CN109439984B - Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material - Google Patents

Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material Download PDF

Info

Publication number
CN109439984B
CN109439984B CN201811091941.5A CN201811091941A CN109439984B CN 109439984 B CN109439984 B CN 109439984B CN 201811091941 A CN201811091941 A CN 201811091941A CN 109439984 B CN109439984 B CN 109439984B
Authority
CN
China
Prior art keywords
powder
ball milling
amorphous alloy
magnesium
alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201811091941.5A
Other languages
Chinese (zh)
Other versions
CN109439984A (en
Inventor
彭建洪
杨永潇
毛多鹭
李海琴
李海宾
韩精卫
许珂琳
周德华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qinghai Nationalities University
Original Assignee
Qinghai Nationalities University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Qinghai Nationalities University filed Critical Qinghai Nationalities University
Priority to CN201811091941.5A priority Critical patent/CN109439984B/en
Publication of CN109439984A publication Critical patent/CN109439984A/en
Application granted granted Critical
Publication of CN109439984B publication Critical patent/CN109439984B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder

Abstract

The invention discloses a primary micro/nano-scale titanium carbide and amorphous alloy co-reinforced magnesium alloy composite material and a preparation method thereof, which mainly comprises the following steps: ball-milling titanium powder and graphite powder in proportion to obtain native titanium carbide (TiCp) alloy powder; mixing magnesium powder or aluminum powder or titanium powder with other alloy elements in proportion, and performing high-energy ball milling to obtain magnesium-based/aluminum-based/titanium-based amorphous alloy powder; adding TiCp alloy powder into amorphous alloy powder in proportion, performing high-energy ball milling to obtain mixed powder of TiCp and amorphous alloy, adding the mixed powder into magnesium alloy powder in proportion, adding alcohol, performing mechanical stirring in an ultrasonic-assisted mode, uniformly mixing, and drying; compacting the dried composite powder at high pressure to obtain a compact composite block blank, and then sintering at low temperature by hot pressing; and (3) performing thermal extrusion on the composite block obtained by sintering to obtain the high-strength and high-toughness native micro/nano-scale titanium carbide and amorphous alloy co-reinforced magnesium alloy composite material.

