CN107187124A - A kind of magnesium-based superhybrid composite laminate and preparation method thereof - Google Patents
A kind of magnesium-based superhybrid composite laminate and preparation method thereof Download PDFInfo
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- CN107187124A CN107187124A CN201710440720.3A CN201710440720A CN107187124A CN 107187124 A CN107187124 A CN 107187124A CN 201710440720 A CN201710440720 A CN 201710440720A CN 107187124 A CN107187124 A CN 107187124A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/42—Alternating layers, e.g. ABAB(C), AABBAABB(C)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
Abstract
The invention provides a kind of magnesium-based superhybrid composite laminate, if if comprising dried layer fiber reinforced resin layer and dried layer fiber metal, the fiber reinforced resin layer and fiber metal are alternately laminated to be set；Fibres bond layer of the fiber metal comprising metal core board two surfaces relative with metal core board is arranged at, the fibres bond layer is bonded to the metal core board and fiber reinforced resin layer；The metal core board is magnesium plate or magnesium alloy plate.The magnesium-based superhybrid composite laminate for the special construction that the present invention is provided has excellent mechanical property, and tensile strength is 1295~1300MPa, and stretch modulus is 91~94GPa, and specific strength is 744.25~786.13Mpa/ (g/cm3), specific modulus is 52.3~54.36GPa/ (g/cm3), bending strength is 1213~1235MPa, and layer cuts intensity for 85~89MPa.
Description
Technical field
The present invention relates to superhybrid composite technical field, more particularly to a kind of magnesium-based superhybrid composite laminate and
Its preparation method.
Background technology
Fiber metal laminate is the new hybrid buildup structural composite material of a class, and FML is referred to as in the world
(Fiber-Metal Laminate) laminate, its Typical Representative is aramid fiber-aluminum alloy laminate (ARALL laminates) and glass
Glass fiber-aluminum alloy laminate (GLARE laminates).Superhybrid composite both remains fiber-reinforced resin matrix compound material
It is high than strong, Gao Bimo, excellent fatigue performance the features such as, the good rigidity of metal material is remained again, impact resistance, easy
The features such as processability, the deficiencies such as material easy firing, the easy moisture absorption, easy aging, the low, poorly conductive of case hardness are also overcomed, are one
The rising structural material of class.
The preparation method and properties of product of superhybrid composite have been widely studied, and result of study shows super mix again
Condensation material has potential application field.At present, GLARE laminates have applied the upper body housing in A380 aircrafts in large area
It is a significant innovative point of A380 aircraft materials technologies in body structure.
But, although the species of existing superhybrid composite is of all kinds and each has something to recommend him in the prior art.But,
The overall mechanical properties of the existing all kinds of superhybrid composites of in the market are universal relatively low, it is impossible to which satisfaction has to mechanical property
The application demand of high requirement.
The content of the invention
It is an object of the invention to provide a kind of magnesium-based superhybrid composite laminate with excellent mechanical property and
Its preparation method, to meet the application demand being had higher requirements to mechanical property.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of magnesium-based superhybrid composite laminate, if if including dried layer fiber-resin layer and dried layer
Fiber metal layer, the alternately laminated setting of the fiber-resin layer and fiber metal layer；
The fiber metal layer includes the fibres bond on metal core board two surface relative with metal core board is arranged at
Layer, the fibres bond layer is bonded to the metal core board and fiber-resin layer；
The metal core board is magnesium plate or magnesium alloy plate.
It is preferred that, the fiber in fiber and every layer of fiber metal layer in every layer of fiber-resin layer is independently that carbon is fine
One kind in dimension, glass fibre, aramid fiber, basalt fibre, Fypro, aromatic polyester fiber, polyethylene fibre
Or it is several；
The fiber is unidirectional fibre or fabric.
It is preferred that, the resin in the fiber-resin layer is epoxy resin, span comes amide resin, unsaturated polyurethanes
Resin, phenolic resin, polyurethane, polyethylene, polyvinyl chloride, polystyrene, polypropylene, acrylonitrile-butadiene-benzene second
One kind in alkene copolymer, polyvinyl alcohol, polyacetal resin, polyamide, polyformaldehyde, makrolon, polyphenylene oxide, polysulfones and rubber
Or it is several.
It is preferred that, the binding agent in the fibres bond layer is epoxy adhesive, span carrys out amide resin binding agent,
Unsaturated polyurethane resin binding agent, phenolic resin adhesive, polyurethane binding agent, polyethylene binder, polychlorostyrene second
Alkene binding agent, polystyrene binder, polypropylene adhesive, acrylonitrile-butadiene-styrene copolymer binding agent, polyethylene
Alcohol binding agent, polyacetal resin binding agent, polyamide binders, polyformaldehyde binding agent, polycarbonate adhesive agent, polyphenylene oxide are bonded
One or more in agent, polysulfones binding agent and rubber cement.
It is preferred that, the thickness of the fiber-resin layer is 0.1~5mm；
The thickness of the fiber metal layer is 0.1~5mm；
The thickness of the metal core board be 0.05~5mm, and metal core board thickness be less than fiber metal layer thickness.
