CN105647110B - For the polyether-ether-ketone under corrosive medium erosion operating mode/foam nickel-base alloy bicontinuous composites and preparation method thereof - Google Patents
For the polyether-ether-ketone under corrosive medium erosion operating mode/foam nickel-base alloy bicontinuous composites and preparation method thereof Download PDFInfo
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- CN105647110B CN105647110B CN201610005393.4A CN201610005393A CN105647110B CN 105647110 B CN105647110 B CN 105647110B CN 201610005393 A CN201610005393 A CN 201610005393A CN 105647110 B CN105647110 B CN 105647110B
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- base alloy
- ether
- polyether
- ketone
- foam nickel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/18—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. compression moulding around inserts or for coating articles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
Abstract
The invention discloses a kind of polyether-ether-ketone/foam nickel-base alloy bicontinuous composites being used under corrosive medium erosion operating mode and preparation method thereof, the preparation of the composite is processed into foam nickel-base alloy plate after required shape, in the foam nickel-base alloy that the polyether-ether-ketone of molten state is pressed into column using compression molding method, obtain structural integrity, fill close polyether-ether-ketone/foam nickel-base alloy bicontinuous composites.Prepared composite is made up of the continuous matrix of three-dimensional and reinforcement, and it has three dimensions topological structure, and material distribution continuous uniform, interface binding power is good；Metal material is as reinforcement, beneficial to scattered and transmission stress, good heat conduction effect；Nickel-base alloy (contains chromium, aluminium), and corrosion resistance is strong；Polyetheretherketonematerials materials specific strength is high, and anti-wear performance is good, can obtain preferable erosion resistance effect.The scantling is controllable, traditional material can be substituted under corrosive medium erosion working condition or be used as traditional material liner.
Description
Technical field
The present invention relates to the bicontinuous composites and its preparing technical field under corrosive medium erosion operating mode, specially one
Plant for polyether-ether-ketone/foam nickel-base alloy bicontinuous composites under corrosive medium erosion operating mode and preparation method thereof.
Background technology
Erosive wear refers to the loose little particle of certain particle size in swiftly flowing carrier with certain speed and angle
The phenomenon of spillage of material is impacted and caused to material surface, and this wear phenomenon is because influence is extensive, destruction is serious always
Paid close attention to by domestic and foreign scholars.However, in most of erosion situation, Korrosionsmedium (corrosivity carrier or corrosivity
Grain) participation further exacerbate the destruction of material, reduce the life-span of material.In hydrometallurgy process, corrosivity
Liquid mixes the solid mixed ore pulp of a certain proportion of liquid of composition with slag, its react in high-temperature kettle or in the duct high speed (0.5~
When 5m/s) transporting, various pipes, valve, pump, tank, agitating device etc. can be caused all under the erosion operating mode of corrosive medium, be particularly
In the complex working condition of Fluid-particle two-phase flows erosion, bearing part is occurred defect too early, reduce the operating efficiency of integral device and make
Use the life-span.It is because in engine working process, having sucked the gas of saline mist, high speed gas that the life-span of carrier-borne aircraft, which substantially reduces,
Body is mingled with the critical components such as corrosivity drop damaged blade, makes its premature failure.So far, for corrosion-resistant medium erosion work
Material needed for condition is always the focus of people's research, but a kind of still no material can be good at solution corrosive medium erosion and ask
Topic.
Existing composite is mainly strengthened matrix material using small fiber and particle, and such material is main
Prepared using injection molding forming method, but this method dynamic model temperature is relatively low, and the material of straight forming after mixing can only be carried out
Prepare.And for composite of the foam nickel-base alloy for enhancing phase, due in injection molding process, foamed material hole rate
Greatly, low intensity, easily conquassation is deformed under larger pressure, and can not prepare each mutually uniform composite.Y.Liu et al.
