ℃ can be used. The vacuum high-temperature sintering furnace has low equipment cost because of no complex pressurizing system. The liquid metal infiltration process has low cost and simple preparation process, and can prepare compact composite material blocks. The main advantages of the present invention over existing technology are therefore:
1) The invention adopts a mechanical alloying process and a heat treatment process to prepare Ni 3 The method comprises the steps of ball milling Ti intermetallic compound powder for 60 hours through mechanical alloying to prepare Ni-Ti intermetallic compound powder, and carrying out heat treatment at a heat treatment temperature of 800 ℃,900 ℃,1000 ℃,1100 ℃,1150 ℃ and 1200 ℃ for 1 hour to ensure that the molar ratio of the Ni powder to the Ti powder is 75:25 to generate Ni 3 Ti intermetallic compound powder, and Ni 3 Mixing Ti intermetallic compound powder with WC powder and adding Al 2 O 3 Powder and Y 2 O 3 The powder sintering aid and the phenolic resin binder are mixed by wet ball grinding and dried to prepare Ni 3 Ti/WC composite powder and Ni 3 The Ti/WC composite powder is made into a strip sample by pressure molding, and Ni is prepared by a liquid metal infiltration process 3 Ti/WC composite material blocks. The liquid metal infiltration process has the advantages of low preparation cost, simple preparation process, high preparation efficiency, and uniform and compact structure of Ni 3 Ti/WC composite material block and Ni prepared by adopting liquid metal infiltration method 3 The Ti/WC composite material block has higher mechanical property and excellent wear resistance. Ni with complex shape can be manufactured by adopting liquid metal infiltration method 3 Ti/WC composite articles.
2) At Ni 3 In the preparation process of the Ti/WC composite material block, 10 parts by weight of Al is added 2 O 3 Powder and Y 2 O 3 The function of the powder sintering aid is to contain Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix, plays a role in filling pores, and improves the mechanical property of the ceramic composite material. The phenolic resin binder with the mass portion of 10 parts is added into the composite powder to improve the strength and the hardness of the strip-shaped sample blank after pressure molding, prevent the sample from being broken and destroyed when the sample is taken and put into a graphite crucible, ensure the integrity of the sample, and decompose the phenolic resin binder into gas at high temperature to volatilize, wherein only a small amount of residual carbon is mixed in the sintered sample, and the final product is not affected.
3) Ni prepared by adopting liquid metal infiltration process 3 The Ti/WC composite material has a uniform and compact microstructure, has higher mechanical property, and simultaneously has Ni 3 High melting point, high hardness, high elastic modulus, and the like of Ti intermetallic compounds. Ni prepared by liquid metal infiltration process 3 The Ti/WC composite material has higher density and uniform and compact microstructure. Ni prepared by liquid metal infiltration process 3 The Ti/WC composite material has higher mechanical property and higher hardness, and has good wear resistance, good high-temperature oxidation resistance and the like. The invention is Ni 3 The invention develops a new preparation process for low-cost manufacture of Ti/WC composite materials, and the invention is used for promoting and promoting Ni 3 The Ti/WC composite material lays a foundation for wide application in the engineering field.
FIG. 1 shows Ni prepared by liquid metal infiltration process according to the method provided by the invention 3 X-ray diffraction pattern of Ti/WC composite material blocks. FIG. 1 shows Ni prepared by liquid metal infiltration process 3 XRD pattern of Ti/WC composite material block. As can be seen from FIG. 1, there is Ni in the XRD pattern 3 Diffraction peaks of Ti intermetallic compound phase and WC ceramic phase. In addition, there is a small amount of Y 3 Al 5 O 12 Diffraction peaks of the phases, i.e. of the YAG phase. Wherein Al during sintering 2 O 3 Powder and Y 2 O 3 The powder sintering aid reacts at high temperature to form liquid phase Y 3 Al 5 O 12 Namely YAG phase, forms liquid phase to promote densification of the ceramic composite material matrix and improves the mechanical property of the ceramic composite material. In XRD pattern there is Ni 3 Diffraction peaks of Ti intermetallic compound phase, and WC ceramic phase, which indicates Ni during the preparation of liquid metal infiltration process 3 The Ti intermetallic compound and WC ceramic do not react to generate other impurity phases, and Ni 3 The Ti intermetallic compound has good compatibility with WC ceramic, so Ni can be infiltrated by liquid metal 3 The Ti intermetallic compound and WC ceramic are sintered together to form compact Ni 3 Ti/WC composite material, wherein Ni 3 The Ti intermetallic compound is a strengthening and toughening phase, and WC ceramic is used as a matrix. Ni (Ni) 3 Ti intermetallic compound has strengthening and toughening effects on WC ceramic, ni 3 The Ti intermetallic compound can obviously improve the mechanical property of WC ceramic. Ni (Ni) 3 The Ti/WC composite material has Ni 3 The excellent properties of Ti intermetallic compounds also have the excellent properties of WC ceramics. The invention is Ni 3 The low-cost manufacture of Ti/WC composite material develops a new preparation process, and Ni is prepared by adopting a liquid metal infiltration process 3 The Ti/WC composite material has high preparation efficiency, low preparation cost and Ni prepared by a liquid metal infiltration process 3 The Ti/WC composite material has higher density and uniform and compact microstructure. Ni prepared by liquid metal infiltration process 3 The Ti/WC composite material has higher mechanical property and higher hardness, and has good wear resistance, good high-temperature oxidation resistance and the like. The invention is Ni 3 The invention develops a new preparation process for low-cost manufacture of Ti/WC composite materials, and the invention is used for promoting and promoting Ni 3 The Ti/WC composite material lays a foundation for wide application in the engineering field.