Present invention also offers a kind of preparation method of magnesium-based superhybrid composite laminate described in above-mentioned technical proposal, bag
Containing following steps：
By fiber-resin layer fiber impregnation in resin emulsion, fibre resin prepreg is obtained；
By fibres bond layer fiber impregnation in binding agent, fiber binder prepreg is obtained；
The fibre resin prepreg, fiber binder prepreg and metal core board are subjected to laying setting, are combined
Laminate precursor；
Hot pressing is carried out to the composite layered plate precursor, magnesium-based superhybrid composite laminate is obtained.
It is preferred that, the resin emulsion is epoxy resin latex, span comes amide resin emulsion, unsaturated polyurethane resin
Emulsion, Phenolic resin emulsion, polyurethane fat liquor, polyethylene emulsion, polyvinyl chloride emulsion, polystyrene emulsion, poly- third
Alkene emulsion, acrylonitrile-butadiene-styrene copolymer emulsion, polyvinyl alcohol emulsions, polyacetal resin emulsion, polyamide emulsion,
One or more in polyformaldehyde emulsion, polycarbonate emulsion, polyphenylene oxide emulsion, polysulfones emulsion and rubber latex.
It is preferred that, the temperature of the hot pressing is 60~350 DEG C；
The pressure of the hot pressing is 0.1~1.6MPa；
The time of the hot pressing is 1~10 hour.
The invention provides a kind of magnesium-based superhybrid composite laminate, if if including dried layer fiber-resin layer and dried layer
Fiber metal layer, the alternately laminated setting of the fiber-resin layer and fiber metal layer；The fiber metal layer includes metal
The fibres bond layer on core plate two surfaces relative with metal core board is arranged at, fibres bond layer to the metal core board and
Fiber-resin layer is bonded；The metal core board is magnesium plate or magnesium alloy plate.The magnesium-based for the special construction that the present invention is provided surpasses
Mixed composite material laminate, enable to fiber-resin layer and metal core layer closely combine, the two cooperate, mutually more
Mend so that obtained composite layered plate has excellent mechanical property.From the experimental result of embodiment, tensile strength is 1295
~1300MPa, stretch modulus is 91~94GPa, and specific strength is 744.25~786.13Mpa/ (g/cm3), specific modulus is 52.3
~54.36GPa/ (g/cm3), bending strength is 1213~1235MPa, and layer cuts intensity for 85~89MPa.
Brief description of the drawings
Fig. 1 is the structural representation that phosphoric acid anodizing of the present invention handles equipment therefor；
Fig. 2 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 2；
Fig. 3 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 3；
Fig. 4 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 4；
Fig. 5 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 5；
Fig. 6 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 6；
Fig. 7 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 7；
Fig. 8 is the structural representation of magnesium-based superhybrid composite laminate in the embodiment of the present invention 8.
Embodiment
The invention provides a kind of magnesium-based superhybrid composite laminate, if if including dried layer fiber-resin layer and dried layer
Fiber metal layer, the alternately laminated setting of the fiber-resin layer and fiber metal layer；
The fiber metal layer includes the fibres bond on metal core board two surface relative with metal core board is arranged at
Layer, the fibres bond layer is bonded to the metal core board and fiber-resin layer；
The metal core board is magnesium plate or magnesium alloy plate.
If if the magnesium-based superhybrid composite laminate that provides of the present invention comprising dried layer fiber-resin layer and dried layer fiber-
Metal level.The present invention does not have any particular/special requirement to the particular number of fiber-resin layer and fiber metal layer, at this
In the specific embodiment of invention, the magnesium-based superhybrid composite laminate comprises at least one layer of fiber-resin layer and one layer of fibre
Dimension-metal level.
In the present invention, fiber-resin layer and fiber metal layer is alternately laminated sets, the fiber-resin layer and
Fiber metal layer can as the magnesium-based superhybrid composite laminate outer surface.In the present invention, every layer of fibre
The thickness of dimension-resin bed is preferably 0.1~5mm, more preferably 0.1~4mm, most preferably 0.2~3mm；Every layer of fiber-
The thickness of metal level is preferably 0.1~5mm, more preferably 0.1~4mm, most preferably 0.2~3mm.
In the present invention, the fiber metal layer includes metal core board two surfaces relative with metal core board is arranged at
Fibres bond layer, fibres bond layer bonds to the metal core board and fiber-resin layer.In the present invention, institute
Metal core board is stated for magnesium plate or magnesium alloy plate.Metal core board described in preferred pair of the present invention is surface-treated, metal-cored to improve
The surface contact strength of plate and fibres bond layer.In the present invention, the surface treatment preferably comprises following steps：
That removes metal core board surface sticks thing, is not glued metal core board；
To it is described do not glue metal core board sequentially carry out that organic solvent cleaning, salt are washed, alkaline etching, hot water wash, first time cold water are washed,
Light extraction processing, second of cold water are washed, the metal core board after being cleaned；
Anodized, the metal core board being surface-treated are carried out to the metal core board after the cleaning.
It is of the invention preferred remove metal core board surface stick thing, do not glued metal core board.The present invention removes the gold
The thing that sticks for belonging to core plate surface is due to that metallic article surface typically can all stick one or more impurity, such as oxide-film, Jiao
Paste thing, protection gummed paper, antirust oil, paint word, coating, antiscuffing paste, glue and fingerprint etc..In the present invention, the metal core board
The sweep-out method of surface adhesion thing is specifically as shown in table 1 below.In a particular embodiment of the present invention, the present invention can be according to institute
State the specific species for sticking thing being infected with metal core board surface and select corresponding sweep-out method.The present invention is to described specific glutinous
The determination methods of addendum do not have any particular/special requirement, are judged using method well-known to those skilled in the art.