[Preparation and its cavitation performance of nickel foam/epoxy/SiC co-
Continuous composites] the fine and close epoxy resin/nickel foam doubly-linked of filling is prepared for using the method impregnated under vacuum
Continuous composite, but viscosity is relatively low in the curing process for epoxy resin, and nickel foam smoothly can be voluntarily immersed under vacuum conditions
In.Compared to epoxy resin, polyetheretherketonematerials materials specific strength is high, and anti-wear performance is good but higher for viscosity under molten condition
Polyether-ether-ketone, is difficult to fill using vacuum infusion techniques.Therefore polyether-ether-ketone/foam nickel-base alloy bicontinuous composites can not
Prepared with conventional method.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art part to be used for there is provided one kind under corrosive medium erosion operating mode
Polyether-ether-ketone/foam nickel-base alloy bicontinuous composites and preparation method thereof, the polyether-ether-ketone/bubble prepared by this method
Foam nickel-base alloy bicontinuous composites show good erosive wear resistance in corrosive medium erosion experiment, to solve excessively stream
The corrosive medium erosion problem of part provides a kind of new way.
The technical scheme is that：
A kind of polyether-ether-ketone/foam nickel-base alloy bicontinuous composites being used under corrosive medium erosion operating mode, it is described
The composite that bicontinuous composites are made up of polyether-ether-ketone matrix and foam nickel-base alloy reinforcement, the polyether-ether-ketone
It is filled in foam nickel-base alloy skeleton and forms bicontinuous structure；The polyether-ether-ketone/foam nickel-base alloy co-continuous composite wood
Volumn concentration shared by matrix polyether-ether-ketone in material is 64~99%.
In the bicontinuous composites, matrix and reinforcement are continuous on three-dimensional, two phase material is evenly distributed,
It is strong with three dimensions topological structure, interface binding power.
Bubble is made by conductive treatment, plating and reduction sintering by polyurethane foam first in the foam nickel-base alloy plate
Foam nickel plate, reuses powder investment and porous nickel mesh chromising or aluminising is made foam nickel-base alloy plate；Finally use numerical control line
The foam nickel-base alloy of shape needed for porous nickel mesh is processed into by cutting off machine.According to required polyether-ether-ketone/nickel foam co-continuous
The structure and technical indicator of composite choose suitable porous nickel mesh, and the porosity of porous nickel mesh is 64~99%, aperture chi
Very little 0.18~0.87mm, hole density is 50~130PPI.
The preparation method of bicontinuous composites that the present invention is used under corrosive medium erosion operating mode is：First by nickel foam
After the foam nickel-base alloy plate of shape needed for plate is prepared into, then using compression molding method by the polyetheretherketonematerials materials of molten condition
Composite construction is formed in press-in foam nickel-base alloy, annealing heat-treats are carried out to the composite construction after the completion of molding, it is final to obtain
Structural integrity, the close polyether-ether-ketone/foam nickel-base alloy bicontinuous composites of filling.
The compression molding method is carried out in molding die, in forming process, 10 DEG C/min of programming rate, and mould temperature 370~
380 DEG C, soaking time 10min, pressing speed 0.4MPa/min, clamping pressure 4MPa, dwell time 15min.
The annealing heat-treats are that the composite in after compression molding cooling is put into baking oven to carry out；Wherein：Annealing
210 DEG C of temperature, soaking time 40min, with stove Slow cooling.
Compression molding method is prepared before bicontinuous composites, first successively using alcohol and petroleum ether to foam nickel-base alloy point
Not Jin Hang when a length of 10min ultrasonic wave cleaning, remove the oil stain in raw material and be dissolved in the impurity of water；Again to polyether-ether-ketone powder
150 DEG C, 3h drying process are carried out with nickel foam, moisture contained in dusty material is removed；By polyether-ether-ketone powder before compression molding
End, which is placed in mould while applying, to be not less than 35MPa pressure to exclude the air in mould.
The foam nickel-base alloy plate, according to the structure needed for bicontinuous composites, determines its specification and size.
Bicontinuous composites prepared by the present invention are used for corrosive medium (corrosivity carrier or erosive parti) erosion work
Traditional material is substituted under the conditions of condition or is used as traditional material liner.
The beneficial effects of the invention are as follows：
1st, polyether-ether-ketone/foam nickel-base alloy bicontinuous composites will be used in corrosive medium erosion operating mode, wet method smelting
Golden equipment can produce swiftly flowing corrosivity carrier in operation process, and these carriers take solid particle and enter consersion unit
In, flow through pipe, valve, pump, tank and agitating device of equipment etc..Therefore composite must possess isotropic, it is higher resistance to
Corrosive nature, excellent binding ability and good comprehensive mechanical property, conventional composites materials can not meet this requirement.Sent out for this
Understand for the bicontinuous composites and its technology of preparing under corrosive medium erosion operating mode, polyether-ether-ketone/nickel foam of preparation
Based alloy is showed well under the erosion operating mode of corrosive medium.
