CN106756352A - Raw Cr in a kind of2B and MgO diphase particles strengthen the preparation method of magnesium base composite material - Google Patents
Raw Cr in a kind of2B and MgO diphase particles strengthen the preparation method of magnesium base composite material Download PDFInfo
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- CN106756352A CN106756352A CN201611025666.8A CN201611025666A CN106756352A CN 106756352 A CN106756352 A CN 106756352A CN 201611025666 A CN201611025666 A CN 201611025666A CN 106756352 A CN106756352 A CN 106756352A
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000011777 magnesium Substances 0.000 title claims abstract description 86
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 83
- 239000002245 particle Substances 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 62
- 239000011812 mixed powder Substances 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 238000013329 compounding Methods 0.000 claims abstract description 34
- 230000004907 flux Effects 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000007670 refining Methods 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 15
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000007872 degassing Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 230000002708 enhancing effect Effects 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 7
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000011156 metal matrix composite Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 235000001055 magnesium Nutrition 0.000 description 67
- 235000019580 granularity Nutrition 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 surface no-pollution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
- C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention discloses raw Cr in a kind of2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, belong to field of metal matrix composite, using B2O3Powder, Cr2O3Powder is raw material, and well mixed, drying, compacting obtain mixed-powder base, and mixed-powder base is dividedly in some parts into CO2Interior raw reaction is carried out in magnesium or magnesium alloy fused mass under gas shield, is stirred while reaction, after interior raw reaction terminates, add C2Cl6And MgCO3Admixture refining agent carry out degasification, deslagging refining；Mold will be poured into after compounding flux standing, removing surface residual debris, obtain interior raw Cr2B and MgO diphase particles strengthen magnesium base composite material；Magnesium base composite material involved in the present invention, the Cr with interior life2B and MgO particles are good with the interface compatibility of matrix, and enhancing particle size is controllable, and enhancing distributed mutually is uniform, and the features such as Gao Biqiang, high elastic modulus, process is simple is adapted to large-scale production.
Description
Technical field
The present invention relates to raw Cr in one kind2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, belong to gold
Metal-matrix composite material technical field.
Background technology
The density of magnesium is 1.8g/cm3, it is most light nonferrous materials, magnesium and magnesium alloy have high specific strength, Gao Bigang
The characteristic such as degree, preferable electrical and thermal conductivity, good damping shock absorption and capability of electromagnetic shielding, shaping easy to process, in space flight boat
The fields such as sky, automobile, electronics, communication are widely used.But intensity and the not high, high-temperature creep resistance of rigidity due to magnesium alloy
The shortcomings of and wearing no resistance, limits its range of application.In order to improve the performance of magnesium alloy, expand the application of magnesium alloy, draw
Enter particulates reinforcements to carry out complex intensifying to magnesium alloy is an important developing direction.
The preparation method of current magnesium base composite material mainly has two kinds, and one is the method for additional particle, such as stirring casting, pressure
Power infusion process, powder metallurgic method etc., these production technologies have additional enhancing, and grain graininess is larger, particle is combined with basal body interface
The deficiency such as bad, particle agglomeration, composite materials property be poor；Two is interior life（Fabricated in situ）Particle preparation magnesium-based composite wood
The method of material, the composite of preparation has tiny enhancing particle, surface no-pollution, particle and matrix is compatible, material is comprehensive
Can be good the features such as.The present invention is a kind of interior raw Cr2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, Cr2B
Have the advantages that high intensity, high rigidity, high elastic modulus, low thermal coefficient of expansion, high-melting-point and heat endurance are good with MgO particles,
The Cr of interior life in magnesium or magnesium alloy2B and MgO particle dispersions are distributed in magnesium matrix, Cr2B and MgO particles are tiny and be evenly distributed,
Clean surface and matrix are well combined without interfacial reaction, and obtained magnesium base composite material has lightweight, high-strength, high elastic modulus
The features such as, process is simple is adapted to large-scale production.