In the present invention, when the metal core board surface comprising it is a variety of stick thing when, the removal order that the present invention sticks thing to described does not have
There is any particular/special requirement, all things that stick can be removed totally.
The different types of sweep-out method for sticking thing of table 1
Obtain after the not viscous metal core board, the present invention is preferred to carry out organic solvent cleaning operation.Of the invention specific real
Apply in example, the organic solvent is preferably gasoline or acetone.The operating process that the present invention is cleaned to the organic solvent is not appointed
What particular/special requirement, is carried out by the way of metal device well-known to those skilled in the art cleaning.
The present invention preferably after organic solvent cleaning, carries out sand paper polishing, by the metal to the metal core board
The impurity that core plate surface is difficult to clean is polished off.
After the organic solvent cleaning, metal core board described in preferred pair of the present invention carries out salt and washed.In the present invention, the salt
Wash and deionized water, tertiary sodium phosphate, sodium metasilicate and detergent are preferably comprised with chemical reagent.In the specific embodiment of the invention,
The detergent selection product such as commonly used detergent or dish detergent on the market.In chemical reagent of the present invention,
The concentration of the tertiary sodium phosphate is preferably 50~60g/L, more preferably 52~58g/L, most preferably 54~56g/L；It is described inclined
The concentration of sodium metasilicate is preferably 10~20g/L, more preferably 12~18g/L, most preferably 14~16g/L；The detergent
Concentration is preferably 0.5~1g/L, more preferably 0.6~0.9g/L, most preferably 0.7~0.8g/L.
In the present invention, the temperature that the salt is washed is preferably 60~70 DEG C, more preferably 62~68 DEG C, most preferably 64~
66℃；The time that the salt is washed is preferably 1~5min, more preferably 2~4min, most preferably 3min.
After the salt is washed, metal core board described in preferred pair of the present invention carries out alkaline etching.In the present invention, alkali used in the alkaline etching
Erosion liquid preferably comprises deionized water, sodium hydroxide, tertiary sodium phosphate, sodium carbonate, sodium metasilicate and detergent.In the present invention, this
Locate the detergent identical with detergent species described above, no longer repeated herein.In Alkaline etchant of the present invention, institute
The concentration for stating sodium hydroxide is preferably 10~20g/L, more preferably 12~18g/L, most preferably 14~16g/L；The phosphoric acid
The concentration of trisodium is preferably 30~50g/L, more preferably 35~45g/L, most preferably 40g/L；The concentration of the sodium carbonate is excellent
Elect 10~20g/L, most preferably more preferably 12~18g/L, 14~16g/L as；The concentration of the sodium metasilicate is preferably 10
~20g/L, more preferably 12~18g/L, most preferably 14~16g/L；The concentration of the detergent is preferably 0.5~1g/L,
More preferably 0.6~0.9g/L, most preferably 0.7~0.8g/L.
In the present invention, the alkaline etching process can thoroughly remove metal core board surface film oxide and dirt, make metal-cored
Plate surface uniform activation, wherein the sodium hydroxide component will can be changed into being dissolved in the soap and glycerine of water after fat saponification；Institute
Sodium carbonate components solution alkaline is stated, there is the effect that pH value is adjusted to Alkaline etchant and cleaning fluid, deoiling effect is fine；The phosphorus
Sour trisodium component have with sodium carbonate identical advantage, but also with certain emulsification, because washing property itself is good, have
Help the elution of sodium metasilicate；The sodium pyrophosphate component is similar to sodium phosphate, while having complexing power, prevents article surface from giving birth to
Into insoluble hard water soap-film, raising salt is conducive to wash quality；The sodium metasilicate component has certain surface-active and soap
Change ability.
In the present invention, the temperature of the alkaline etching process is preferably 60~80 DEG C, more preferably 65~75 DEG C, is most preferably
70℃；The time of the alkaline etching process is preferably 1~5min, more preferably 2~4min, most preferably 3min.
After the alkaline etching, metal core board described in preferred pair of the present invention carries out hot water wash.In the present invention, the hot water wash
Temperature is preferably 40~60 DEG C, more preferably 45~55 DEG C, most preferably 50 DEG C；The time of the hot water wash is preferably 1~
5min, more preferably 2~4min, most preferably 3min.
After the hot water wash, metal core board described in preferred pair of the present invention carries out first time cold water and washed.In the present invention, it is described
The temperature that first time cold water is washed preferably normal temperature.In the present invention, the time that the first time cold water is washed is preferably 1~5min,
More preferably 2~4min, most preferably 3min.
After the first time cold water is washed, metal core board described in preferred pair of the present invention carries out light extraction processing.In the present invention, institute
It is preferably nitric acid or sulfuric acid that light extraction processing, which is stated, with light-emitting solution, and the volumetric concentration of the light-emitting solution is preferably 10~30%, more excellent
Elect 15~25%, most preferably 20% as.The present invention does not have any particular determination to the method for light extraction processing, will be described
Metal core board is immersed in light-emitting solution.In the present invention, the time of the light extraction processing is preferably 5~15min, more preferably
For 8~13min, most preferably 10min.
