CN108467962A - A kind of preparation method of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites - Google Patents
A kind of preparation method of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites Download PDFInfo
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- CN108467962A CN108467962A CN201810328616.XA CN201810328616A CN108467962A CN 108467962 A CN108467962 A CN 108467962A CN 201810328616 A CN201810328616 A CN 201810328616A CN 108467962 A CN108467962 A CN 108467962A
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- C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0057—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
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Abstract
The present invention relates to the preparation methods of a kind of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites, the case where being for magnesium-based composite material poor mechanical property, using magnesium alloy as matrix, within raw quasi-crystalline substance magnesium zinc yttrium and boron carbide be hardening constituent, through frequency induction melting furnace melting in a vacuum, magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites is made in argon gas bottom blowing, mechanical agitation, extrusion casint and heat treatment;This preparation method technique is advanced, and process is tight, and data are accurately full and accurate, and the magnesium-based composite material tensile strength of preparation reaches 315MPa, and for elongation up to 7%, hardness reaches 108Hv, is the preparation method of advanced magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites.
Description
Technical field
The present invention relates to the preparation method of a kind of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites, category has
Non-ferrous metal material preparation and the technical field of application.
Background technology
Magnesium alloy materials have the characteristics that density is low, specific strength is high, good anti-vibration, electromagnetic shielding capability are strong and easy processing,
It is widely used to automobile and aerospace field;But magnesium alloy hardness is low, tensile strength is low and poor corrosion resistance, limits magnesium
Application of the alloy in industrial circle.
Quasi-crystalline substance has high rigidity, high elastic modulus, low-expansion coefficient and good corrosion resistance, is highly suitable as magnesium conjunction
The hardening constituent of gold, can effectively improve the mechanical property of magnesium alloy;Boron carbide particles have low density, good chemical stability and
Wearability, and can be evenly distributed in magnesium matrix, interface stability has prodigious application potential, hybrid particles reinforced type magnesium
Also in conceptual phase, technology need to be improved based composites.
Invention content
Goal of the invention
The purpose of the present invention is being directed to background technology, using magnesium alloy as matrix, within raw magnesium zinc yttrium quasi-crystalline substance and carbon
Change boron is reinforced phase, through the melting of frequency induction melting furnace, extrusion casint in a vacuum, magnesium zinc yttrium quasi-crystalline substance is made and boron carbide mixing increases
Strong type magnesium-based composite material, to improve the mechanical property of magnesium alloy.
Technical solution
The chemical substance material that the present invention uses is:Magnesium, zinc, magnesium yttrium intermediate alloy, boron carbide, zinc oxide, talcum powder, water
Glass, deionized water, aluminium foil, absolute ethyl alcohol, argon gas, it is as follows that a combination thereof prepares dosage:With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) casting die is prepared
Open-close type squeeze casting mould hot-work die steel making, mold cavity is rectangular, cavity dimension be 200mm ×
160mm × 90mm, mold cavity surface roughness are Ra0.08-0.16 μm;
(2) coating agent is configured
Zinc oxide 80g ± 1g, talcum powder 50g ± 1g, waterglass 25g ± 1g are weighed, deionized water 300mL ± 1mL is measured,
It is added in mixing hollander and is stirred, agitation revolution 50r/min, mixing time 80min is as applied at viscous liquid after stirring
Cover agent;
(3) boron carbide particles are pre-processed
1. ball milling weighs boron carbide 300g ± 0.1g, is placed in the ball grinder of ball mill, ball milling, rotational speed of ball-mill are carried out
80r/min, Ball-milling Time 3h, at fine powder, fine powder grain size≤9 μm after ball milling;
2. ultrasonic wave dispersion cleaning:Fine powder after ball milling is placed in beaker, absolute ethyl alcohol 500mL ± 1mL is then added,
Mixing;
Beaker is placed in ultrasonic wave separating apparatus, ultrasonic wave dispersion cleaning, ultrasonic frequency 60kHz, ultrasonic wavelength-division are carried out
Time 80min is dissipated, at mixed liquor;