The content of the invention
It is an object of the invention to provide raw Cr in one kind2B and MgO diphase particles strengthen the preparation side of magnesium base composite material
Method, preparation method process is simple, the low cost, endogenetic particle content and size are controllable, and particle is tiny and Dispersed precipitate is in melt
In, it is clean not generate accessory substance, melt in course of reaction, and obtained composite has lightweight, high-strength, high elastic modulus and good
Good resistance to elevated temperatures and anti-wear performance.
The technical scheme is that：By B2O3Powder, Cr2O3Powder is well mixed, dry, compacting obtains mixed-powder
Base, mixed-powder base is added in CO in batches2In magnesium or magnesium alloy fused mass under gas shield, while being stirred；It is interior
After raw reaction terminates, add refining agent to carry out degasification, deslagging refining, casting will be poured into after compounding flux standing, removing surface residual debris
Mould, obtains interior raw Cr2B and MgO diphase particles strengthen magnesium base composite material, comprise the following steps that：
（1）It is prepared by mixed-powder：According to B2O3Powder and Cr2O3The mol ratio of powder is 1:2 ratio, by B2O3Powder and
Cr2O3Powder batch mixing 1~4 hour in batch mixer, then dries 2~4 hours in drying box at a temperature of 200~250 DEG C
Obtain mixed-powder；
（2）Mixed-powder pressed compact：By step（1）The mixed-powder of acquisition is pressed with forcing press under the pressure of 50~400MPa
Mixed-powder base is obtained；
（3）Magnesium or magnesium alloy melting and heat preservation：By magnesium or magnesium alloy in CO2750~850 DEG C are heated under gas shield to melt and protect
10~30min of temperature, obtains magnesium or magnesium alloy fused mass；
（4）By step（2）The mixed-powder base of acquisition is added in CO in batches2Step under gas shield（3）Magnesium or magnesium close
In golden melt, the temperature of reaction is controlled for 750~850 DEG C, while being stirred with the mixing speed of 100~500r/min, carry out interior
Raw reaction, 70~90min of stirring reaction obtains containing Cr after slagging-off2The compounding flux of B and MgO diphase particles；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained is smart to being added in melt at 700~740 DEG C
Refining agent, addition is the 0.2~1.0% of compounding flux quality, and 5~15min of stirring carries out degasification, deslagging refining, is refined
Compounding flux；
（6）Casting forming：By step（5）In the compounding flux that obtains stand 5~20min at 700~740 DEG C, after removing residue
It is cast in 200~400 DEG C of molds of preheating, obtains interior raw Cr2B and MgO biphase ceramic granules strengthen magnesium base composite material.
Step（1）The B2O3Powder and Cr2O3The granularity of powder is 100~400 mesh.
Step（3）Described in magnesium or magnesium alloy be one kind in pure magnesium, cast magnesium alloy or wrought magnesium alloy.
Step（4）The mixed-powder addition accounts for the 3.4%~17.16% of magnesium or quality of magnesium alloy.
Step（4）Described in mixed-powder base be equally divided into five batches and be added in magnesium or magnesium alloy fused mass, it is each between
It is 5~15min every the time.
Step（5）Described in refining agent be C2Cl6And MgCO3Mixture, wherein C2Cl6And MgCO3Mass ratio be 4 ︰
6。
The interior raw Cr that the present invention is obtained2In B and MgO biphase ceramic granules enhancing magnesium base composite material, Cr2B and MgO two-phases
The size of particle is 90~245nm, Cr2B granular mass percentage compositions are that the weight/mass percentage composition of 2~9%, MgO particles is 3.14
~14.13%.
Inventive principle
（1）Cr2The interior raw reaction principle of B and MgO particles
In CO2Under gas shield, by B2O3With Cr2O3Mixing base be added in 750~850 DEG C of magnesium or magnesium alloy fused mass,
B2O3MgO particles, activity [B] atom are obtained with fusant reaction, while active [B] atom and Cr2O3Reaction obtains B2O3And Cr2B
Particle, Cr2The interior raw course of reaction of B and MgO particles is as follows：
Combined reaction is：（3）
Can be obtained according to thermodynamics handbook（1）~（3）Three reaction Gibbs free energys and temperature between relation be：
When temperature is at 750~850 DEG C,（4）~（6）FormulaRespectively less than 0, illustrate that reaction can be what is carried out.