After the light extraction processing, metal core board described in preferred pair of the present invention carries out second of cold water and washed.In the present invention, institute
State the temperature preferably normal temperature that second of cold water is washed.In the present invention, the time that second of the cold water is washed is preferably 1~
5min, more preferably 2~4min, most preferably 3min.In the present invention, second of the cold water, which is washed, is preferred to use deionized water
Cleaned, to avoid introducing unnecessary impurity.
After second of the cold water is washed, metal core board described in preferred pair of the present invention carries out phosphoric acid anodizing processing.At this
In invention, the concentration of phosphoric acid solution is preferably 140~160g/L used in the phosphoric acid anodizing, more preferably 145~155g/
L, most preferably 150g/L.In the specific embodiment of the invention, the phosphoric acid anodizing handles equipment therefor preferably such as Fig. 1 institutes
Show, described Fig. 1 is the structural representation that phosphoric acid anodizing of the present invention handles equipment therefor.As shown in Figure 1, described device is under
It is supreme sequentially to include magnetic force temperature control agitator, magnetic stir bar, magnesium alloy test specimen, Alkaline etchant, beaker, thermometer and direct current
Source, wherein the Alkaline etchant is the phosphoric acid solution；The thermometer thermometric end is inserted into below Alkaline etchant liquid level；The magnesium
Alloy test specimen is the specific embodiment of a metal core board；The magnesium alloy test specimen, Alkaline etchant and magnetic stir bar are placed in burning
In cup.
In the specific embodiment of the invention, the temperature of the phosphoric acid anodizing processing is preferably 10~30 DEG C, more preferably
For 15~25 DEG C, most preferably 20 DEG C；Voltage is preferably 10~20V, more preferably 12~18V, most preferably 15V；Time is excellent
Elect 10~25min, most preferably more preferably 15~20min, 15min as；Electrode spacing is preferably 90~110mm, more preferably
For 95~105mm, most preferably 100mm.
After the phosphoric acid anodizing processing, processing is dried in metal core board described in preferred pair of the present invention, obtains surface
Metal core board after processing.In the present invention, the temperature of the drying process is preferably 100~150 DEG C, more preferably 110~
140 DEG C, most preferably 120~130 DEG C；The time of the drying process is preferably 1~3 hour, and more preferably 1.5~2.5 is small
When, most preferably 2 hours.
In a particular embodiment of the present invention, metal core board and fibres bond the layer contact surface is preferably up to lateral area
Side；Fiber-resin layer and fiber metal the layer contact surface is preferably up to the side of lateral area.In the present invention, institute
The thickness for stating metal core board is preferably 0.1~5mm, more preferably 0.1~4mm, most preferably 0.2~3mm, the metal core board
Thickness be less than fiber metal layer thickness.
In the present invention, the fiber in the fiber and every layer of fiber metal layer in every layer of fiber-resin layer is excellent
Choosing is independently carbon fiber, glass fibre, aramid fiber, basalt fibre, Fypro, aromatic polyester fiber, poly- second
One or more in alkene fiber.In the present invention, when in the fiber in fiber-resin layer or fiber metal layer
Fiber be carbon fiber, glass fibre, aramid fiber, basalt fibre, Fypro, aromatic polyester fiber, polyethylene
During two kinds, three kinds, four kinds, five kinds, six kinds or seven kinds in fiber, the addition for adding fibre fractionation is preferably equal.
In the present invention, the kinds of fibers in every layer of fiber metal layer in two relative fibres bonds layers is identical or not
It is identical.In the present invention, the preferably unidirectional fiber of the fiber or fabric.In a particular embodiment of the present invention, institute
State fiber in the fiber and fiber metal layer in fiber-resin layer it is preferred can according to actual demand direction
Arranged, without other any particular/special requirements；Fiber in every layer of fiber metal layer in two relative fibres bond layers
Can also be identical or differ in direction.
In the present invention, the resin in fiber-resin layer is preferably that epoxy resin, span come amide resin, insatiable hunger
With polyurethane resin, phenolic resin, polyurethane, polyethylene, polyvinyl chloride, polystyrene, polypropylene, acrylic nitrile-butadiene
Diene-styrene copolymer, polyvinyl alcohol, polyacetal resin, polyamide, polyformaldehyde, makrolon, polyphenylene oxide, polysulfones and rubber
One or more in glue.In specific embodiment of the present invention, when the resin is preferably epoxy resin, double maleic amide trees
Fat, unsaturated polyurethane resin, phenolic resin, polyurethane, polyethylene, polyvinyl chloride, polystyrene, polypropylene, third
It is alkene nitrile-BS, polyvinyl alcohol, polyacetal resin, polyamide, polyformaldehyde, makrolon, polyphenylene oxide, poly-
One kind in sulfone and rubber, two kinds, three kinds, four kinds, five kinds, six kinds, seven kinds, eight kinds, nine kinds, ten kinds, it is ten a kind of, 12 kinds,
At 13 kinds or 14 kinds, the addition for adding resin Composition is preferably equal.
In a particular embodiment of the present invention, in the fiber-resin layer fiber and the mass ratio of resin is preferably (40
~80):(20~60), more preferably (50~70):(30~50), most preferably 60:40.