3. filtering, mixed liquor is placed in the cloth funnel of bottle,suction, is filtered with miillpore filter, cleaning solution is discarded,
Retain filter cake;
4. dry oxidation processes, filter cake is placed in heat-treatment furnace, it is dried and high temperature oxidation process, dry oxidation is warm
500 DEG C of degree, dry oxidization time 2h, must be carbonized boron fine powder after dry;
(4) magnesium, zinc, magnesium yttrium intermediate alloy and open-close type squeeze casting mould are pre-processed
1. magnesium, zinc and magnesium yttrium intermediate alloy are cut into fritter, tile size≤30mm × 30mm × 10mm with machinery;
2. to the surface washes of absolute alcohol of magnesium, zinc and magnesium yttrium intermediate alloy, cleaning is placed in vacuum drying chamber and does
It is dry, 100 DEG C, vacuum degree 2Pa, drying time 30min of drying temperature;
3. carbonization boron fine powder is coated with aluminium foil, dry, 100 DEG C of drying temperature, vacuum degree are placed in vacuum drying chamber
2Pa, drying time 60min;
4. preheating open-close type squeeze casting mould, the coating agent of preparation is coated uniformly on mold cavity inner surface, is coated
Oxidant layer thickness 1mm;After the completion of to be coated, open-close type squeeze casting mould is placed in heating furnace and is preheated, 150 DEG C of preheating temperature,
Preheating time 1h;
(5) melting of magnesium alloy
The melting of magnesium alloy, which is that frequency induction melting furnace is interior in a vacuum, to be carried out, and is in Frequency Induction Heating, is vacuumized, argon
It is completed in gas bottom blowing and mechanical agitation process;
1. opening vacuum intermediate-frequency induction melting furnace, clear up inside graphite melting kettle, makes clean inside crucible;
2. weighing MAG block 4127g ± 0.1g, spelter 784g ± 0.1g and magnesium yttrium intermediate alloy block 571g ± 0.1g, it is placed in earthenware
Crucible bottom;
3. closing vacuum intermediate-frequency induction melting furnace, and closed;
Vacuum pump is opened, furnace air is extracted, pressure in stove is made to reach 1Pa;
Medium frequency induction melting furnace heater is opened, is begun to warm up, 610 DEG C ± 1 DEG C of heating temperature;
4. opening argon gas bottom-blowing device, argon gas, argon gas bottom blowing speed 200C are inputted into crucible3/ min adjusts stove internal pressure
By force, invariablenes pressure of liquid in stove is made to regulate and control in 1 atmospheric pressure, and by outlet pipe valve;
5. when melt temperature is 610 DEG C ± 1 DEG C, carbonization boron fine powder is added using vacuum feeding device;And open machinery
Blender, mixing speed 20r/min, mixing time 10min;
6. stopping stirring, continue to heat, when melt temperature is 730 DEG C ± 1 DEG C, closes mechanical agitator and argon gas bottom blowing
Pipe stands 10min, prepares casting;
(6) extrusion casint
1. opening vacuum intermediate-frequency induction melting furnace, crucible inner melt surface slag is removed, aluminium alloy is cast to extruding casting
It makes in mold cavity;Extrusion casting machine is opened, is squeezed into molten metal by punch-pin, squeeze pressure 250MPa, dwell time 20s;
During solidification alloying reaction occurs for Mg-Zn-Y quasi-crystalline substances, produces stable state quasi-crystalline substance Mg3Zn6Y phases, instead
Answer formula as follows:
α-Mg:Matrix magnesium phase
Mg3Zn6Y:Magnesium zinc yttrium Icosahedral phases
2. ejecting casting, it is cooled to 25 DEG C in air, it is compound to mix enhanced magnesium-based at magnesium zinc yttrium quasi-crystalline substance and boron carbide
Material block;
(7) heat treating castings
1. by magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites block be placed in vacuum heat treatment furnace into
Row heat treatment, 420 DEG C, vacuum degree 2Pa of heat treatment temperature, constant temperature keep the temperature 15h;After constant temperature heat preservation, casting is put into 50 DEG C rapidly
Warm water in carry out quenching treatment, cool time 20s;
2. quenched casting is placed in heat-treatment furnace and carries out ageing treatment, 200 DEG C of aging temp, soaking time 8h;
After heat preservation, stops heating, 25 DEG C are cooled to heat-treatment furnace:
(8) cleaning, test, analysis and characterization
Cast(ing) surface is cleaned, its cleaning is made;Carry out microstructure and mechanics properties testing, analysis, characterization;
Metallographic structure analysis is carried out with light microscope;
Tensile strength and hardness test are carried out with universal tensile testing machine and hardometer;
Appearance analysis is carried out with scanning electron microscope;
XRD analysis is carried out with X-ray diffractometer;
Conclusion:Magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites are rectangular blocks, tensile strength
315MPa, for elongation up to 7%, hardness reaches 108Hv.