（2）Cr in composite2B and content of MgO control principle
Pass through（3）Formula can respectively set up the magnesium of reaction consumption or the quality of magnesium alloy, add the quality of mixed-powder base, answered
The gross mass of condensation material and interior life (Cr2B+MgO) the mass fraction of particle（）Between
Relational expression：
（7）
（7）In formula：
When the magnesium or the quality of magnesium alloy for weighing are n (quality c, n ＞ c comprising reaction consumption magnesium), add mixed-powder base
Quality is M（y+z）When, the matter of the quality n+addition mixed-powder base of the gross mass m of composite=weigh magnesium or magnesium alloy
Amount M, i.e.,：
SoObtain：
（8）
If adding mixing base quality to account for weighs the percentage of magnesium or quality of magnesium alloy for a, then:
（9）
Because 5.14wt.%≤x≤23.13wt.%, therefore 3.4%≤a≤17.16%；
Consider that the burn out rate in melting and course of reaction is 8%, therefore the quality for actually weighing magnesium or magnesium alloy is：
（10）
（3）Interior raw Cr2The control principle of B, MgO particle mean size R
In the present invention, the Cr of interior life2The average-size of B and MgO particles is controllable, is melted in mixed-powder base and magnesium or magnesium alloy
On the premise of body fully reacts, interior raw Cr2The average-size R of B, MgO particle be mainly by addition mixed-powder base mass M,
Reaction temperature T, reaction time t and mixing speed V are controlled.
The addition of M is mainly and have impact on the viscosity size of melt so as to influence the average-size of endogenetic particle；T is mainly
Influence reacts severe degree and particle growth speed so as to influence the average-size of endogenetic particle；T is that influence endogenetic particle is grown up
Factor；The speed of V have impact on the degree of crushing of matrix dendrite and break up the degree of endogenetic particle reunion so as to influence interior life
The average-size of grain, the average-size of endogenetic particle reduces with reaction temperature increase, mixing speed, adds mixed-powder base quality
Increase and the reaction time extends and increases, its correlation is：
(11)
（11）In formula：
Beneficial effects of the present invention
（1）Two-phase is prepared using interior raw reaction method（Cr2B、MgO）Particle reinforced magnesium base compound material, overcome outer addition
The problems such as grain is poor with matrix wetability, interfacial reaction hardly possible is controlled.
（2）Cr2The content of B and MgO particulates reinforcements, size are controllable, are evenly distributed in the base, are combined with matrix good
Good, interfacial cleanliness；The Cr of interior life2B and MgO particles are remarkably improved intensity, hardness, elastic modelling quantity and the height of magnesium base composite material
Warm mechanical property.
Brief description of the drawings
Fig. 1 is the process chart of the embodiment of the present invention 1.
Specific embodiment
Embodiment 1
A kind of interior raw Cr described in the present embodiment2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, specific steps
It is as follows：
（1）It is prepared by mixed-powder：Weigh the B of the mesh of 30g granularities 100~1502O3Powder and the mesh Cr of 131g granularities 100~1502O3Powder
End, wherein B are 1 with Cr mol ratios:2, then batch mixing 1 hour in batch mixer dries 2 in drying box with 200 DEG C of temperature
Hour, obtain mixed-powder；
（2）The pressed compact of mixed-powder：By step（1）The mixed-powder of acquisition is suppressed with forcing press under the pressure of 50MPa
Obtain mixed-powder base；
（3）The melting of magnesium alloy：5114.4g ZM1 magnesium alloys are weighed, the weight/mass percentage composition of magnesium is 94.5%, root in the alloy
It is 93.07g according to the amount of magnesium needed for raw reaction in calculating, in CO2Under gas shield, the ZM1 magnesium alloys that will be weighed are heated to 750