In the present invention, the fibres bond layer includes binding agent and fiber.In the present invention, in the fibres bond layer
Binding agent be preferably that epoxy adhesive, span come amide resin binding agent, unsaturated polyurethane resin binding agent, phenolic aldehyde
Resinoid bond, polyurethane binding agent, polyethylene binder, polyvinyl-chloride binders, polystyrene binder, poly- third
It is alkene binding agent, acrylonitrile-butadiene-styrene copolymer binding agent, polyvinyl alcohol adhesive, polyacetal resin binding agent, poly-
In acid amides binding agent, polyformaldehyde binding agent, polycarbonate adhesive agent, polyphenylene oxide binding agent, polysulfones binding agent and rubber cement
One or more.In specific embodiment of the present invention, when the binding agent is preferably that epoxy adhesive, span carry out acyl
Polyimide resin binding agent, unsaturated polyurethane resin binding agent, phenolic resin adhesive, polyurethane binding agent, polyethylene
Binding agent, polyvinyl-chloride binders, polystyrene binder, polypropylene adhesive, acrylonitrile-butadiene-styrene copolymer
Binding agent, polyvinyl alcohol adhesive, polyacetal resin binding agent, polyamide binders, polyformaldehyde binding agent, polycarbonate adhesive
Two kinds in agent, polyphenylene oxide binding agent, polysulfones binding agent and rubber cement, three kinds, four kinds, five kinds, six kinds, seven kinds, eight kinds,
When nine kinds, ten kinds, ten one kind, 12 kinds, 13 kinds or 14 kinds, the addition for adding binder component is preferably equal.
In a particular embodiment of the present invention, in fibres bond layer fiber and the mass ratio of binding agent be preferably
(40~80):(20~60), more preferably (50~70):(30~50), most preferably 60:40.
Present invention also offers a kind of preparation method of magnesium-based superhybrid composite laminate described in above-mentioned technical proposal, bag
Containing following steps：
By each fiber-resin layer fiber impregnation in resin emulsion, fibre resin prepreg is obtained；
By each fibres bond layer fiber impregnation in binding agent, fiber binder prepreg is obtained；
By the fibre resin prepreg, fiber binder prepreg and metal core board according to the super hybrid composite manner of the magnesium-based
The structural requirement of material laminate carries out laying setting, obtains composite layered plate precursor；
Hot pressing is carried out to the composite layered plate precursor, magnesium-based superhybrid composite laminate is obtained.
Each fiber-resin layer fiber impregnation in resin emulsion, is obtained fibre resin prepreg by the present invention.In this hair
In bright, the resin emulsion be preferably epoxy resin latex, span come amide resin emulsion, unsaturated polyurethane resin emulsion,
Phenolic resin emulsion, polyurethane fat liquor, polyethylene emulsion, polyvinyl chloride emulsion, polystyrene emulsion, polypropylene breast
Liquid, acrylonitrile-butadiene-styrene copolymer emulsion, polyvinyl alcohol emulsions, polyacetal resin emulsion, polyamide emulsion, poly- first
One or more in aldehyde emulsion, polycarbonate emulsion, polyphenylene oxide emulsion, polysulfones emulsion and rubber latex；Described several have
Body is two kinds, three kinds, four kinds, five kinds, six kinds, seven kinds, eight kinds, nine kinds, ten kinds, it is ten a kind of, 12 kinds, 13 kinds or 14
Kind.
In specific embodiment of the present invention, when the resin emulsion is preferably epoxy resin latex, double maleic amide trees
Fat liquor, unsaturated polyurethane resin emulsion, Phenolic resin emulsion, polyurethane fat liquor, polyethylene emulsion, polyvinyl chloride
Emulsion, polystyrene emulsion, polypropylene emulsion, acrylonitrile-butadiene-styrene copolymer emulsion, polyvinyl alcohol emulsions, bunching
In urea formaldehyde emulsion, polyamide emulsion, polyformaldehyde emulsion, polycarbonate emulsion, polyphenylene oxide emulsion, polysulfones emulsion and rubber latex
Two kinds, three kinds, four kinds, five kinds, six kinds, seven kinds, eight kinds, nine kinds, ten kinds, it is ten a kind of, 12 kinds, 13 kinds or 14 kinds
When, the addition for adding resin emulsion component is preferably equal.
The present invention does not have any requirement, the tree to the ratio of fiber and resin emulsion in the fibre resin prepreg
Fat liquor can submerge the fiber.In a particular embodiment of the present invention, the fiber in the fibre resin prepreg
Mass ratio with resin emulsion is preferably (40~80):(20~60), more preferably (50~70):(30~50), be most preferably
60:40。
Each fibres bond layer fiber impregnation in binding agent, is obtained fiber binder prepreg by the present invention.The present invention
There is no any requirement to the ratio of fiber and binding agent in the fiber binder prepreg, the binding agent can submerge institute
State fiber.In a particular embodiment of the present invention, in the fiber binder prepreg fiber and the quality of binding agent
Than being preferably (40~80):(20~60), more preferably (50~70):(30~50), most preferably 60:40.
Obtain after the fibre resin prepreg and fiber binder prepreg, the present invention presoaks the fibre resin
Material, fiber binder prepreg and metal core board carry out laying according to the structural requirement of the magnesium-based superhybrid composite laminate
Set, obtain composite layered plate precursor.In a particular embodiment of the present invention, the laying setting up procedure can be to each layer fiber
Arragement direction and each thickness degree are configured.
