CN104947008B - A kind of preparation method of carbon fiber reinforced magnesium-base composite material - Google Patents
A kind of preparation method of carbon fiber reinforced magnesium-base composite material Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of carbon fiber reinforced magnesium-base composite material, use magnesium, carbon fiber is raw material, carbon fiber is through plating zinc on surface, ball milling mixes powder, die-filling, vacuum discharge plasma agglomeration, rolling, make carbon fiber reinforced magnesium-base composite material, this preparation method technique is advanced, data are the fullest and the most accurate, the zinc coat of carbon fiber surface can effectively improve the wetability of carbon fiber and magnesium matrix, interface cohesion is good, the carbon fiber reinforced magnesium-base composite material microhardness of preparation reaches 58HV, bending strength reaches 206MPa, tensile strength reaches 172MPa, it it is the preparation method of very good carbon fiber reinforced magnesium-base composite material.
Description
Technical field
The present invention relates to the preparation method of a kind of carbon fiber reinforced magnesium-base composite material, belong to metal-based compound material
The preparation of material and the technical field of application.
Background technology
Magnesium and magnesium alloy have low-density, high specific strength and high ratio modulus, have good damping characteristics,
Electromagnetic wave shielding and Environmental compatibility；But the rigidity of itself, intensity, thermal coefficient of expansion are low, under hot conditions
Easily it is plastically deformed, poor corrosion resistance in an atmosphere, makes application receive greatly restriction.
Carbon fiber has low-density, high intensity, high-modulus, low-thermal-expansion, radiation-resistant premium properties, carbon
Fiber not only has the mechanical property of material with carbon element, also has the soft machinability of textile fabric, is a new generation
Reinforcing fiber.
Prepare carbon fiber reinforced magnesium-base composite material so that magnesium and carbon fiber are compound, will have that density is low, specific strength,
Specific modulus is high, and thermal coefficient of expansion is low, has good dimensional stability in large temperature range, multiple
Industrial circle has broad application prospects, and magnesium and carbon fiber also have biological characteristics, is equally applicable for raw
Thing Material Field, has boundless development prospect.
The method of processing carbon fiber magnesium base composite material is liquid infiltration at present, but this method exists technique
The shortcoming complicated, cost is high, the problem that simultaneously there is also magnesium and carbon fiber wetability difference.
Summary of the invention
Goal of the invention
It is an object of the invention to the present situation for background technology, with magnesium, carbon fiber as raw material, pre-through carbon fiber
Process, carbon fiber surface is zinc-plated, ball milling mixes powder, discharge plasma sintering, rolling, makes fibre reinforced
Magnesium base composite material, to improve the mechanical property of magnesium base composite material, expanded application scope.
Technical scheme
The present invention use chemical substance material be: magnesium, carbon fiber, acetone, deionized water, absolute ethyl alcohol,
Zinc sulfate, ammonium chloride, boric acid, zine plate, graphite block, graphite cushion block, graphite briquetting, graphite paper, sand paper,
It is as follows that it prepares consumption: with gram, millimeter, milliliter as measurement unit
Magnesium: Mg 1000g ± 0.01g
Carbon fiber: C 50g ± 0.01g
Acetone: C3H6O 1500mL±5mL
Deionized water: H2O 3000mL±10mL
Zinc sulfate: ZnSO4 300g±0.01g
Ammonium chloride: NH4Cl 10g±0.01g
Boric acid: H3BO3 10g±0.01g
Graphite block: C 500mm × 500mm × 100mm
Graphite cushion block: C 200mm × 160mm × 50mm
Graphite briquetting: C 200mm × 160mm × 50mm
Graphite paper: C 1000mm × 1mm × 500mm
Absolute ethyl alcohol: C2H6O 1000mL±10mL
Zine plate: Zn 60mm × 70mm × 3mm
Sand paper: 400 mesh 300mm × 0.5mm × 200mm