Advantageous effect
There is apparent advance compared with the background technology, the present invention, be the feelings for magnesium-based composite material poor mechanical property
Condition, using magnesium alloy as matrix, within raw magnesium zinc yttrium quasi-crystalline substance and boron carbide be hardening constituent, it is molten through frequency induction melting furnace in a vacuum
Refining, magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium is made in argon gas bottom blowing protection, mechanical agitation, extrusion casint and heat treatment
Based composites;This preparation method technique is advanced, and process is tight, and data are accurately full and accurate, and the magnesium-based composite material tension of preparation is strong
Degree reaches 315MPa, and for elongation up to 7%, hardness reaches 108Hv, is the preparation method of advanced mixing reinforced type magnesium based composites.
Description of the drawings
Fig. 1, magnesium-based composite material melting state diagram;
Fig. 2, magnesium-based composite material metallographic structure figure:
Fig. 3, magnesium-based composite material fracture apperance figure:
Fig. 4, magnesium-based composite material X-ray diffraction intensity collection of illustrative plates:
As shown in the figure, list of numerals is as follows:
1, vacuum intermediate-frequency induction melting furnace, 2, stove seat, 3, furnace chamber, 4, escape pipe, 5, air outlet valve, 6, workbench, 7, graphite
Melting kettle, 8, medium frequency induction heater, 9, alloy molten solution, 10, argon gas, 11, bottom blowing motor, 12, bottom blowpipe, 13, vacuum pump,
14, vacuum tube, 15, argon bottle, 16, tunger tube, 17, argon gas valve, 18, electric cabinet, 19, display screen, 20, indicator light, 21, power supply
Switch, 22, Frequency Induction Heating modulator, 23, bottom blowing motor modulator, 24, vacuum pump modulator, the 25, first cable, 26,
Second cable, 27, charge pipe, 28, charging valve, 29, mechanical agitator.
Specific implementation mode
Below in conjunction with attached drawing, the present invention will be further described:
It is magnesium-based composite material melting state diagram, each portion position, connection relation will be matched correctly, pressed according to quantity shown in Fig. 1
Sequence operates.
The magnitude for preparing the chemical substance material that melting uses is determined by pre-set range, with gram, milliliter, li
Rice3For measurement unit.
The melting of magnesium-based composite material, which is that frequency induction melting furnace is interior in a vacuum, to be carried out, and is in Frequency Induction Heating, argon
It is completed in gas bottom blowing and mechanical agitation.