2nd, the present invention is using polyether-ether-ketone as the matrix of bicontinuous composites, and polyether-ether-ketone is a kind of hypocrystalline high-performance
Speciality polymer material, can with excellent mechanical property, good decay resistance and excellent endurance destructive characteristics
Metal enhancing is mutually played a good protection.
3rd, the present invention by the chromising in nickel foam or is oozed using foam nickel-base alloy as the reinforcement of bicontinuous composites
Aluminium is with the overall decay resistance for improving nickel-base material.Using foam metal as the reinforcement of bicontinuous composites, a side
Dispersion-strengthened action is played in face, on the other hand also helps the scattered and transmission of heat and stress.
4th, using compression molding method prepared by bicontinuous composites, minimum is determined in preparation process and chokes pressure
The nickel foam that power makes intensity relatively low is not deformed during choking by conquassation；Interface has opened up a plurality of row above and below molding die
Gas passage, to make highly viscous molten state polyether-ether-ketone be totally immersed into the Ni-based conjunction of foam of hole very little (about 200 μm or so)
Jin Zhong.
5th, the annealing heat-treats under certain temperature are carried out to bicontinuous composites, by being carried out to bicontinuous composites
40min annealing heat-treats at 210 DEG C, can be greatly improved the crystallinity of polyetheretherketonematerials materials and further in the short period
Lift the comprehensive mechanical property of bicontinuous composites.
Brief description of the drawings
Fig. 1 is the preparation technology flow of bicontinuous composites of the present invention.
Fig. 2 prepares the compression molding device used during bicontinuous composites for the present invention.
In figure：1- compression legs；2- feed compartments；The upper moulds of 3-；Mould under 4-；5- workbenches；6- polyether-ether-ketone powder；7- nickel foams
Based alloy；8- jack.
Fig. 3 is polyether-ether-ketone/foam nickel-base alloy co-continuous composite wood of prepared matrix material percentage composition 97%
Material；Wherein：(a) it is (Φ 30 × 10) mm polyether-ether-ketones/foam nickel-base alloy bicontinuous composites of preparation shaping；(b) it is
Polyether-ether-ketone/foam nickel-base alloy bicontinuous composites surface microscopic topographic.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
The present invention be for the polyether-ether-ketone under corrosive medium erosion operating mode/foam nickel-base alloy bicontinuous composites and
Its preparation method, the preparation flow of the composite as shown in figure 1, be processed into foam nickel-base alloy after required shape,
The polyether-ether-ketone of molten state is pressed into foam nickel-base alloy skeleton using compression molding method, structural integrity, filling is obtained closely
Polyether-ether-ketone/foam nickel-base alloy bicontinuous composites.The structure of compression molding device used is as shown in Figure 2.
The compression molding device includes workbench 5, upper mould 3, lower mould 4, feed compartment 2 and compression leg 1；Lower mould 4 is fixed on work
Make on platform, upper mould is fixed on lower mould 4, foam nickel-base alloy 7 is placed in the inner chamber of upper mould 3, and inner chamber can be according to be prepared
The shape and size of composite are designed；Feed compartment 2 is placed on mould 3, compression leg 1 and work by the top of feed compartment 2
The jack 8 of platform lower is engaged, and polyether-ether-ketone is pressed into foam nickel-base alloy skeleton.In the compression molding device, pressure
Exhaust passage (being opened on the surface being in contact with raw material) is opened up on post 1 and lower mould 4, is respectively used to discharge raw material polyethers ether
Gas in ketone powder 6 and lower mold cavity, so that the bicontinuous composites for avoiding preparation have the defects such as hole.
Polyether-ether-ketone of the present invention/foam nickel-base alloy bicontinuous composites preparation technology detailed process is following (referring to figure
1)：
1st, the preparation and processing of nickel foam
According to the size and technical requirement of bicontinuous composites, by calculating, the specification of porous nickel mesh is determined, i.e.,
Surface density, aperture, thickness, porosity, chromium aluminium content etc., select the uniform nickel foam chromium plate of superior in quality, hole.Using numerical control
The column foam nickel chromium triangle of size needed for wire cutting machine tool is processed as, needs to ensure that nickel foam chromium plate is protected during cutting
Maintain an equal level whole, it is ensured that the uniformity of the size of column foam nickel chromium triangle；Using water base coolant as cutting liquid, nickel foam is avoided as far as possible
The pollution of chromium.Nickel foam adds it to Ultrasonic 10min in alcohol after having cut, finally use petroleum ether sonic oscillation
10min；Dry in an oven, then samples weighing, measure its size, and be placed on standby in drying box.