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material using preparation to carry out selected, and carries out quality purity control:
Magnesium: solid powder 99.99%
Carbon fiber: solid fabric 99.6%
Acetone: liquid liquid 99.9%
Deionized water: liquid liquid 99.9%
Zinc sulfate: solid powder 99.5%
Ammonium chloride: solid powder 99.5%
Boric acid: solid powder 99.5%
Graphite block: solid slug 98.5%
Graphite cushion block: solid slug 98.5%
Graphite briquetting: solid slug 98.5%
Graphite paper: solid-state paper-like 98.5%
Absolute ethyl alcohol: liquid liquid 99.7%
Zine plate: solid-state tabular 99.99%
Sand paper: solid-state tabular
(2) graphite jig is made
Graphite jig graphite block makes, and mold cavity is rectangular cavities, and cavity dimension is
200mm × 160mm × 100mm, mold cavity surface roughness Ra≤0.08～0.16 μm；
(3) pretreatment carbon fiber
1. carbon fiber is put in vacuum heat treatment furnace, airtight, then extract furnace air, make furnace chamber internal pressure
Reach by force 2Pa, then carry out being heated to 400 DEG C ± 5 DEG C, constant temperature insulation 15min, then stop heating, with stove
It is cooled to 25 DEG C；
2. the carbon fiber after cooling is put in acetone, soak 2h；
3. clean by deionized water, dry；
(4) carbon fiber surface is zinc-plated
1. prepare galvanizing flux, weigh zinc sulfate 300g ± 0.01g, ammonium chloride 7g ± 0.01g, boric acid 5g ± 0.01g,
Putting in beaker, be dissolved in 1000mL deionized water, stirring and dissolving, pH is 3.9, in acidity；
2. dress carbon fiber, by carbon fiber dress into strips, a size of Φ 10mm × 80mm；
The most zinc-plated, galvanizing flux is placed in galvanizing bath, the carbon fiber of dress is vertically put into galvanizing bath, and
It is fixed as negative electrode；Zine plate is vertically put into galvanizing bath, and is fixed as anode；Galvanizing flux carbon fiber to be flooded,
Zine plate；
4. connecting negative electrode, anode supply, voltage 220V, current strength 1A, the zinc-plated time is 5min；
After the most zinc-plated, carbon fiber taken out and dries；
6. clean, the carbon fiber after zinc-plated is placed in beaker, add deionized water 1000mL, soak, stir
Dynamic cleaning 10min, dries after cleaning；
7. it is vacuum dried, the carbon fiber dried is placed in quartz container, be subsequently placed in vacuum drying chamber dry
Dry, baking temperature is 100 DEG C, vacuum 20Pa, drying time 300min；
8. shear carbon fiber, the carbon fiber after zinc-plated is cut into strip, length≤1mm；
(5) preparation, ball milling
1. in vacuum glove box, weigh magnesium powder 932g ± 0.01g, carbon fiber 28g ± 0.01g, load ball grinder,
And it is airtight；
2. ball grinder is placed on ball mill, carries out ball milling, ball milling speed 300r/min, Ball-milling Time 60min,
Mixing fine powders is become after ball milling；
(6) die-filling
Graphite jig is vertically arranged on steel flat board, graphite cushion block is placed in bottom mold cavity, by graphite
Paper is placed on graphite cushion block, and then mixing fine powders is placed in graphite paper top, and top graphite paper covers, and
Fastened by graphite briquetting；
(7) vacuum discharge plasma agglomeration shaping
The sintering of carbon fiber reinforced magnesium-base composite material is carried out in vacuum discharge plasma agglomeration stove, is
Under vacuum conditions, heating, course of exerting pressure complete；
1. die-filling graphite jig parallel vertical is moved on the workbench in vacuum discharge plasma agglomeration stove,
And vertically fastened by upper holder block, pressure block；
2. vacuum discharge plasma agglomeration stove is closed, and airtight；
3. open outer water circulating cooling pipe, carry out outer water circulating cooling；
4. opening vavuum pump, extract furnace air, in making furnace chamber, pressure reaches 5Pa, and constant；
5. unlatching vacuum discharge plasma heating furnace heater switch, the graphite jig in heating furnace chamber and mixing fine powders,
Heating-up temperature 420 DEG C ± 2 DEG C, constant temperature temperature retention time is 20min；
Opening pressure motor, press the mixing fine powders in graphite jig, press pressure 40MPa；