Vacuum intermediate-frequency induction melting furnace is vertical, and the bottom of vacuum intermediate-frequency induction melting furnace 1 is stove seat 2, inside is furnace chamber
3;Bottom is equipped with workbench 6 in furnace chamber 3, the storing graphite melting kettle 7 on workbench 6, outside graphite melting kettle 7 in
Frequency induction heater 8 is surround, and is alloy molten solution 9 in graphite melting kettle 7;The upper right quarter of frequency induction melting furnace 1 is set in a vacuum
There is escape pipe 4, and is controlled by air outlet valve 5;The left part of frequency induction melting furnace 1 is equipped with argon bottle 15 in a vacuum, on argon bottle 15
Equipped with tunger tube 16, argon gas valve 17, tunger tube 16 connects bottom blowing motor 11, and bottom blowing motor 11 connects bottom blowpipe 12, bottom blowpipe 12
It is passed through in graphite melting kettle 7 across stove seat 2, workbench 6, and bottom blowing is carried out to alloy molten solution 9;It is set in the right lower quadrant of stove seat 2
There is vacuum pump 13, and furnace chamber 3 is connected to by vacuum tube 14;The top of frequency induction melting furnace 1 is equipped with charge pipe 27, adds in a vacuum
Material valve 28 and mechanical agitator 29, charge pipe 27, mechanical agitator 29 are stretched into across furnace roof seat in graphite melting kettle 7;
The right part of frequency induction melting furnace 1 is equipped with electric cabinet 18 in a vacuum, and display screen 19, instruction are equipped on electric cabinet 18
Lamp 20, power switch 21, Frequency Induction Heating modulator 22, bottom blowing motor modulator 23, vacuum pump modulator 24;Electric cabinet 18
Medium frequency induction heater 8 is connected by the first cable 25;Electric cabinet 18 connects bottom blowing motor 11, vacuum pump by the second cable 26
13;It is filled by argon gas 10 in furnace chamber 3.
Be the metallographic structure figure of magnesium-based composite material shown in Fig. 2, in metallographic structure figure there is no be mingled with, stomata the defects of,
And Icosahedral phases Mg3Zn6Y and boron carbide particles more can be uniformly distributed in the grain.
Shown in Fig. 3, it is the fracture apperance figure of magnesium-based composite material, there is a large amount of tiny dimple in fracture figure, show it
With good plasticity.
It is magnesium-based composite material X-ray diffraction intensity collection of illustrative plates, as shown in the figure, ordinate refers to for diffracted intensity shown in Fig. 4
Number, abscissa are 2 θ of the angle of diffraction, therefrom it can be found that being primarily present α-Mg matrix magnesium phase, Mg in magnesium-based composite material3Zn6Y quasi-crystalline substances
Phase and B4C hardening constituents.
Claims (2)
1. the preparation method of a kind of magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites, it is characterised in that:It uses
Chemical substance material be:Magnesium, zinc, magnesium yttrium intermediate alloy, boron carbide, zinc oxide, talcum powder, waterglass, deionized water, aluminium
Foil, absolute ethyl alcohol, argon gas, it is as follows that a combination thereof prepares dosage:With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) casting die is prepared
Open-close type squeeze casting mould hot-work die steel making, mold cavity is rectangular, and cavity dimension is 200mm × 160mm
× 90mm, mold cavity surface roughness are Ra0.08-0.16 μm;
(2) coating agent is configured
Zinc oxide 80g ± 1g, talcum powder 50g ± 1g, waterglass 25g ± 1g are weighed, deionized water 300mL ± 1mL is measured, is added
It is stirred in mixing hollander, agitation revolution 50r/min, mixing time 80min, at viscous liquid, as coating agent after stirring;
(3) boron carbide particles are pre-processed
1. ball milling weighs boron carbide 300g ± 0.1g, is placed in the ball grinder of ball mill, ball milling, rotational speed of ball-mill 80r/ are carried out
Min, Ball-milling Time 3h, at fine powder, fine powder grain size≤9 μm after ball milling;
2. ultrasonic wave dispersion cleaning:Fine powder after ball milling is placed in beaker, absolute ethyl alcohol 500mL ± 1mL is then added, is mixed
It closes;
Beaker is placed in ultrasonic wave separating apparatus, ultrasonic wave dispersion cleaning, ultrasonic frequency 60kHz, when ultrasonic wave disperses are carried out
Between 80min, at mixed liquor;
3. filtering, mixed liquor is placed in the cloth funnel of bottle,suction, is filtered with miillpore filter, discard cleaning solution, retained
Filter cake;
4. dry oxidation processes, filter cake is placed in heat-treatment furnace, it is dried and high temperature oxidation process, dry oxidizing temperature