DEG C melt and be incubated 10min, obtain ZM1 magnesium alloy fused mass；
（4）Interior raw Cr2B and MgO diphase particles：The 3.4% of quality of magnesium alloy ratio is accounted for according to mixed-powder, step is taken（2）Obtain
Mixed-powder base and be equally divided into 5 times, be once added to step every 5min（3）ZM1 magnesium alloy fused mass in carry out in
The reaction of raw particle, reaction temperature is 750 DEG C, stirs 70min with the mixing speed of 100r/min during the course of the reaction, and interior life is anti-
Should carry out, magnesium alloy fused mass temperature has been maintained at 700 DEG C, obtained with Cr after slagging-off2The compounding flux of B and MgO particles；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained at 700 DEG C, to adding C in melt2Cl6With
MgCO3Admixture refining agent, addition for compounding flux quality 0.2%, C in admixture refining agent2Cl6And MgCO3Mass ratio
It is 4 ︰ 6, and degasification, deslagging refining is carried out with graphite rod stirring 5min, the compounding flux for being refined；
（6）The casting forming of magnesium base composite material：By step（5）In compounding flux 700 DEG C stand 5min after be poured into 200
DEG C preheating mold in, obtain gross mass be 4943.16g interior raw Cr2B and MgO biphase ceramic granules strengthen magnesium-based composite wood
Material, wherein Cr2The mass fraction of B particles is 3.14%, Cr for the mass fraction of 2%, MgO particles2The average-size of B and MgO particles
It is 105nm.
Embodiment 2
A kind of interior raw Cr described in the present embodiment2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, specific steps
It is as follows：
（1）It is prepared by mixed-powder：Weigh the B that 70g granularities are 150~200 mesh2O3Powder and 306g granularities are 150~200 purposes
Cr2O3Powder, wherein B are 1 with Cr mol ratios:2, batch mixing 2 hours in batch mixer, then 220 DEG C of dryings 2.5 in drying box
Hour, obtain mixed-powder；
（2）The pressed compact of mixed-powder：By step（1）The mixed-powder of acquisition is suppressed with forcing press under the pressure of 150MPa
Obtain mixed-powder base；
（3）The melting of magnesium alloy：5971.76g ZM5 magnesium alloys are weighed, the weight/mass percentage composition of magnesium is 91% in the alloy, according to
The amount of raw reaction consumption magnesium is 217.4g in calculating, in CO2Under gas shield, the ZM5 magnesium alloys that will be weighed are heated to 780 DEG C
20min is melted and be incubated, ZM5 magnesium alloy fused mass is obtained；
（4）Interior raw Cr2B and MgO diphase particles：Weigh quality of magnesium alloy 6.8% ratio is accounted for according to mixed-powder, step is taken
（2）The mixed-powder base of acquisition is simultaneously equally divided into 5 times, is once added to step every 12min（3）ZM5 magnesium alloy fused mass in
The reaction of endogenetic particle is carried out, reaction temperature is 780 DEG C, stirs 75min with the mixing speed of 200r/min during the course of the reaction,
Interior raw reaction has been carried out, and magnesium alloy fused mass temperature is maintained at into 720 DEG C, is obtained with Cr after slagging-off2B and MgO particles it is compound
Melt；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained at 720 DEG C, to adding C in melt2Cl6With
MgCO3Admixture refining agent, addition for compounding flux quality 0.5%, C in admixture refining agent2Cl6And MgCO3Mass ratio
It is 4 ︰ 6, and degasification, deslagging refining is carried out with graphite rod stirring 8min, the compounding flux for being refined；
（6）The casting forming of magnesium base composite material：By step（5）In compounding flux 720 DEG C stand 10min after be poured into
In 270 DEG C of molds of preheating, the interior raw Cr that gross mass is 5905.4g is obtained2B and MgO biphase ceramic granules enhancing magnesium-based is combined
Material, wherein Cr2The mass fraction of B particles is 6.1%, Cr for the mass fraction of 3.9%, MgO particles2B and MgO particles it is average
Size is 95nm.