In heating, course of exerting pressure, the mixing fine powders sinter molding in graphite jig is block；
6. after sinter molding, stop heating, continue pressure, make block cool to 25 DEG C with the furnace；
7. blow-on, die sinking, take out block, be carbon fiber reinforced magnesium-base composite material block；
(8) cleaning block surface
Block materials is placed on steel flat board, with the positive and negative surface of sand papering block and periphery so that it is bright and clean；
(9) rolling
1. block materials is placed in heating furnace, preheats, preheat temperature 280 DEG C, preheating time 30min；
2. the block materials of preheating is placed on hot-rolling mill, carries out vertical hot-roll forming, block materials after hot rolling
For template, template thickness is 1mm；
(10) cleaning, cleaner plate shape surface
Flat-form material is placed on steel flat board, with machinery, flat-form material periphery is cut；Then sand is used
Polished in positive and negative surface and periphery by paper；
With washes of absolute alcohol flat-form material periphery and positive and negative surface so that it is clean；
(11) detect, analyze, characterize
The carbon fiber reinforced magnesium-base composite material of preparation is detected, analyzes, characterizes；
By SEM, composite section is carried out morphology analysis；
With universal testing machine, composite is carried out Resarch on A New Type；
Conclusion: the carbon fiber reinforced magnesium-base composite material of preparation, microhardness reaches 58HV, and bending strength reaches
To 206MPa, tensile strength reaches 172MPa；
(12) store
The carbon fiber reinforced magnesium-base composite material of preparation soft material is vacuum-packed, and is stored in shady and cool clean ring
Border, acid-alkali salt moistureproof, sun-proof, anti-corrodes, storage temperature 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, and using magnesium, carbon fiber is raw material, and carbon is fine
Dimension plating zinc on surface, ball milling mix powder, die-filling, vacuum discharge plasma agglomeration, rolling, make fibre reinforced
Magnesium base composite material, this preparation method technique is advanced, and data are the fullest and the most accurate, and the zinc coat of carbon fiber surface can
Being effectively improved the wetability of carbon fiber and magnesium matrix, interface cohesion is good, and the carbon fiber reinforced magnesium-base of preparation is multiple
Condensation material microhardness reaches 58HV, and bending strength reaches 206MPa, and tensile strength reaches 172MPa, is
The preparation method of very good carbon fiber reinforced magnesium-base composite material.
Accompanying drawing explanation
Fig. 1, carbon fiber reinforced magnesium-base composite material vacuum discharge plasma agglomeration state diagram
Fig. 2, carbon fiber reinforced magnesium-base composite material cross-section morphology figure
Shown in figure, list of numerals is as follows:
1, vacuum discharge plasma agglomeration stove, 2, footstock, 3, base, 4, bearing, 5, the circulation of outer water cold
But manage, 6, vavuum pump, 7, vacuum tube, 8, cooling water tank, 9, water pump, 10, water inlet pipe, 11 backwater
Pipe, 12, workbench, 13, pressure block, 14, graphite jig, 15, lower cushion block, the 16, first graphite paper,
17, mixing fine powders, the 18, second graphite paper, 19, upper holder block, 20, pipe valve of giving vent to anger, 21, pressure motor,
22, electric cabinet, 23, display screen, 24, indicator lamp, 25, heating temperature control, 26, vavuum pump control
Device processed, 27, water pump controller, 28, pressure electric machine controller, the 29, first wire, the 30, second wire,
31, privates, 32, furnace chamber.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, for carbon fiber reinforced magnesium-base composite material vacuum discharge plasma agglomeration state diagram, each portion
Position, annexation is wanted correctly, and proportioning according to quantity sequentially operates.
The value of chemical substance that preparation uses is to determine by the scope pre-set, with gram, milliliter, in the least
Rice is measurement unit.