Description

Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material
Technical Field
The invention relates to a light metal composite material, in particular to a hard carbide and amorphous alloy co-reinforced magnesium alloy composite material and a preparation method thereof.
Background
The magnesium alloy material has the characteristics of low density, high specific strength, high specific stiffness, good damping performance, good thermal conductivity, easy recycling and the like, and is widely applied to the fields of aviation, aerospace, vehicles, 3C electronic products and the like. However, since most magnesium alloys have a Hexagonal Close Packed (HCP) crystal structure, the HCP structure has less independent sliding systems, resulting in a magnesium alloy having lower room temperature ductility and toughness, and in addition, the mechanical strength and creep resistance of the magnesium alloy are also lower, which limits the wide application of the magnesium alloy material.
According to the strengthening mechanism, the micro-nano-scale particles with high hardness and high modulus are compounded with the fine-grained magnesium alloy material, so that the comprehensive mechanical property of the magnesium alloy material can be obviously improved. At present, in the literature reports of research on magnesium-based composite materials at home and abroad, the reinforcements commonly used mainly include silicon carbide, oxides (such as alumina and silica), boron carbide, titanium boride, graphene, whiskers/fibers, carbon nanotubes and the like, and the preparation methods mainly include a stirring casting method, an extrusion casting method, a powder metallurgy method, a mechanical alloying method, a pressureless infiltration method, a plasma sintering method, friction stir welding and the like. Chinese patent (CN107523727A) discloses that a silicon carbide reinforced magnesium-based composite material with excellent mechanical properties (the maximum tensile strength is 305MPa, and the elongation reaches 8.25%) is prepared by an extrusion casting method. Chinese patent (CN201710138404.0) discloses a method for preparing a nano titanium carbide particle reinforced magnesium-based composite material, which comprises the steps of adding a prefabricated body into a liquid magnesium alloy, synchronously applying mechanical stirring under the action of ultrasonic vibration to a magnesium alloy melt which is heated to a temperature of above 70 ℃ and is doped with the nano titanium carbide particle prefabricated body, effectively solving the problem of uniform distribution of nano titanium carbide particles, realizing uniform distribution of the added nano titanium carbide particles, ensuring that the maximum tensile strength of the added nano titanium carbide particles reaches 345MPa, and simultaneously ensuring that the composite material has good plastic toughness (the elongation of the composite material reaches 18%). Chinese patent (application No. 201710900751.2) discloses a mixed phase reinforced magnesium-based composite material and a preparation method thereof, which mainly comprises the following process steps: pretreating magnesium alloy powder, nano diamond particles and magnesium borate whiskers to prepare mixed powder, mixing and ball-milling to obtain ball-milled mixed powder, and then carrying out vacuum hot-pressing to form a blank and hot-extrusion treatment. The friction wear and the tensile-compression symmetry of the mixed-phase reinforced magnesium-based composite material prepared by the method are remarkably improved, and the comprehensive mechanical properties are also remarkably improved (the tensile/compression yield strengths are 390MPa and 433MPa respectively, the highest tensile/compression strengths are 418MPa and 480MPa respectively, and the tensile/compression strain rates are 6.2% and 10.1% respectively).
At present, no report is found on the research of in-situ synthesis of micro-nano carbide and amorphous alloy particles for co-strengthening the magnesium-based composite material at home and abroad. Chinese patent (CN101368242A) discloses an amorphous reinforced magnesium-based composite material and a preparation process thereof, wherein the material comprises amorphous particles NixMyTz(M represents one or two of Zr and Nb, T represents at least one of Ta, Ti, Hf, Ti, Si, Pd, P, Sn, Co, Mo, B, Cr and Al; x is more than or equal to 30 and less than or equal to 70, y is more than or equal to 3 and less than or equal to 50, z is more than or equal to 0 and less than or equal to 35; a is more than or equal to 80 and less than or equal to 100, B is more than or equal to 0 and less than or equal to 18, c is more than or equal to 0 and less than or equal to 5, and d isaAlbQcRd(a + B + c + d is 100 weight percent, a is more than or equal to 80 and less than or equal to 100, B is more than or equal to 0 and less than or equal to 18, c is more than or equal to 0 and less than or equal to 5, d is more than or equal to 0 and less than or equal to 3, Q represents one or two of Mn and Zn, and R represents at least one of Ce, Zr, Cu, Ni, Si, Fe, B and Gd). The main process of the invention comprises the following steps: uniformly mixing magnesium alloy particles and amorphous alloy particles, performing cold pressing at a cold pressing pressure of 30-250MPa, and then sintering in a hot-pressing sintering furnace at a hot-pressing pressure of 5-60MPa and a sintering temperature of 500-700 ℃ for 30-180 min. The strength and toughness indexes of the amorphous reinforced magnesium-based composite material obtained by the invention are not ideal (the yield strength is 145MPa at most, the tensile strength is 263MPa at the same time, and the elongation is 4.3%), and the possible reasons are that the grain size of a matrix structure is larger (the toughness of the matrix structure is poor) due to the adoption of higher sintering temperature, and in addition, the phase interface in the deformation process is easy to damage due to poor bonding performance of the amorphous phase and the matrix phase interface, so that cracks are generated and rapidly expanded, and the composite material is brittle.
Disclosure of Invention