Embodiment 3
A kind of interior raw Cr described in the present embodiment2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, specific steps
It is as follows：
（1）It is prepared by mixed-powder：Weigh the B that 144g granularities are 230~300 mesh2O3Powder and 629g granularities are 230~300 mesh
Cr2O3Powder, wherein B are 1 with Cr mol ratios:2, batch mixing 3 hours in batch mixer, then with 240 DEG C of temperature in drying box
Degree is dried 3 hours, obtains mixed-powder；
（2）The pressed compact of mixed-powder：By step（1）The mixed-powder of acquisition is suppressed with forcing press under the pressure of 300MPa
Obtain mixed-powder base；
（3）The melting of magnesium alloy：7387.9g ZM10 magnesium alloys are weighed, the weight/mass percentage composition of magnesium is 89% in the alloy, according to
The amount of raw reaction consumption magnesium is 446.8g in calculating, in CO2Under gas shield, the ZM10 magnesium alloys that will be weighed are heated to 800
DEG C melt and be incubated 25min, obtain ZM10 magnesium alloy fused mass；
（4）Interior raw Cr2B and MgO diphase particles：Claim quality of magnesium alloy 11.3% ratio is accounted for according to mixed-powder, step is taken
（2）The mixed-powder base of acquisition is simultaneously equally divided into 5 times, is added to step per septum secundum 13min（3）The ZM10 magnesium alloy fused mass of acquisition
In carry out the reaction of endogenetic particle, reaction temperature is 800 DEG C, is stirred with the mixing speed of 350r/min during the course of the reaction
80min, interior raw reaction has been carried out, and magnesium alloy fused mass temperature is maintained at into 730 DEG C, is obtained with Cr after slagging-off2B and MgO particles
Compounding flux；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained at 730 DEG C, to adding C in melt2Cl6With
MgCO3Admixture refining agent, addition for compounding flux quality 0.7%, C in admixture refining agent2Cl6And MgCO3Mass ratio
It is 4 ︰ 6, and degasification, deslagging refining is carried out with graphite rod stirring 11min, the compounding flux for being refined；
（6）The casting forming of magnesium base composite material：By step（5）In compounding flux 730 DEG C stand 15min after be poured into
In 340 DEG C of molds of preheating, the interior raw Cr that gross mass is 7613.7g is obtained2B and MgO biphase ceramic granules enhancing magnesium-based is combined
Material, wherein Cr2The mass fraction of B particles is 9.8%, Cr for the mass fraction of 6.2%, MgO particles2B and MgO particles it is average
Size is 90nm.
Embodiment 4
A kind of interior raw Cr described in the present embodiment2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, specific steps
It is as follows：
（1）It is prepared by mixed-powder：Weigh the B that 300g granularities are 300~400 mesh2O3Powder and 1309g granularities are 300~400 mesh
Cr2O3Powder, wherein B are 1 with Cr mol ratios:2, batch mixing 4 hours in batch mixer, then with 250 DEG C of temperature in drying box
Degree is dried 4 hours, obtains mixed-powder；
（2）The pressed compact of mixed-powder：By step（1）The mixed-powder of acquisition is suppressed with forcing press under the pressure of 400MPa
Obtain mixed-powder base；
（3）The melting of magnesium alloy：10126.58g AZ61M magnesium alloys are weighed, the weight/mass percentage composition of magnesium is 98% in the alloy,
Amount according to raw reaction consumption magnesium in calculating is 930.21g, in CO2Under gas shield, the AZ61M magnesium alloys heating that will be weighed
Melted to 850 DEG C and be incubated 30min, obtain AZ61M magnesium alloy fused mass；
（4）Interior raw Cr2B and MgO diphase particles：The 17.16% of quality of magnesium alloy ratio is accounted for according to mixed-powder, step is taken（2）
The mixed-powder base of acquisition is simultaneously equally divided into 5 times, is added to step per septum secundum 15min（3）In the AZ61M magnesium alloy fused mass of acquisition
The reaction of endogenetic particle is carried out, reaction temperature is 850 DEG C, stirs 90min with the mixing speed of 500r/min during the course of the reaction,
Interior raw reaction has been carried out, and magnesium alloy fused mass temperature is maintained at into 740 DEG C, is obtained with Cr after slagging-off2B and MgO particles it is compound
Melt；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained at 740 DEG C, to adding C in melt2Cl6With
MgCO3Admixture refining agent, addition for compounding flux quality 1.0%, C in admixture refining agent2Cl6And MgCO3Mass ratio
It is 4 ︰ 6, and degasification, deslagging refining is carried out with graphite rod stirring 15min, the compounding flux for being refined；
（6）The casting forming of magnesium base composite material：By step（3）In Composite Melt 740 DEG C stand 20min after pour into a mould
To in 400 DEG C of molds of preheating, the interior raw Cr that gross mass is 10985.46g is obtained2B and MgO biphase ceramic granules strengthen magnesium-based
Composite, wherein Cr2The mass fraction of B particles is 14.13%, Cr for the mass fraction of 9%, MgO particles2B and MgO particles
Average-size is 245nm.