Claims (7)
1. Ni (nickel) 3 The Ti/WC composite material is characterized by comprising the following components in parts by weight:
Ni 3 10 to 60 parts of Ti intermetallic compound powder, 40 to 90 parts of WC powder and Al 2 O 3 3 to 8 parts of powder, Y 2 O 3 2 to 7 parts of powder and 5 to 10 parts of phenolic resin binder.
2. Ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized by comprising the following steps:
ni is prepared by adopting a mechanical alloying process and a heat treatment process 3 The Ti intermetallic compound powder is ball-milled for 60 hours by adopting mechanical alloying process to prepare Ni-Ti intermetallic compound powder, wherein the mol ratio of the Ni powder to the Ti powder is 75:25, a step of selecting a specific type of material;
the prepared Ni-Ti intermetallic compound powder is subjected to a heat treatment process, wherein the heat treatment process is carried out at the temperature of 800-1200 ℃ for 1h under the vacuum condition, and Ni is prepared through the heat treatment process 3 Ti intermetallic compound powder.
3. A Ni according to claim 1 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized in that the Ni 3 Intermetallic Ti compounds in Ni 3 The Ti/WC composite material comprises 10-60 parts by mass.
4. A Ni according to claim 1 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized in that the Ni 3 The molar ratio of the Ni powder to the Ti powder in the Ti intermetallic compound powder was 75:25.
5. ni (nickel) 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized by comprising the following steps of:
firstly, preparing Ni-Ti intermetallic compound powder by adopting a mechanical alloying process, which comprises the following specific steps:
ni powder and Ti powder were charged into a ball milling pot of a planetary ball mill of QM-1SP2 type, wherein the molar ratio of Ni powder to Ti powder was 75:25, after fixing four ball milling tanks, starting a planetary ball mill for ball milling, wherein the mechanical ball milling time is 60 hours, the rotating speed of the ball mill is 350r/min, adopting dry ball milling, and adopting an intermittent ball milling mode, and filling argon into the ball milling tanks as protective gas to prepare Ni-Ti intermetallic compound powder; the purity of the Ni powder is 99 percent, and the granularity is 75-100 mu m; the purity of the Ti powder is 99 percent, and the granularity is 75-100 mu m;
And step two, carrying out a heat treatment process on the Ni-Ti intermetallic compound powder prepared in the step one, wherein the specific method comprises the following steps:
filling Ni-Ti intermetallic compound powder into a graphite crucible, and then putting the graphite crucible into a vacuum sintering furnace, wherein the heat treatment temperature is 800-1200 ℃, the heat preservation time is 1h, and the vacuum degree is 10 -2 Performing heat treatment under Pa vacuum condition to obtain Ni 3 Ti intermetallic compound powder;
step three, ni prepared in the step two is processed 3 10 to 60 parts of Ti intermetallic compound powder and 40 to 90 parts of WC powder are mixed, and Al is added into the mixed powder 2 O 3 3 to 8 parts of powder and Y 2 O 3 2-7 parts of powder of sintering aid, and 5-10 parts of phenolic resin binder are added to be mixed to obtain mixed powder; carrying out wet ball milling mixing process on the mixed powder through mechanical ball milling, loading the mixed powder into a ball milling tank, adding 100-300 ml of absolute ethyl alcohol and 30-50 agate grinding balls with the diameter of 10-15 mm into the ball milling tank, and carrying out mechanical ball milling mixing for 24 hours to prepare slurry; filling the slurry into a glass beaker, and putting the glass beaker into an oven to dry at 100 ℃ for 24 hours to prepare Ni 3 Ti/WC composite powder; and Ni is added with 3 The Ti/WC composite powder is made into a strip sample by pressure molding, ni is used for preparing a strip sample 3 Filling Ti/WC composite powder into a steel mold, placing the steel mold into a molding press for a pressure molding process, wherein the molding pressure is 200MPa, the dwell time is 60s, and the dimensions of a strip-shaped sample blank obtained after the pressure molding are 50mm multiplied by 5mm multiplied by 6mm; the blank of the strip sample is put into a drying oven to be dried for 24 hours at 150 ℃ to completely solidify the phenolic resin, thus obtaining Ni with certain strength and containing phenolic resin binder 3 Prefabrication of Ti/WC composite powder strip-shaped sampleA body.
Step four, placing the strip-shaped blank body manufactured in the step three into a graphite crucible, and placing the graphite crucible into a vacuum high-temperature sintering furnace to be treated by a liquid metal infiltration process; the liquid metal infiltration process is carried out at 1500-1750 deg.C for 2h and 10 deg.C under vacuum condition -2 Pa, the temperature rising speed in the sintering process is 10-35 ℃/min; cooling with furnace after sintering process is finished, thus preparing Ni 3 Ti/WC composite material.
6. A Ni according to claim 5 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized in that in the first step and the second step, the average particle size of Ni-Ti intermetallic compound powder is 10-15 mu m, the powder particle size is extremely fine, and the Ni is obtained after the heat treatment process 3 The average particle size of the Ti intermetallic compound powder is still 10-15 μm, and Ni 3 The Ti intermetallic compound powder has an ordered structure.
7. A Ni according to claim 5 3 The preparation method of the Ti/WC composite material by the liquid metal infiltration process is characterized in that in the third step, WC powder has the granularity of 5-8 mu m and Ni 3 Ti intermetallic compound powder in Ni 3 The Ti/WC composite powder is 10-60 parts by mass.
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