The main ideas of the invention are as follows: native micro/nano TiC with high specific surface area, high activity and high hardness prepared by mechanical alloying method in-situ synthesispAnd light metal-based amorphous alloy particles with high crystallization temperature and high hardness, and then the WC particles are mixed with the amorphous alloy particles to carry out high-energy ball milling (to large-size TiC)pThe particle part is embedded into the large-size amorphous alloy particles), and TiC is stirred by an ultrasonic-assisted mechanical stirring methodpGranules,Fully and uniformly mixing the amorphous alloy particles and the magnesium alloy powder, then densifying the composite powder under high pressure, and finally obtaining the high-strength high-toughness magnesium alloy composite material with a special three-phase coexisting structure by utilizing low-temperature sintering and hot extrusion processes. The main technical innovation of the invention is as follows: (1) forming a special three-phase coexistence structure, namely TiC with larger size in the composite materialpThe particles are simultaneously embedded in large-size amorphous alloy particles and a magnesium alloy matrix phase, the special structure can prevent the amorphous alloy phase from rotating along with matrix grains in the deformation process of the composite material, simultaneously, the amorphous phase has the function of preventing dislocation movement, and a phase interface with excellent mechanical property cannot be damaged under the action of larger shear stress, so that the integral strength of the composite material is greatly improved; (2) and fine TiCpAnd the amorphous alloy particles can be dispersed in the superfine crystal magnesium alloy matrix, and can play a good role in dispersion strengthening.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
step 1, mixing titanium powder and graphite powder in proportion, and performing high-energy ball milling for a period of time to obtain high-activity and high-specific-surface-area native TiCpGranular powder;
step 2, mixing light metal magnesium powder or aluminum powder or titanium powder with other alloy elements according to a certain proportion, and performing high-energy ball milling for a period of time to obtain magnesium-based or aluminum-based or titanium-based amorphous alloy particle powder with high activity and high crystallization temperature;
step 3, TiC obtained in the step 1pAdding the particle powder into the amorphous alloy particle powder obtained in the step 2 according to a certain proportion, and performing high-energy ball milling to obtain TiCpAnd amorphous alloy mixed powder;
step 4, TiC obtained in step 3pAdding the amorphous alloy mixed powder into magnesium alloy powder according to a certain proportion, adding a certain amount of alcohol, mechanically stirring in an ultrasonic-assisted mode to obtain uniformly mixed slurry, then putting the slurry into a vacuum oven for drying, and then obtaining composite powder;
step 5, placing the composite powder obtained in the step 4 in a mould, and performing high-pressure compaction by using a cold isostatic press or a four-column hydraulic press to obtain a compact composite block blank;
step 6, placing the compact composite block blank obtained in the step 5 into a vacuum hot-pressing sintering furnace for low-temperature hot-pressing sintering to obtain a high-density hot-pressing composite block material;
step 7, carrying out hot extrusion on the block composite material obtained in the step 6 at a high extrusion ratio to finally obtain the high-strength and high-toughness primary micro-nano/meter TiCpAnd the amorphous alloy is used for co-strengthening the magnesium alloy composite material bar.
Further, in the step 1, the molar ratio of the titanium powder to the graphite powder is 1: 1, the mixture is subjected to high-energy ball milling, and Ti and C elements react in situ by utilizing high ball milling energy to synthesize native TiC with high specific surface area and high activityp(according to the difference of ball milling energy and ball milling time, the degree of in-situ chemical reaction is different, and the range of the obtained p is 0.85-1). the ball milling time is 40-80 h, the ball-material ratio is 10: 1-20: 1, and the rotating speed is 300-600 r/min.
Further, in the step 2, magnesium powder or aluminum powder or titanium powder and other alloy elements (such as one or more of Cu, Ni, Si, Y, Fe, Ca, Zn, Nd, B, etc.) are mixed according to a certain proportion, and then the mixture is subjected to high-energy ball milling to obtain magnesium-based or aluminum-based or titanium-based amorphous alloy particle powder (the breaking strength of which is required to be not lower than 800MPa, the crystallization temperature is required to be not lower than 350 ℃), the ball milling time is 40-100 h, the ball-to-material ratio is 10: 1-50: 1, and the rotating speed is 300-600 r/min.
Further, in the step 3, TiCpThe mixing ratio of the particles to the amorphous alloy particles is 1: 6-1: 20, and TiC is obtained after high-energy ball millingpThe ball milling time of the mixed powder of the particles and the amorphous alloy particles is 20-40 h, the ball-material ratio is 10: 1-20: 1, and the rotating speed is 300-600 r/min. The purpose of this step is to make the TiC partially larger in sizepThe particles are embedded in the amorphous alloy particles and form a special three-phase coexisting structure, namely large TiC, in the final bulk composite materialpThe particles are embedded in the amorphous alloy phase and the matrix phase at the same time and are changed in the composite materialThe amorphous phase is prevented from rotating in the forming process, so that the overall strength of the composite material is greatly improved; and fine TiCpAnd the amorphous alloy particles are dispersed in the magnesium alloy matrix to play a role in dispersion strengthening.
Further, in the step 4, TiC added to the magnesium alloy powderpThe particles and the amorphous alloy particles respectively account for 0.25-5% and 5-30% of the total mass of the mixed powder, and the balance is magnesium alloy powder; the adding amount of the alcohol is only required to ensure that the slurry has enough fluidity during stirring; the ultrasonic power is 100-200 Hz, the rotating speed of the blades is 300-1000 rpm, and the stirring time is 30-60 min.