Embodiment 5
A kind of interior raw Cr described in the present embodiment2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, specific steps
It is as follows：
（1）It is prepared by mixed-powder：Weigh the B that 50g granularities are 200~230 mesh2O3Powder and 218g granularities are 200~230 purposes
Cr2O3Powder, wherein B are 1 with Cr mol ratios:2, batch mixing 1.5 hours in batch mixer, then 210 DEG C of dryings in drying box
3.5 hours, obtain mixed-powder；
（2）The pressed compact of mixed-powder：By step（1）The mixed-powder of acquisition is suppressed with forcing press under the pressure of 100MPa
Obtain mixed-powder base；
（3）The melting of pure magnesium：5461.13g pure magnesiums are weighed, the purity of the pure magnesium is 99.8%, in calculating
The amount of raw reaction consumption magnesium is 155g, in CO2Under gas shield, the pure magnesium that will be weighed is heated to 770 DEG C and melts and protect
Warm 15min, obtains pure magnesium melt；
（4）Interior raw Cr2B and MgO diphase particles：Weigh pure magnesium quality 5.3% ratio is accounted for according to mixed-powder, step is taken
Suddenly（2）The mixed-powder base of acquisition is simultaneously equally divided into 5 times, is once added to step every 11min（3）The pure magnesium of acquisition melts
The reaction of endogenetic particle is carried out in body, reaction temperature is 770 DEG C, is stirred with the mixing speed of 150r/min during the course of the reaction
85min, interior raw reaction has been carried out, and pure magnesium melt temperature is maintained at into 710 DEG C, is obtained with Cr after slagging-off2B and MgO
The compounding flux of grain；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained at 710 DEG C, to adding C in melt2Cl6With
MgCO3Admixture refining agent, addition for compounding flux quality 0.3%, C in admixture refining agent2Cl6And MgCO3Mass ratio
It is 4 ︰ 6, and degasification, deslagging refining is carried out with graphite rod stirring 8min, the compounding flux for being refined；
（6）The casting forming of magnesium base composite material：By step（5）In compounding flux 710 DEG C stand 8min after be poured into 240
DEG C preheating mold in, obtain gross mass be 5324.6g interior raw Cr2B and MgO biphase ceramic granules strengthen magnesium-based composite wood
Material, wherein Cr2The mass fraction of B particles is 4.9%, Cr for the mass fraction of 3.1%, MgO particles2The average chi of B and MgO particles
Very little is 154nm.
Specific embodiment of the invention is explained in detail above in association with accompanying drawing, but the present invention be not limited to it is above-mentioned
Implementation method, in the ken that those of ordinary skill in the art possess, can also be before present inventive concept not be departed from
Put that various changes can be made.