The preparation of carbon fiber reinforced magnesium-base composite material is carried out in vacuum discharge plasma agglomeration stove, is
Under vacuum conditions, heating, course of exerting pressure complete；
Vacuum discharge plasma agglomeration stove is vertical, on the top of vacuum discharge plasma agglomeration stove 1 be footstock 2,
Bottom is base 3, bearing 4；Top, top 2 is provided with pressure motor 21；It is provided with in base 3, bearing 4
Vavuum pump 6, cooling water tank 8；In the outside of vacuum discharge plasma agglomeration stove 1 by outer water circulating cooling pipe 5
Cincture；Being furnace chamber 32 in vacuum discharge plasma agglomeration stove 1, the inner bottom part at furnace chamber 32 is provided with workbench
12, the most vertically graphite jig 14；It is lower cushion block 15 at graphite jig 14 inner bottom part,
It is the first graphite paper 16 on lower cushion block 15 top, is mixing fine powders 17 on the first graphite paper 16 top, mixed
Closing fine powder 17 top is the second graphite paper 18, and the second graphite paper 18 top is upper holder block 19, upper holder block 19
Top connects pressure block 13, and pressure block 13 is connected with the pressure motor 21 on footstock 2 top；Vavuum pump 6 leads to
Cross vacuum tube 7 and connect furnace chamber 32；Be provided with water pump 9 on cooling water tank 8 top, water pump 9 is by water inlet pipe 10
Connecting the outer water circulating cooling pipe 5 of right part, outer water circulating cooling pipe 5 connects cold by the return pipe 11 of left part
But water tank 8, form cooling water circulation loop；Right part at vacuum discharge plasma agglomeration stove 1 is provided with electric cabinet
22, electric cabinet 22 is provided with display screen 23, indicator lamp 24, heating temperature control 25, vavuum pump control
Device 26 processed, water pump controller 27, pressure electric machine controller 28；Electric cabinet 22 is by the second wire 30 and water
Pump 9 connects, and electric cabinet 22 is connected with vavuum pump 6 by the first wire 29, and electric cabinet 22 is led by the 3rd
Line 31 is connected with pressure motor 21.
Shown in Fig. 2, for carbon fiber reinforced magnesium-base composite material cross-section morphology figure, shown in figure, carbon fiber divides
The interface being distributed between magnesium granules, a part for carbon fiber has embedded in magnesium granules so that between particle
Boundary strength improves, and can significantly improve the mechanical property of this composite.
Claims (2)
1. the preparation method of a carbon fiber reinforced magnesium-base composite material, it is characterised in that: make
Chemical substance material be: magnesium, carbon fiber, acetone, deionized water, absolute ethyl alcohol, sulphur
Acid zinc, ammonium chloride, boric acid, zine plate, graphite block, graphite cushion block, graphite briquetting, graphite paper,
Sand paper, it is as follows that it prepares consumption: with gram, millimeter, milliliter as measurement unit
Magnesium: Mg 1000g ± 0.01g
Carbon fiber: C 50g ± 0.01g
Acetone: C3H6O 1500mL±5mL
Deionized water: H2O 3000mL±10mL
Zinc sulfate: ZnSO4 300g±0.01g
Ammonium chloride: NH4Cl 10g±0.01g
Boric acid: H3BO3 10g±0.01g
Graphite block: C 500mm × 500mm × 100mm
Graphite cushion block: C 200mm × 160mm × 50mm
Graphite briquetting: C 200mm × 160mm × 50mm
Graphite paper: C 1000mm × 1mm × 500mm
Absolute ethyl alcohol: C2H6O 1000mL±10mL
Zine plate: Zn 60mm × 70mm × 3mm
Sand paper: 400 mesh 300mm × 0.5mm × 200mm
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material using preparation to carry out selected, and carries out quality purity control
System:
Magnesium: solid powder 99.99%
Carbon fiber: solid fabric 99.6%
Acetone: liquid liquid 99.9%
Deionized water: liquid liquid 99.9%
Zinc sulfate: solid powder 99.5%
Ammonium chloride: solid powder 99.5%
Boric acid: solid powder 99.5%
Graphite block: solid slug 98.5%
Graphite cushion block: solid slug 98.5%
Graphite briquetting: solid slug 98.5%
Graphite paper: solid-state paper-like 98.5%
Absolute ethyl alcohol: liquid liquid 99.7%