Furthermore, in the step 4, the grade of the magnesium alloy powder can be one of Mg-Al series, Mg-Zn series, Mg-Mn series, Mg-RE series or Mg-Zn-RE-Zr series.
Further, in the step 4, the slurry which is uniformly stirred and mixed is dried in vacuum, the vacuum degree is less than 100Pa, the drying temperature is 80 ℃, and the drying time is 24 hours.
Further, in the step 5, the mold is a stainless steel mold, the pressure of the cold isostatic pressing or the four-column hydraulic pressure is 300-600MPa, and the pressure maintaining time is 10-30 min.
Further, in the step 6, in order to prevent the crystal grain growth of the magnesium alloy matrix material in the sintering process, the vacuum hot pressing process adopts low-temperature sintering, the sintering temperature range is 300-350 ℃, the pressure is 50-100 MPa, and the pressure maintaining time is 20min-1 h. The purpose of low temperature sintering is: (1) the magnesium-based amorphous alloy is prevented from being crystallized and transformed in the compounding process, so that the strengthening effect of the amorphous alloy on the finally prepared composite material is ensured; (2) the magnesium alloy matrix of the final composite material is kept to be an ultrafine grain structure, so that the final composite material is ensured to have good plastic toughness.
Further, in the step 7, the temperature of hot extrusion is 280-300 ℃, the extrusion ratio is 25: 1, and the extrusion rate is 0.05-0.2 mm/s. The purpose of high extrusion specific heat extrusion is: further densifying the composite and possibly refining the matrix structure.
Further, the preparation method of the invention can also comprise a common magnesium alloy heat treatment method: t1-partial solution treatment and natural aging; t2-post-casting annealing; t3-solid solution + cold working; t4-solution treatment; t5-artificial aging; t6-solution treatment and artificial aging; t7-solution treatment and stabilization treatment; t8-polishing treatment, cold working and artificial aging.
Drawings
FIG. 1 is a process flow diagram of the preparation of the primary micro/nano-scale titanium carbide and amorphous alloy co-reinforced magnesium alloy composite material
Fig. 2 is a stress-strain graph of examples 1, 2, and 3.
Detailed Description
Example 1:
a method for preparing a native micro/nano titanium carbide and titanium-based amorphous alloy co-reinforced magnesium alloy composite material comprises the following steps:
step 1, weighing 8g of titanium powder and 2g of graphite powder, putting the titanium powder and the graphite powder into a 250ml ball milling tank, and then putting 100g of ball milling steel balls. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9 vol.%) into the ball milling tank from an air inlet at one end, putting the ball milling tank into a ball mill, wherein the ball milling time is 60 hours, and the rotating speed of the ball mill is 500rpm, so that the micro/nano TiC is obtainedpAnd (3) granular powder.
Step 2, according to Ti50Zr15Cu15Ni5V5Be10The molar ratio of elements in the molecular formula of the alloy compound is that titanium powder, zirconium powder, copper powder, nickel powder, vanadium powder and beryllium powder (the total mass of the powder is 25g) are weighed and put into a 500ml ball milling tank, and then 250g ball milling steel balls are put into the ball milling tank. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9v 01%) into the ball milling tank from an air inlet at one end, putting the ball milling tank into a ball mill, wherein the ball milling time is 100 hours, and the rotating speed of the ball mill is 500rpm, so that Ti is obtained50Zr15Cu15Ni5V5Be10Amorphous alloy particle powder.
Step 3, then TiC obtained in the step 1pGranular powder (5g) was added to the Ti obtained in step 250Zr15Cu15Ni5V5Be10Ball milling is continuously carried out on the amorphous alloy particle powder (the ball milling time is 20 hours, and the rotating speed of the ball mill is 500rpm), and then TiC is obtainedpParticles and Ti50Zr15Cu15Ni5V5Be10Mixed powder of amorphous alloy particles.
Step 4, taking out the mixed powder obtained in the step 3, weighing 75g of AZ91 magnesium alloy powder, putting the powder into a 500ml beaker, adding 200ml of alcohol into the beaker, and then carrying out ultrasonic-assisted mechanical stirring (the ultrasonic power is 100Hz, the blade rotation speed is 1000rpm, and the stirring time is 60 min); after stirring, putting the uniformly mixed slurry into a vacuum drying oven for drying (the vacuum degree is 50Pa, the drying temperature is 80 ℃, and the drying time is 24 h).
Step 5, placing the dried composite powder obtained in the step 4 into a stainless steel mold, and performing high-pressure compaction (the pressure is 500MPa, and the pressure maintaining time is 10-30min) by using a four-column hydraulic press to obtain a compact composite block blank;
step 6, putting the compact composite block blank obtained in the step 5 into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 100MPa, the temperature is 300 ℃, and the pressure maintaining time is 1 hour), so as to obtain a high-density hot-pressing composite block material;
and 7, carrying out hot extrusion on the block composite material obtained in the step 6 at a high extrusion ratio (the extrusion temperature is 300 ℃, the extrusion ratio is 25: 1, and the extrusion rate is 0.05mm/s), and finally obtaining the magnesium alloy composite material bar.
The primary micro-nano/nano TiC finally obtained by the embodimentp(5%) and Ti50Zr15Cu15Ni5V5Be10Machining an amorphous alloy (25%) co-reinforced magnesium alloy composite bar to obtain a standard tensile test sample, and then performing a tensile test on a universal mechanical testing machine, wherein the test result is as follows (see fig. 2): the yield strength of the composite material is 514MPa, the maximum tensile strength is 546MPa, and the maximum elongation is 6.2%.
Example 2:
a method for preparing a native micro/nano-scale titanium carbide and aluminum-based amorphous alloy co-reinforced magnesium alloy composite material comprises the following steps:
step 1, weighing 8g of titanium powder and 2g of graphite powder, putting the titanium powder and the graphite powder into a 250ml ball milling tank, and then putting 100g of ball milling steel balls. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9 vol.%) into the ball milling tank from an air inlet at one end, putting the ball milling tank into a ball mill, wherein the ball milling time is 60 hours, and the rotating speed of the ball mill is 500rpm, so that the micro/nano TiC is obtainedpAnd (3) granular powder.
Step 2, according to Al65Cu20Ti10Y5The molar ratio of elements in the molecular formula of the alloy compound is that aluminum, copper powder, titanium powder and yttrium powder (the total mass of the powder is 15g) are weighed and put into a 500ml ball milling tank, and then 300g ball milling steel balls are put into the ball milling tank. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9 vol.%) into the ball milling tank from an air inlet at one end, putting the ball milling tank into a ball mill, wherein the ball milling time is 80 hours, and the rotating speed of the ball mill is 500rpm, so that Al is obtained65Cu20Ti10Y5Amorphous alloy particle powder.
Step 3, then TiC obtained in the step 1pAdding granular powder (2g) to the Al obtained in step 265Cu20Ti10Y5Ball milling is continuously carried out on the amorphous alloy particle powder (the ball milling time is 20 hours, and the rotating speed of the ball mill is 500rpm), and then TiC is obtainedpParticles and Al65Cu20Ti10Y5Mixed powder of amorphous alloy particles.
Step 4, taking out the mixed powder obtained in the step 3, weighing 83g of AZ91 magnesium alloy powder, putting the powder into a 500ml beaker, adding 200ml of alcohol into the beaker, and then carrying out ultrasonic-assisted mechanical stirring (the ultrasonic power is 100Hz, the blade rotation speed is 600rpm, and the stirring time is 60 min); after stirring, putting the uniformly mixed slurry into a vacuum drying oven for drying (the vacuum degree is 50Pa, the drying temperature is 80 ℃, and the drying time is 24 h).
Step 5, placing the dried composite powder obtained in the step 4 into a stainless steel mold, and performing high-pressure compaction (the pressure is 500MPa, and the pressure maintaining time is 10-30min) by using a four-column hydraulic press to obtain a compact composite block blank;
step 6, putting the compact composite block blank obtained in the step 5 into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 100MPa, the temperature is 300 ℃, and the pressure maintaining time is 1 hour), so as to obtain a high-density hot-pressing composite block material;
and 7, carrying out hot extrusion on the block composite material obtained in the step 6 at a high extrusion ratio (the extrusion temperature is 300 ℃, the extrusion ratio is 25: 1, and the extrusion rate is 0.1mm/s), and finally obtaining the magnesium alloy composite material bar.
The primary micro-nano/nano TiC finally obtained by the embodimentp(2%) and Al65Cu20Ti10Y5The amorphous alloy (15%) co-reinforced magnesium alloy composite material bar is machined to obtain a standard tensile test sample, and then a tensile test is carried out on a universal mechanical testing machine, wherein the test result is as follows (see figure 2): the yield strength of the composite material is 416MPa, the maximum tensile strength is 448MPa, and the maximum elongation is 6.7%.
Example 3:
a method for preparing a primary micro/nano titanium carbide and magnesium-based amorphous alloy co-reinforced magnesium alloy composite material comprises the following steps:
step 1, weighing 8g of titanium powder and 2g of graphite powder, putting the titanium powder and the graphite powder into a 250ml ball milling tank, and then putting 100g of ball milling steel balls. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9 vol.%) into the ball milling tank from an air inlet at one end, putting the ball milling tank into a ball mill, wherein the ball milling time is 60 hours, and the rotating speed of the ball mill is 500rpm, so that the micro/nano TiC is obtainedpAnd (3) granular powder.
And 2, weighing 7.30g of magnesium powder and 17.70g of nickel powder, putting into a 500ml ball milling tank, and then putting into 250g of ball milling steel balls. Vacuumizing a ball milling tank, introducing argon (with the purity of 99.9 vol.%) into the ball milling tank from an air inlet at one end, filling the ball milling tank into a ball mill, wherein the ball milling time is 80 hours, and the rotating speed of the ball mill is 500rpm, so that Mg is obtained50Ni50Amorphous alloy particle powder.
Step 3, weighing the TiC obtained in the step 1p0.25g of granular powder, and weighing the Mg obtained in the step 250Ni5010g of amorphous alloy particle powder, namely 89.75g of AZ91 magnesium alloy powder, putting the three powder into a 500ml beaker, adding 200ml of alcohol into the beaker, and then carrying out ultrasonic-assisted mechanical stirring (the ultrasonic power is 100Hz, the blade rotation speed is 600rpm, and the stirring time is 60 min); after stirring, putting the uniformly mixed slurry into a vacuum drying oven for drying (the vacuum degree is 50Pa, the drying temperature is 80 ℃, and the drying time is 24 h).
Step 5, placing the dried composite powder obtained in the step 4 into a stainless steel mold, and performing high-pressure compaction (the pressure is 500MPa, and the pressure maintaining time is 10-30min) by using a four-column hydraulic press to obtain a compact composite block blank;
step 6, putting the compact composite block blank obtained in the step 5 into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 100MPa, the temperature is 300 ℃, and the pressure maintaining time is 1 hour), so as to obtain a high-density hot-pressing composite block material;
and 7, carrying out hot extrusion on the block composite material obtained in the step 6 at a high extrusion ratio (the extrusion temperature is 300 ℃, the extrusion ratio is 25: 1, and the extrusion rate is 0.15mm/s), and finally obtaining the magnesium alloy composite material bar.
The primary micro-nano/nano TiC finally obtained by the embodimentp(0.25%) and Mg50Ni50The amorphous alloy (10%) co-reinforced magnesium alloy composite material bar is machined to obtain a standard tensile test sample, and then a tensile test is carried out on a universal mechanical testing machine, wherein the test result is as follows (see figure 2): the yield strength of the composite material is 338MPa, the maximum tensile strength is 418MPa, and the maximum elongation is 9.6%.