Claims (6)
1. Cr is given birth in one kind2B and MgO diphase particles strengthen the preparation method of magnesium base composite material, it is characterised in that specific steps
Including：
（1）It is prepared by mixed-powder：According to B2O3Powder and Cr2O3The mol ratio of powder is 1:2 ratio, by B2O3Powder and Cr2O3
Powder batch mixing 1~4 hour, then drying obtains mixed-powder in 2~4 hours at a temperature of 200~250 DEG C；
（2）Mixed-powder pressed compact：By step（1）The mixed-powder of acquisition under the pressure of 50~400MPa suppress being mixed
Close powder base；
（3）Magnesium or magnesium alloy melting and heat preservation：By magnesium or magnesium alloy in CO2750~850 DEG C are heated under gas shield to melt and protect
10~30min of temperature, obtains magnesium or magnesium alloy fused mass；
（4）By step（2）The mixed-powder base of acquisition is added in CO in batches2Step under gas shield（3）Magnesium or magnesium alloy
In melt, controlling reaction temperature is 750~850 DEG C, while being stirred with the mixing speed of 100~500r/min, carries out interior life anti-
Should, 70~90min of stirring reaction obtains containing Cr after slagging-off2The compounding flux of B and MgO diphase particles；
（5）Melt is refined：By step（4）The temperature control of the compounding flux of gained is smart to being added in melt at 700~740 DEG C
Refining agent, addition is the 0.2~1.0% of compounding flux quality, and 5~15min of stirring carries out degasification, deslagging refining, is refined
Compounding flux；
（6）Casting forming：By step（5）In the compounding flux that obtains stand 5~20min at 700~740 DEG C, after removing residue
It is cast in 200~400 DEG C of molds of preheating, obtains interior raw Cr2B and MgO biphase ceramic granules strengthen magnesium base composite material.
2. interior raw Cr according to claim 12B and MgO diphase particles strengthen the preparation method of magnesium base composite material, its feature
It is, step（1）The B2O3Powder and Cr2O3The granularity of powder is 100~400 mesh.
3. interior raw Cr according to claim 12B and MgO diphase particles strengthen the preparation method of magnesium base composite material, its feature
It is, step（3）Described in magnesium or magnesium alloy be one kind in pure magnesium, cast magnesium alloy or wrought magnesium alloy.
4. interior raw Cr according to claim 12B and MgO diphase particles strengthen the preparation method of magnesium base composite material, its feature
It is, step（4）The mixed-powder addition accounts for the 3.4%~17.16% of magnesium or quality of magnesium alloy.
5. interior raw Cr according to claim 12B and MgO diphase particles strengthen the preparation method of magnesium base composite material, its feature
It is, step（4）Described in mixed-powder base be equally divided into five batches and be added in magnesium or magnesium alloy fused mass, during each interval
Between be 5~15min.
6. interior raw Cr according to claim 12B and MgO diphase particles strengthen the preparation method of magnesium base composite material, its feature
It is, step（5）Described in refining agent be C2Cl6And MgCO3Mixture, wherein C2Cl6And MgCO3Mass ratio be 4 ︰ 6.
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| CN108165793A (en) * | 2017-06-12 | 2018-06-15 | 吉林大学 | Raw nano-sized particles reinforced aluminium alloy material preparation method in one kind |
| CN113699404A (en) * | 2021-08-25 | 2021-11-26 | 苏州大学 | Composite salt for purifying aluminum waste and preparation and use methods thereof |
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| CN103045916A (en) * | 2012-12-26 | 2013-04-17 | 四川材料与工艺研究所 | Composite shielding material and preparation method thereof |
| CN105603279A (en) * | 2016-01-27 | 2016-05-25 | 国网山东省电力公司莱阳市供电公司 | Chromium diboride-enhanced magnesium alloy wire for cable and preparation method and application of magnesium alloy wire |
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| US6290748B1 (en) * | 1995-03-31 | 2001-09-18 | Merck Pateng Gmbh | TiB2 particulate ceramic reinforced Al-alloy metal-matrix composites |
| CN103014474A (en) * | 2012-12-18 | 2013-04-03 | 江苏新亚特钢锻造有限公司 | Oxide particle reinforced laser cladding nickel-base alloy powder and preparation method thereof |
| CN103045916A (en) * | 2012-12-26 | 2013-04-17 | 四川材料与工艺研究所 | Composite shielding material and preparation method thereof |
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| CN108165793A (en) * | 2017-06-12 | 2018-06-15 | 吉林大学 | Raw nano-sized particles reinforced aluminium alloy material preparation method in one kind |
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| CN113699404A (en) * | 2021-08-25 | 2021-11-26 | 苏州大学 | Composite salt for purifying aluminum waste and preparation and use methods thereof |
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