Zine plate: solid-state tabular 99.99%
Sand paper: solid-state tabular
(2) graphite jig is made
Graphite jig graphite block makes, and mold cavity is rectangular cavities, and cavity dimension is
200mm × 160mm × 100mm, mold cavity surface roughness Ra≤0.08～0.16 μm；
(3) pretreatment carbon fiber
1. carbon fiber is put in vacuum heat treatment furnace, airtight, then extract furnace air, make
In furnace chamber, pressure reaches 2Pa, then carries out being heated to 400 DEG C ± 5 DEG C, constant temperature insulation 15min,
Then stop heating, cool to 25 DEG C with the furnace；
2. the carbon fiber after cooling is put in acetone, soak 2h；
3. clean by deionized water, dry；
(4) carbon fiber surface is zinc-plated
1. prepare galvanizing flux, weigh zinc sulfate 300g ± 0.01g, ammonium chloride 7g ± 0.01g, boron
Acid 5g ± 0.01g, puts in beaker, is dissolved in 1000mL deionized water, stirring and dissolving,
PH is 3.9, in acidity；
2. dress carbon fiber, by carbon fiber dress into strips, a size of Φ 10mm × 80mm；
The most zinc-plated, galvanizing flux is placed in galvanizing bath, the carbon fiber of dress is vertically put into zinc-plated
In groove, and it is fixed as negative electrode；Zine plate is vertically put into galvanizing bath, and is fixed as anode；Plating
Zinc liquid carbon fiber to be flooded, zine plate；
4. connecting negative electrode, anode supply, voltage 220V, current strength 1A, the zinc-plated time is
5min；
After the most zinc-plated, carbon fiber taken out and dries；
6. clean, the carbon fiber after zinc-plated be placed in beaker, add deionized water 1000mL,
Soak, 10min is cleaned in agitation, dries after cleaning；
7. it is vacuum dried, the carbon fiber dried is placed in quartz container, be subsequently placed in vacuum and do
In dry case be dried, baking temperature is 100 DEG C, vacuum 20Pa, drying time 300min；
8. shear carbon fiber, the carbon fiber after zinc-plated is cut into strip, length≤1mm；
(5) preparation, ball milling
1. in vacuum glove box, weigh magnesium powder 932g ± 0.01g, carbon fiber 28g ± 0.01g,
Load ball grinder, and airtight；
2. ball grinder is placed on ball mill, carries out ball milling, ball milling speed 300r/min, ball milling
Time 60min, becomes mixing fine powders after ball milling；
(6) die-filling
Graphite jig is vertically arranged on steel flat board, graphite cushion block is placed in bottom mold cavity,
Being placed in by graphite paper on graphite cushion block, then mixing fine powders is placed in graphite paper top, top is used
Graphite paper covers, and is fastened by graphite briquetting；
(7) vacuum discharge plasma agglomeration shaping
The sintering of carbon fiber reinforced magnesium-base composite material is in vacuum discharge plasma agglomeration stove
Carry out, be under vacuum conditions, heating, course of exerting pressure complete；
1. die-filling graphite jig parallel vertical is moved in vacuum discharge plasma agglomeration stove
On workbench, and vertically fastened by upper holder block, pressure block；
2. vacuum discharge plasma agglomeration stove is closed, and airtight；
3. open outer water circulating cooling pipe, carry out outer water circulating cooling；
4. opening vavuum pump, extract furnace air, in making furnace chamber, pressure reaches 5Pa, and constant；
5. vacuum discharge plasma heating furnace heater switch is opened, graphite jig in heating furnace chamber and mixed
Closing fine powder, heating-up temperature 420 DEG C ± 2 DEG C, constant temperature temperature retention time is 20min；
Opening pressure motor, press the mixing fine powders in graphite jig, press pressure 40MPa；
In heating, course of exerting pressure, the mixing fine powders sinter molding in graphite jig is block；
6. after sinter molding, stop heating, continue pressure, make block cool to 25 DEG C with the furnace；
7. blow-on, die sinking, take out block, be carbon fiber reinforced magnesium-base composite material block；
(8) cleaning block surface
Block materials is placed on steel flat board, with the positive and negative surface of sand papering block and periphery,
Make it bright and clean；
(9) rolling