Claims (5)

1. A method for preparing a native micro/nano-scale titanium carbide and amorphous alloy co-reinforced magnesium alloy composite material is characterized by comprising the following steps:
step 1, mixing titanium powder and graphite powder in proportion, and performing high-energy ball milling for a period of time to obtain native titanium carbide TiC with high activity and high specific surface areapGranular powder;
step 2, mixing light metal magnesium powder or aluminum powder or titanium powder with other alloy elements according to a certain proportion, and performing high-energy ball milling for a period of time to obtain magnesium-based or aluminum-based or titanium-based amorphous alloy particle powder with high activity and high crystallization temperature;
step 3, TiC obtained in the step 1pAdding the particle powder into the amorphous alloy particle powder obtained in the step 2 according to a certain proportion, and performing high-energy ball milling to obtain TiCpAnd amorphous alloy mixed powder;
step 4, TiC obtained in step 3pAdding the amorphous alloy mixed powder into magnesium alloy powder according to a certain proportion, adding a certain amount of alcohol, mechanically stirring in an ultrasonic-assisted mode to obtain uniformly mixed slurry, then putting the slurry into a vacuum oven for drying, and then obtaining composite powder;
step 5, placing the composite powder obtained in the step 4 in a mould, and performing high-pressure compaction by using a cold isostatic press or a four-column hydraulic press to obtain a compact composite block blank;
step 6, placing the compact composite block blank obtained in the step 5 into a vacuum hot-pressing sintering furnace for low-temperature hot-pressing sintering to obtain a high-density hot-pressing composite block;
step 7, carrying out hot extrusion on the block composite material obtained in the step 6 at a high extrusion ratio to finally obtain the high-strength and high-toughness native micro/nano-scale titanium carbide and amorphous alloy co-reinforced magnesium alloy composite material;
step 8, carrying out heat treatment on the magnesium alloy composite material obtained in the step 7;
in the step 1, the molar ratio of the titanium powder to the graphite powder is 1: 1, and the native TiC with high activity and high specific surface area is obtained after high-energy ball milling for a period of timepAccording to the difference of ball milling energy and ball milling time and the difference of in-situ reaction degree, obtaining particle powder with p in the range of 0.85-1, wherein the ball milling time is 40-80 h, the ball-material ratio is 10: 1-20: 1, and the rotating speed is 300 ion 600 r/min; in the step 2, light metal magnesium powder or aluminum powder or titanium powder and one or more of other alloying elements Cu, Ni, Si, Y, Fe, Ca, Zn, Nd and B are mixed according to a certain proportion, and the mixture is subjected to high-energy ball milling to obtain magnesium-based or aluminum-based or titanium-based amorphous alloy particle powder, wherein the breaking strength of the magnesium-based or aluminum-based or titanium-based amorphous alloy particle powder is required to be not less than 800MPa, and the magnesium-based or aluminum-based or titanium-based amorphous alloy particleThe temperature is not lower than 350 ℃, the ball milling time is 40-100 h, the ball material ratio is 10: 1-50: 1, and the rotating speed is 300-;
in the step 3, TiCpThe mixing ratio of the particles to the amorphous alloy particles is 1: 6-1: 20, and TiC is obtained after high-energy ball millingpBall milling time of mixed powder of particles and amorphous alloy particles is 20-40 h, ball-material ratio is 10: 1-20: 1, and rotating speed is 300-;
in the step 4, TiC added into the magnesium alloy powderpThe particles and the amorphous alloy particles respectively account for 0.25-5% and 5-30% of the total mass of the mixed powder, and the balance is magnesium alloy powder; the adding amount of the alcohol is only required to ensure that the slurry has enough fluidity during stirring; the ultrasonic power is 100-200 Hz, the rotating speed of blades is 300-1000 rpm, and the stirring time is 30-60 min;
in the step 6, in order to prevent the crystal grains of the magnesium alloy matrix material from growing up in the sintering process, the vacuum hot pressing process adopts low-temperature sintering, the sintering temperature range is 300-350 ℃, the pressure is 50-100 MPa, and the pressure maintaining time is 20min-1 h;
in the step 7, the temperature of hot extrusion is 280-300 ℃, the extrusion ratio is 25: 1, and the extrusion rate is 0.05-0.2 mm/s.
2. The method of claim 1, wherein: in the step 4, the magnesium alloy powder is one of Mg-Al series, Mg-Zn series, Mg-Mn series and Mg-RE series.
3. The method of claim 1, wherein: and in the step 4, the slurry which is uniformly stirred and mixed is dried in vacuum, the vacuum degree is less than 100Pa, the drying temperature is 80 ℃, and the drying time is 24 hours.
4. The method of claim 1, wherein: in the step 5, the used mold is a stainless steel mold, the pressure of the cold isostatic pressing or the four-column hydraulic pressure is 300-600MPa, and the pressure maintaining time is 10-30 min.
5. The method of claim 1, wherein: in the step 8, the prepared magnesium alloy composite material is subjected to appropriate heat treatment, that is, some common magnesium alloy heat treatment methods are adopted: t1-partial solution treatment and natural aging; t2-post-casting annealing; t3-solid solution + cold working; t4-solution treatment; t5-artificial aging; t6-solution treatment and artificial aging; t7-solution treatment and stabilization treatment; t8-solution treatment, cold working and artificial aging.
CN201811091941.5A 2018-09-19 2018-09-19 Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material Expired - Fee Related CN109439984B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811091941.5A CN109439984B (en) 2018-09-19 2018-09-19 Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811091941.5A CN109439984B (en) 2018-09-19 2018-09-19 Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material