2nd, the preparation and processing of polyether-ether-ketone powder
According to the technical requirement of bicontinuous composites, by calculating, the quality of polyether-ether-ketone powder is determined.To it
Carry out the water in 150 DEG C, 3h drying process, discharge polyether-ether-ketone powder.Powder after processing is put into standby in drying box.
3rd, compression molding method prepares bicontinuous composites
The polyether-ether-ketone powder after processing is put into molding die first, applies 35MPa pressure venting mould to it
With the additional air in powder.Then column foam nickel-base alloy is equally put into molding die, with 10 DEG C/min heating speed
Mould is heated to after 380 DEG C, insulation 10min with 0.4MPa/min speed to the slow application matched moulds of bicontinuous composites by rate
Pressure so as not to due between mould tolerance make polyether-ether-ketone all spillings more greatly, control final clamping pressure to be no more than 4MPa in order to avoid will
The conquassation of foam nickel-base alloy is deformed.Last pressurize 15min ensures that the polyether-ether-ketone of molten condition is totally immersed into the tiny bubble in aperture
In foam nickel-base alloy, power-off cooling.
4th, the heat treatment of bicontinuous composites
Bicontinuous composites mechanical property after compression molding is still unstable, it is necessary to carry out certain temperature to it
Annealing heat-treats.When material to be composite is cooled to 230 DEG C with mould, puts it into and be warming up in advance in 210 DEG C of baking oven, be incubated
40min is so that the crystallinity of polyether-ether-ketone is maximized in composite.Cool to the furnace after room temperature and composite is taken out and taken off
Mould.Stable mechanical property, compact structure, polyether-ether-ketone/foam nickel-base alloy co-continuous of composite performance index is finally given to answer
Condensation material.
Embodiment 1：
The preparation of the polyether-ether-ketone of matrix material percentage composition 97%/foam nickel-base alloy bicontinuous composites：
Exemplar size needed for tester for testing scouring wear is (Φ 30 × 10) mm, it is therefore desirable to prepare the installation of Pass Test machine
Bicontinuous composites.It is 0.26g/cm from volume density3, aperture be that 100PPI, porosity are that 97.1%, size is
1000mm × 1000mm × 10mm nickel foam chromium plate (chromium content 12%), (Φ 30 is processed into numerically controlled wire cutting machine
× 10) mm column foam nichrome, cleans respectively through 10min alcohol and petroleum ether ultrasonic wave and dries and weigh.
Used polyether-ether-ketone powder provides for Jilin University, and its particle diameter is 200 μm.Weigh 10g polyether-ether-ketone powder
And the drying process for carrying out 150 DEG C of duration 3h is put it into baking oven.
Dried powder is put into molding die, the precompression for applying 35MPa is compacted into for bulk, being put into processing
Column foam nickel-base alloy afterwards.With 10 DEG C/min programming rate heating, mould is to 380 DEG C and is incubated 10min.With 0.4MPa/
Min speed, which is slowly forced into mould after 4MPa, pressurize 15min, powers off cooling.Material to be composite is cooled to after 230 DEG C, will
It, which is put into be preheated in 210 DEG C of baking oven, is incubated 40min, then cools to room temperature demoulding sampling with the furnace, obtains polyether-ether-ketone body
Polyether-ether-ketone/foam nickel-base alloy bicontinuous composites that product percentage amounts are 97%
Fig. 3 is polyether-ether-ketone/foam nickel-base alloy co-continuous composite wood of prepared matrix material percentage composition 97%
Material.By observation, bicontinuous composites surfacing manufactured in the present embodiment, inside filling is uniform complete, polyether-ether-ketone
Volume basis amount is about 97%, can carry out related experiment as erosion experiment exemplar.