Obtain after the composite layered plate precursor, the present invention carries out hot pressing to the composite layered plate precursor, obtains magnesium-based super mixed
Miscellaneous composite-material laminates.In the present invention, the temperature of the hot pressing is preferably 60~350 DEG C, more preferably 100~300 DEG C, most
Preferably 150~250 DEG C；The pressure of the hot pressing is preferably 0.1~1.6MPa, more preferably 0.2~1MPa, is most preferably
0.4~0.6MPa；The time of the hot pressing is preferably 1~10 hour, more preferably 2~8 hours, most preferably 3~5 hours.
Magnesium-based superhybrid composite laminate provided with reference to embodiment the present invention and preparation method thereof carries out detailed
Thin explanation, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
Metal core board used in each embodiment is surface-treated:
The material and thickness of metal core board used in the embodiment 2~8 of table 2
Wherein, metal core board used in embodiment 2 is not surface-treated；Metal core board used in embodiment 3 is as steps described below
It is surface-treated；Metal core board used in embodiment 4 is surface-treated as steps described below, and cleans it in organic solvent
Afterwards, polished before salt is washed using sand paper.
(1) remove and stick thing：The oxide-film on metal core board surface is removed according to scheme described in above-mentioned table 1, be charred thing, protection
Gummed paper, antirust oil, paint word, coating, antiscuffing paste, glue and fingerprint etc..
(2) organic solvent is cleaned：Cleaned using acetone.
(3) salt is washed：Main purpose is to remove the oxide-film of Mg alloy surface, the pretreatment work that this step belongs to before alkaline etching
Skill.Test specimen will be separated and hung, it is not possible to be contacted, and prevented that cleaning is uneven, constantly can be shaken test specimen to accelerate magnesium alloy during cleaning
The chemical reaction velocity on surface.Salt lotion places standby after a period of time after should preparing.The colligation of magnesium alloy member needs to use
Magnesium rod, without other kinds of metal, prevents from bringing corrosiveness.Salt washes technical recipe：Deionized water 1000g, tertiary sodium phosphate
(Na3PO4·12H2O) 55g/L, sodium metasilicate (Na2SiO3) 15g/L, detergent 0.8g/L, salt washes 65 DEG C of temperature, and salt washes the time
2min, salt washes instrument for waste toothbrush.
(4) alkaline etching：Mg alloy surface oxide-film and dirt are thoroughly removed, makes Mg alloy surface uniform activation.Alkaline etchant
Technical recipe is as follows, and the effect of wherein each component is respectively：Sodium hydroxide：Highly basic, will can be changed into that water can be dissolved in after fat saponification
Soap and glycerine；Meanwhile, there is significant corrosiveness to magnesium.Sodium carbonate：Solution alkaline, has to Alkaline etchant and cleaning fluid
There are PH regulations, generally do not have obvious corrosiveness to magnesium product, deoiling effect is fine.Tertiary sodium phosphate：Have and carbon
Sour sodium identical advantage, but also with certain emulsification, because washing property itself is good, contribute to the elution of sodium metasilicate.
Sodium pyrophosphate：Sodium pyrophosphate is similar to sodium phosphate, while having complexing power, prevents article surface from generating insoluble hard water soap
Film, is conducive to raising salt to wash quality.Sodium metasilicate：With certain surface-active and saponifying ability, there is cushioning effect to magnesium,
But washing performance is poor, it not can be used alone.Alkaline etchant technical recipe is：Deionized water 1000g/L, sodium hydroxide (NaOH) 15g/L,
Tertiary sodium phosphate (Na3PO4·12H2O) 40g/L, sodium carbonate (Na2CO3) 15g/L, sodium metasilicate (Na2SiO3) 15g/L, detergent
0.8g/L.Alkaline etching temperature 70 C, alkaline etching time 2min.
(5) hot water wash：Hot water wash temperature is 50 DEG C, time 2min.
(6) cold water is washed：Normal-temperature water, washing time 2min.It should be noted that preventing product surface to be contaminated in cleaning process,
After cleaning surface cannot in atmosphere the residence time it is long, more than 30min, it is necessary to carry out alkaline etching again.
(7) light extraction：Light-emitting solution is the sulfuric acid solution that volume fraction is 25%, at room temperature, soaks 10min.
(8) wash：Product is put into clear water, scrubbed repeatedly with toothbrush in magnesium article surface, water is changed and scrubs 2 times again, often
Secondary 2min.
(9) deionization is washed：Product is put into deionized water, is scrubbed repeatedly with toothbrush in magnesium article surface, changes water brush
Wash 2 times, each 2min.
(10) phosphoric acid anodizing：The oxide layer of phosphate anodizing generation has preferable durability, fatigue durability
Can be good.The phosphoric acid anodizing technical recipe of use is as follows：Phosphoric acid solution 150g/L, 20 DEG C, 15V, 20min, electrode spacing
100mm。
Embodiment 2
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 2：It is comprising two layers of thickness
0.3mm fiber-resin layer and the fiber metal layer that a layer thickness is 0.49mm, the fiber metal layer are located at fiber-tree
In the middle of lipid layer；Fiber architecture direction is consistent in each layer.