Publications (2)

Publication Number Publication Date
CN109439984A CN109439984A (en) 2019-03-08
CN109439984B true CN109439984B (en) 2021-02-12

Family

ID=65533015

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811091941.5A Expired - Fee Related CN109439984B (en) 2018-09-19 2018-09-19 Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material

Country Status (1)

Country Link
CN (1) CN109439984B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110578071B (en) * 2019-08-27 2021-05-25 江苏大学 Heat treatment method for improving hardness of high-temperature titanium alloy-based composite material
CN110791677A (en) * 2019-11-18 2020-02-14 中国科学院上海硅酸盐研究所 High-performance wear-resistant bronze-based composite material and preparation method and application thereof
CN111270101B (en) * 2020-03-25 2021-04-23 西安稀有金属材料研究院有限公司 Microalloying cooperative strengthening graphene titanium-based composite material and preparation method thereof
CN111266592B (en) * 2020-03-25 2022-04-22 燕山大学 Titanium-magnesium composite material with double-communication structure and preparation method and application thereof
CN113005317A (en) * 2021-02-24 2021-06-22 山东省科学院新材料研究所 High-thermal-stability magnesium alloy with mixed crystal structure and controllable preparation method and application
CN114309622B (en) * 2021-11-18 2023-04-14 宁波中乌新材料产业技术研究院有限公司 Preparation method of aluminum alloy powder for multiphase composite additive manufacturing
CN115287513B (en) * 2022-08-06 2023-12-08 陕西天梵镁汇科技有限公司 Red copper particle reinforced magnesium-based composite material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101368242A (en) * 2008-10-16 2009-02-18 上海市机械制造工艺研究所有限公司 Amorphous particle reinforced magnesium-base composite material and manufacture process
CN102061421A (en) * 2011-01-31 2011-05-18 江苏大学 In-situ submicron/nanometer particle-reinforced magnesium-matrix composite material and preparation method thereof
DE112004001910B4 (en) * 2003-10-08 2011-07-21 Miba Gleitlager Gmbh Overlay