500 DEG C, dry oxidization time 2h, must be carbonized boron fine powder after dry;
(4) magnesium, zinc, magnesium yttrium intermediate alloy and open-close type squeeze casting mould are pre-processed
1. magnesium, zinc and magnesium yttrium intermediate alloy are cut into fritter, tile size≤30mm × 30mm × 10mm with machinery;
2. to the surface washes of absolute alcohol of magnesium, zinc and magnesium yttrium intermediate alloy, cleaning is placed on drying in vacuum drying chamber, does
100 DEG C, vacuum degree 2Pa, drying time 30min of dry temperature;
3. carbonization boron fine powder is coated with aluminium foil, dry, 100 DEG C, vacuum degree 2Pa of drying temperature is placed in vacuum drying chamber,
Drying time 60min;
4. preheating open-close type squeeze casting mould, the coating agent of preparation is coated uniformly on mold cavity inner surface, coats oxidant layer
Thickness 1mm;After the completion of to be coated, open-close type squeeze casting mould is placed in heating furnace and is preheated, 150 DEG C of preheating temperature, preheating
Time 1h;
(5) melting of magnesium alloy
The melting of magnesium alloy, which is that frequency induction melting furnace is interior in a vacuum, to be carried out, and is in Frequency Induction Heating, is vacuumized, argon gas bottom
It blows and completes in mechanical agitation process;
1. opening vacuum intermediate-frequency induction melting furnace, clear up inside graphite melting kettle, makes clean inside crucible;
2. weighing MAG block 4127g ± 0.1g, spelter 784g ± 0.1g and magnesium yttrium intermediate alloy block 571g ± 0.1g, it is placed in crucible bottom
Portion;
3. closing vacuum intermediate-frequency induction melting furnace, and closed;
Vacuum pump is opened, furnace air is extracted, pressure in stove is made to reach 1Pa;
Medium frequency induction melting furnace heater is opened, is begun to warm up, 610 DEG C ± 1 DEG C of heating temperature;
4. opening argon gas bottom-blowing device, argon gas, argon gas bottom blowing speed 200C are inputted into crucible3/ min adjusts pressure in stove, makes
Invariablenes pressure of liquid regulates and controls in 1 atmospheric pressure, and by outlet pipe valve in stove;
5. when melt temperature is 610 DEG C ± 1 DEG C, carbonization boron fine powder is added using vacuum feeding device;And open mechanical agitation
Device, mixing speed 20r/min, mixing time 10min;
6. stopping stirring, continue to heat, when melt temperature is 730 DEG C ± 1 DEG C, close mechanical agitator and argon gas bottom blowpipe,
10min is stood, casting is prepared;
(6) extrusion casint
1. opening vacuum intermediate-frequency induction melting furnace, crucible inner melt surface slag is removed, aluminium alloy is cast to extrusion casint mould
Have in cavity;Extrusion casting machine is opened, is squeezed into molten metal by punch-pin, squeeze pressure 250MPa, dwell time 20s;
During solidification alloying reaction occurs for Mg-Zn-Y quasi-crystalline substances, produces stable state quasi-crystalline substance Mg3Zn6Y phases, reaction equation
It is as follows:
α-Mg:Matrix magnesium phase
Mg3Zn6Y:Magnesium zinc yttrium Icosahedral phases
2. ejecting casting, it is cooled to 25 DEG C in air, at magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites
Block;
(7) heat treating castings
1. magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites block are placed in vacuum heat treatment furnace and carry out heat
Processing, 420 DEG C, vacuum degree 2Pa of heat treatment temperature, constant temperature keep the temperature 15h;After constant temperature heat preservation, casting is put into rapidly 50 DEG C of temperature
Quenching treatment, cool time 20s are carried out in water;
2. quenched casting is placed in heat-treatment furnace and carries out ageing treatment, 200 DEG C of aging temp, soaking time 8h;Heat preservation
Afterwards, stop heating, 25 DEG C are cooled to heat-treatment furnace:
(8) cleaning, test, analysis and characterization
Cast(ing) surface is cleaned, its cleaning is made;Carry out microstructure and mechanics properties testing, analysis, characterization;
Metallographic structure analysis is carried out with light microscope;
Tensile strength and hardness test are carried out with universal tensile testing machine and hardometer;
Appearance analysis is carried out with scanning electron microscope;
XRD analysis is carried out with X-ray diffractometer;
Conclusion:Magnesium zinc yttrium quasi-crystalline substance and boron carbide mixing reinforced type magnesium based composites are rectangular blocks, and tensile strength 315MPa stretches
For long rate up to 7%, hardness reaches 108Hv.