Used in one-way glass fiber, fiber-resin layer in the fiber metal layer and fiber-resin layer and use ring
Epoxy adhesive and magnesium alloy plate are used in oxygen tree fat, fiber metal layer.
Embodiment 3
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 3：It is comprising two layers of thickness
0.3mm fiber-resin layer and the fiber metal layer that a layer thickness is 0.45mm, the fiber metal layer are located at fiber-tree
In the middle of lipid layer；Fiber architecture direction is consistent in each layer.
It is one-way glass fiber to be used in the fiber-resin layer in unidirectional carbon, fiber metal layer；Fiber-resin
Used in layer in epoxy resin, fiber metal layer and use epoxy adhesive and magnesium alloy plate.
Embodiment 4
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 4：It is comprising two layers of thickness
0.3mm fiber-resin layer and the fiber metal layer that a layer thickness is 0.46mm, the fiber metal layer are located at fiber-tree
In the middle of lipid layer；Fiber architecture direction is consistent in two layers of fiber-resin layer, fiber and fiber-resin in the fiber metal layer
Fiber in layer is vertical.
One-way glass fiber is used in the fiber metal layer and fiber-resin layer；Using poly- in fiber-resin layer
Polycarbonate adhesive agent and magnesium alloy plate are used in carbonic ester, fiber metal layer.
Embodiment 5
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 5：It is 1mm comprising two layers of thickness
Fiber-resin layer and a layer thickness be 1mm fiber metal layer, fiber metal layer is located in the middle of fiber-resin layer；
Fiber architecture direction is consistent in two layers of fiber-resin layer, the fiber in the fiber metal layer and the fibre in fiber-resin layer
Dimension is vertical.
It is unidirectional polyethylene fibre to be used in the fiber-resin layer in unidirectional carbon, fiber metal layer；Fiber-tree
Used in lipid layer in epoxy resin, fiber metal layer and use epoxy adhesive and magnesium alloy plate.
Embodiment 6
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 6：It is 0.4mm comprising a layer thickness
Fiber-resin layer and two layers of thickness be 0.2mm fiber metal layer, fiber-resin layer is located at fiber metal fat
In the middle of layer；Fiber architecture direction is consistent in each layer.
Use and used in unidirectional Fypro, fiber-resin layer in the fiber metal layer and fiber-resin layer
Phenolic resin adhesive and magnesium alloy plate are used in epoxy resin, fiber metal layer.
Embodiment 7
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 7：It is 1mm's comprising two layers of thickness
Fiber-resin layer and the fiber metal layer that two layers of thickness is 1mm, it is middle that the fiber metal layer is located at fiber-resin layer；Two
Fiber architecture direction is consistent in layer fiber-resin layer, and the fiber in two fiber metals layer is orthogonal, wherein one layer of fiber-gold
The fiber belonged in layer is consistent with the machine direction in fiber-resin layer.
Use and used in unidirectional basalt fibre, fiber-resin layer in the fiber metal layer and fiber-resin layer
Polyethylene binder and magnesium alloy plate are used in epoxy resin, fiber metal layer.
Embodiment 8
A kind of magnesium-based superhybrid composite laminate, its structural representation is as shown in Figure 8：It is 2mm comprising two layers of thickness
Fiber-resin layer and two layers of thickness be 2mm fiber metal layer, fiber-resin layer is located in fiber metal layer
Between；Fiber architecture direction is consistent in two layers of fiber metal layer, and the fiber in two fiber-resins layer is orthogonal, wherein one layer of fibre
Fiber in dimension-resin bed is consistent with the machine direction in fiber metal layer.
Used in unidirectional aramid fiber, fiber-resin layer in the fiber metal layer and fiber-resin layer and use ring
Epoxy adhesive and magnesium alloy plate are used in oxygen tree fat, fiber metal layer.
The magnesium-based superhybrid composite laminate that the present invention is obtained to each embodiment obtains mechanical property and tested, its result
As shown in table 3.
The magnesium-based superhybrid composite laminate that the embodiment of table 3 is obtained is contrasted with current material mechanical property
As shown in Table 3, the magnesium-based superhybrid composite laminate that the present invention is provided has excellent mechanical property, specifically
Its tensile strength is 1295~1300MPa, and stretch modulus is 91~94GPa, and specific strength is 744.25~786.13Mpa/ (g/
cm3), specific modulus is 52.3~54.36GPa/ (g/cm3), bending strength is 1213~1235MPa, layer cut intensity for 85~
89MPa。
As seen from the above embodiment, the invention provides a kind of magnesium-based superhybrid composite laminate, if fine comprising dried layer
If dimension-resin bed and dried layer fiber metal layer, the fiber-resin layer and fiber metal layer are alternately laminated to be set；The fibre
Fibres bond layer of the dimension-metal level comprising metal core board two surfaces relative with metal core board is arranged at, the fibres bond
Layer is bonded to the metal core board and fiber-resin layer；The metal core board is magnesium plate or magnesium alloy plate.The present invention is provided
The magnesium-based superhybrid composite laminate of special construction there is excellent mechanical property.From the experimental result of embodiment,
Tensile strength is 1230~1323MPa, and stretch modulus is 87~90GPa, and specific strength is 549.08~590.59Mpa/ (g/
cm3), specific modulus is 38.84~40.18GPa/ (g/cm3), bending strength is 1325~1382MPa, layer cut intensity for 80~
92MPa。
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of magnesium-based superhybrid composite laminate, if if including dried layer fiber-resin layer and dried layer fiber metal layer, institute
State fiber-resin layer and the alternately laminated setting of fiber metal layer；
Fibres bond layer of the fiber metal layer comprising metal core board two surfaces relative with metal core board is arranged at, institute
Fibres bond layer is stated to bond the metal core board and fiber-resin layer；The metal core board is magnesium plate or magnesium alloy plate.