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE112004001910B4 (en) * 2003-10-08 2011-07-21 Miba Gleitlager Gmbh Overlay
CN101368242A (en) * 2008-10-16 2009-02-18 上海市机械制造工艺研究所有限公司 Amorphous particle reinforced magnesium-base composite material and manufacture process
CN102061421A (en) * 2011-01-31 2011-05-18 江苏大学 In-situ submicron/nanometer particle-reinforced magnesium-matrix composite material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Interfacial structure in AZ91 alloy composites reinforced by graphene nanosheets";Qiu-hongYuan等;《Carbon》;20180228;第127卷;第177-186页 *

Also Published As

Publication number Publication date
CN109439984A (en) 2019-03-08

Similar Documents

Publication Publication Date Title
CN109439984B (en) Preparation method of primary titanium carbide and amorphous phase co-reinforced magnesium-based composite material
Chak et al. A review on fabrication methods, reinforcements and mechanical properties of aluminum matrix composites
CN109207763B (en) Graphene and light metal-based amorphous alloy particle co-reinforced magnesium alloy composite material and preparation method thereof
Yan et al. Microstructure and mechanical properties of in-situ synthesized TiB whiskers reinforced titanium matrix composites by high-velocity compaction
Qu et al. In situ synthesis of a gamma-Al2O3 whisker reinforced aluminium matrix composite by cold pressing and sintering
CN108342667B (en) Titanium boride nano whisker reinforced titanium-based composite material and preparation method thereof
CN113373335B (en) Preparation method of high-strength titanium-based composite material
CN110205536B (en) Titanium/titanium carbide core-shell structure reinforced aluminum-based composite material and preparation method thereof
CN111485129B (en) TiC/Ti5Si3 reinforced copper-based composite material and preparation method thereof
Ghazanlou et al. Fabrication and characterization of GNPs and CNTs reinforced Al7075 matrix composites through the stir casting process
Eacherath et al. Synthesis and characterization of magnesium-based hybrid composites–A review
Zhang et al. Structure and mechanical properties of in-situ titanium matrix composites with homogeneous Ti5Si3 equiaxial particle-reinforcements
Patel et al. Effect of ultrasonic stirring on changes in microstructure and mechanical properties of cast insitu Al 5083 alloy composites containing 5wt.% and 10wt.% TiC particles
Ren et al. Fabrication and mechanical properties of Ti2AlC/TiAl composites with co-continuous network structure
CN114318039B (en) Element alloying preparation method of metal matrix composite material with three-peak grain structure
CN109439983B (en) Native micro/nano vanadium carbide and light metal-based amorphous alloy co-reinforced magnesium alloy composite material and preparation method thereof
CN114411031A (en) Micron titanium particle reinforced magnesium rare earth based composite material
CN113798494A (en) TiB2Particle reinforced magnesium-based composite material and preparation method thereof
CN102021473A (en) Method for preparing Fe3Al-Al2O3 composite material
CN112226639A (en) In-situ ultrafine grain TiC reinforced titanium-based composite material based on cyclohexene ball milling medium and preparation method thereof
CN109439985B (en) Magnesium-based composite material with special three-phase coexisting structure and preparation method thereof
CN110541083A (en) Preparation method for in-situ synthesis of nano MgO reinforced aluminum alloy base composite material
CN109161751B (en) High-strength high-toughness native tantalum carbide and amorphous alloy co-reinforced magnesium-based composite material and preparation method thereof
Çanakçı Production and microstructure of AA2024–B4C metal matrix composites by mechanical alloying method
CN112481516B (en) Al-Ti-SiC intermediate alloy and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20210212

Termination date: 20210919

CF01 Termination of patent right due to non-payment of annual fee