2. the preparation side of a kind of magnesium zinc yttrium quasi-crystalline substance according to claim 1 and boron carbide mixing reinforced type magnesium based composites
Method, it is characterised in that:The melting of magnesium-based composite material, which is that frequency induction melting furnace is interior in a vacuum, to be carried out, and is added in Medium frequency induction
It is completed in heat, argon gas bottom blowing and mechanical agitation.
Vacuum intermediate-frequency induction melting furnace is vertical, and the bottom of vacuum intermediate-frequency induction melting furnace (1) is stove seat (2), inside is furnace chamber
(3);It is equipped with workbench (6) in furnace chamber (3) interior bottom, graphite melting kettle (7), graphite melting earthenware are put on workbench (6)
Crucible (7) is external to be surround by medium frequency induction heater (8), is alloy molten solution (9) in graphite melting kettle (7);Frequency is felt in a vacuum
It answers the upper right quarter of smelting furnace (1) to be equipped with escape pipe (4), and is controlled by air outlet valve (5);Frequency induction melting furnace (1) in a vacuum
Left part is equipped with argon bottle (15), and argon bottle (15) is equipped with tunger tube (16), argon gas valve (17), and tunger tube (16) connects bottom blowing electricity
Machine (11), bottom blowing motor (11) connect bottom blowpipe (12), and bottom blowpipe (12) passes through stove seat (2), workbench (6) to be passed through graphite melting
In crucible (7), and bottom blowing is carried out to alloy molten solution (9);It is equipped with vacuum pump (13) in the right lower quadrant of stove seat (2), and passes through vacuum
Manage (14) connection furnace chamber (3);The top of frequency induction melting furnace (1) is equipped with charge pipe (27), charging valve (28) and machine in a vacuum
Tool blender (29), charge pipe (27), mechanical agitator (29) are stretched into across furnace roof seat in graphite melting kettle (7);
In a vacuum the right part of frequency induction melting furnace (1) be equipped with electric cabinet (18), on electric cabinet (18) be equipped with display screen (19),
Indicator light (20), power switch (21), Frequency Induction Heating modulator (22), bottom blowing motor modulator (23), vacuum pump regulation and control
Device (24);Electric cabinet (18) connects medium frequency induction heater (8) by the first cable (25);Electric cabinet (18) passes through the second cable
(26) connection bottom blowing motor (11), vacuum pump (13);It is filled by argon gas (10) in furnace chamber (3).
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EP19153314.0A EP3553199B1 (en) | 2018-04-13 | 2019-01-23 | A method of preparing magnesium-zinc-yttrium quasicrystal and boron carbide mixed reinforced magnesium-based composite material |
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CN113860313A (en) * | 2021-09-29 | 2021-12-31 | 西安交通大学 | Amorphous boron carbide and preparation method and application thereof |
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CN115608994A (en) * | 2022-09-22 | 2023-01-17 | 哈尔滨理工大学 | Preparation and forming process of magnesium-based composite material lath |
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