1. block materials is placed in heating furnace, preheats, preheat temperature 280 DEG C, preheating
Time 30min；
2. the block materials of preheating is placed on hot-rolling mill, carries out vertical hot-roll forming, after hot rolling
Block materials is template, and template thickness is 1mm；
(10) cleaning, cleaner plate shape surface
Flat-form material is placed on steel flat board, with machinery, flat-form material periphery is cut；
Then with sand paper, polished in positive and negative surface and periphery；
With washes of absolute alcohol flat-form material periphery and positive and negative surface so that it is clean；
(11) detect, analyze, characterize
The carbon fiber reinforced magnesium-base composite material of preparation is detected, analyzes, characterizes；
By SEM, composite section is carried out morphology analysis；
With universal testing machine, composite is carried out Resarch on A New Type；
Conclusion: the carbon fiber reinforced magnesium-base composite material of preparation, microhardness reaches 58HV,
Bending strength reaches 206MPa, and tensile strength reaches 172MPa；
(12) store
The carbon fiber reinforced magnesium-base composite material of preparation soft material is vacuum-packed, and is stored in the moon
Cool clean environment, acid-alkali salt moistureproof, sun-proof, anti-corrodes, storage temperature 20 DEG C, relatively
Humidity≤10%.
The preparation of a kind of carbon fiber reinforced magnesium-base composite material the most according to claim 1
Method, it is characterised in that: the preparation of carbon fiber reinforced magnesium-base composite material is in vacuum discharge etc.
Carry out in ion sintering furnace, be under vacuum conditions, heating, course of exerting pressure complete；
Vacuum discharge plasma heating furnace is vertical, upper in vacuum discharge plasma agglomeration stove (1)
Portion be footstock (2), bottom be base (3), bearing (4)；Top (2) top is provided with pressure
Force motor (21)；It is provided with vavuum pump (6), cooling water tank in base (3), bearing (4)
(8)；In the outside of vacuum discharge plasma agglomeration stove (1) by outer water circulating cooling pipe (5)
Cincture；It is furnace chamber (32) in vacuum discharge plasma agglomeration stove (1), in furnace chamber (32)
Inner bottom part be provided with workbench (12), vertically graphite jig (14) on workbench (12)；
It is lower cushion block (15) at graphite jig (14) inner bottom part, is on lower cushion block (15) top
One graphite paper (16), is mixing fine powders (17) on the first graphite paper (16) top, in mixing
Fine powder (17) top is the second graphite paper (18), and the second graphite paper (18) top is upper pressure
Block (19), upper holder block (19) top connects pressure block (13), pressure block (13) and footstock
(2) the pressure motor (21) on top connects；Vavuum pump (6) is by vacuum tube (7) even
Logical furnace chamber (32)；Be provided with water pump (9) on cooling water tank (8) top, water pump (9) passes through
Water inlet pipe (10) connects the outer water circulating cooling pipe (5) of right part, outer water circulating cooling pipe (5)
Connect cooling water tank (8) by the return pipe (11) of left part, form cooling water circulation loop；
Right part in vacuum discharge plasma agglomeration stove (1) is provided with electric cabinet (22), in electric cabinet (22)
It is provided with display screen (23), indicator lamp (24), heating temperature control (25), vavuum pump
Controller (26), water pump controller (27), pressure electric machine controller (28)；Electric cabinet (22)
Being connected with water pump (9) by the second wire (30), electric cabinet (22) passes through the first wire
(29) being connected with vavuum pump (6), electric cabinet (22) is by privates (31) and pressure
Force motor (21) connects.
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Cited By (1)
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| CN108385040A (en) * | 2018-02-22 | 2018-08-10 | 深圳万佳互动科技有限公司 | A kind of chopped carbon fiber enhancing magnesium-aluminum-based composite material and preparation method |
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