2. magnesium-based superhybrid composite laminate according to claim 1, it is characterised in that in every layer of fiber-resin layer
Fiber and every layer of fiber metal layer in fiber be independently carbon fiber, it is glass fibre, aramid fiber, basalt fibre, poly-
One or more in nylon, aromatic polyester fiber, polyethylene fibre；
The fiber is unidirectional fibre or fabric.
3. magnesium-based superhybrid composite laminate according to claim 1 or 2, it is characterised in that the fiber-resin layer
In resin come amide resin, unsaturated polyurethane resin, phenolic resin, polyurethane, poly- second for epoxy resin, span
It is alkene, polyvinyl chloride, polystyrene, polypropylene, acrylonitrile-butadiene-styrene copolymer, polyvinyl alcohol, polyacetal resin, poly-
One or more in acid amides, polyformaldehyde, makrolon, polyphenylene oxide, polysulfones and rubber.
4. magnesium-based superhybrid composite laminate according to claim 1, it is characterised in that in the fibres bond layer
It is viscous that binding agent is epoxy adhesive, span comes amide resin binding agent, unsaturated polyurethane resin binding agent, phenolic resin
Tie agent, polyurethane binding agent, polyethylene binder, polyvinyl-chloride binders, polystyrene binder, polypropylene bonding
Agent, acrylonitrile-butadiene-styrene copolymer binding agent, polyvinyl alcohol adhesive, polyacetal resin binding agent, polyamide glue
Tie one kind in agent, polyformaldehyde binding agent, polycarbonate adhesive agent, polyphenylene oxide binding agent, polysulfones binding agent and rubber cement
Or it is several.
5. magnesium-based superhybrid composite laminate according to claim 1, it is characterised in that the fiber-resin layer
Thickness is 0.1~5mm；
The thickness of the fiber metal layer is 0.1~5mm；
The thickness of the metal core board be 0.05~5mm, and metal core board thickness be less than fiber metal layer thickness.
6. the preparation method of magnesium-based superhybrid composite laminate, is comprised the following steps described in Claims 1 to 5 any one：
By fiber-resin layer fiber impregnation in resin emulsion, fibre resin prepreg is obtained；
By fibres bond layer fiber impregnation in binding agent, fiber binder prepreg is obtained；
The fibre resin prepreg, fiber binder prepreg and metal core board are subjected to laying setting, composite layered plate is obtained
Precursor；
Hot pressing is carried out to the composite layered plate precursor, magnesium-based superhybrid composite laminate is obtained.
7. preparation method according to claim 6, it is characterised in that the resin emulsion is epoxy resin latex, span
Come amide resin emulsion, unsaturated polyurethane resin emulsion, Phenolic resin emulsion, polyurethane fat liquor, polyethylene emulsion,
Polyvinyl chloride emulsion, polystyrene emulsion, polypropylene emulsion, acrylonitrile-butadiene-styrene copolymer emulsion, polyvinyl alcohol
Emulsion, polyacetal resin emulsion, polyamide emulsion, polyformaldehyde emulsion, polycarbonate emulsion, polyphenylene oxide emulsion, polysulfones emulsion and
One or more in rubber latex.
8. the preparation method according to claim 6 or 7, it is characterised in that the temperature of the hot pressing is 60~350 DEG C；
The pressure of the hot pressing is 0.1~1.6MPa；
The time of the hot pressing is 1~10 hour.
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| US11346499B1 (en) | 2021-06-01 | 2022-05-31 | Helicoid Industries Inc. | Containers and methods for protecting pressure vessels |
| US11376812B2 (en) | 2020-02-11 | 2022-07-05 | Helicoid Industries Inc. | Shock and impact resistant structures |
| US11852297B2 (en) | 2021-06-01 | 2023-12-26 | Helicoid Industries Inc. | Containers and methods for protecting pressure vessels |
| US11952103B2 (en) | 2022-06-27 | 2024-04-09 | Helicoid Industries Inc. | High impact-resistant, reinforced fiber for leading edge protection of aerodynamic structures |
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| CN107825805A (en) * | 2017-09-28 | 2018-03-23 | 南京工程学院 | One kind is super to mix layered composite structure and preparation method thereof |
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| CN112848555A (en) * | 2021-01-07 | 2021-05-28 | 中国商用飞机有限责任公司北京民用飞机技术研究中心 | Fiber metal laminate composite material and preparation method thereof |
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| US11346499B1 (en) | 2021-06-01 | 2022-05-31 | Helicoid Industries Inc. | Containers and methods for protecting pressure vessels |
| US11852297B2 (en) | 2021-06-01 | 2023-12-26 | Helicoid Industries Inc. | Containers and methods for protecting pressure vessels |
| US11952103B2 (en) | 2022-06-27 | 2024-04-09 | Helicoid Industries Inc. | High impact-resistant, reinforced fiber for leading edge protection of aerodynamic structures |
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