Answered using polyether-ether-ketone/foam nickel-base alloy co-continuous of matrix material percentage composition 97% manufactured in the present embodiment
Condensation material and pure polyether-ether-ketone carry out following two erosions experiments respectively：
1. in the H of mass fraction 1%2SO4Mixing quality fraction is 5% ore particles (275 mesh) in solution, with 30m/s
Speed the mixed slurry is impacted into material sample surface, it is carried out duration 2h, 90 ° of the angle of attack jet experiment.
2. in the H of mass fraction 1%2SO4Mixing quality fraction is 5% ore particles (275 mesh) in solution, with 30m/s
Speed the mixed slurry is impacted into material sample surface, it is carried out duration 2h, 30 ° of the angle of attack jet experiment.
After the erosion experiment of the different angles of attack of two above, measure and contrast polyetheretherketonematerials materials and polyether-ether-ketone/bubble
Volume Loss amount (mm before and after the experiment of foam nickel-base alloy bicontinuous composites3).Experimental result shows that polyetheretherketonematerials materials exist
Under 90 ° and 30 ° of angles of attack, Volume Loss amount is respectively 29.5mm3And 6.4mm3；Polyether-ether-ketone/foam nickel-base alloy co-continuous is combined
Material is under 90 ° and 30 ° of angles of attack, and Volume Loss amount is respectively 11.8mm3And 5.7mm3.Experiment proves that polyether-ether-ketone/foam is Ni-based
Alloy bicontinuous composites are either under the big angle of attack or under Low Angle Of Attack, and its Volume Loss amount is respectively less than pure polyether-ether-ketone
Volume Loss amount, therefore illustrate using polyether-ether-ketone as matrix, foam nickel-base alloy is used as the doubly-linked prepared by reinforcement
Continuous composite erosive wear resistance is improved.
Claims (9)
1. a kind of polyether-ether-ketone/foam nickel-base alloy bicontinuous composites, its feature being used under corrosive medium erosion operating mode
It is：The composite that the bicontinuous composites are made up of polyether-ether-ketone matrix and foam nickel-base alloy reinforcement, institute
State polyether-ether-ketone and be filled in foam nickel-base alloy skeleton and form bicontinuous structure, the polyether-ether-ketone/foam nickel-base alloy is double
In continuous composite material, volumn concentration shared by matrix polyether-ether-ketone is 64~99%.
2. bicontinuous composites according to claim 1, it is characterised in that：In the bicontinuous composites, matrix
Continuous in three-dimensional with reinforcement, two phase material is evenly distributed, with three dimensions topological structure.
3. bicontinuous composites according to claim 1, it is characterised in that：The foam nickel-base alloy is to use powder
Investment carries out chromising to nickel foam or aluminising is made.
4. bicontinuous composites according to claim 3, it is characterised in that：The porosity of the nickel foam be 64~
99%, 0.18~0.87mm of aperture size, hole density are 50~130PPI.
5. the preparation method of bicontinuous composites according to claim 1, it is characterised in that：This method chooses institute first
The foam nickel-base alloy of specification and shape is needed, the polyetheretherketonematerials materials of molten condition are then pressed into by foam using compression molding method
Composite construction is formed in nickel-base alloy, annealing heat-treats are carried out to the composite construction after the completion of molding, that is, obtains polyether-ether-ketone/bubble
Foam nickel-base alloy bicontinuous composites.
6. the preparation method of bicontinuous composites according to claim 5, it is characterised in that：The compression molding method exists
Carried out in molding die, in forming process, 10 DEG C/min of programming rate, 370~380 DEG C of mould temperature, soaking time 10min, pressurization
Speed 0.4MPa/min, clamping pressure 4MPa, dwell time 15min.
7. the preparation method of bicontinuous composites according to claim 5, it is characterised in that：The annealing heat-treats are
The composite construction that compression molding is obtained is put into baking oven, and carries out annealing heat-treats to it；Wherein：210 DEG C of annealing temperature, is protected
Warm time 40min, with stove Slow cooling.
8. the preparation method of bicontinuous composites according to claim 5, it is characterised in that：Using compression molding legal system
Before standby bicontinuous composites, ultrasonic wave cleaning, cleaning are carried out to foam nickel-base alloy using alcohol and petroleum ether successively first
Time is 10min, with the impurity for removing the oil stain in raw material and being dissolved in water；Polyether-ether-ketone powder and foam nickel-base alloy are entered again
150 DEG C of row, 3h drying process, remove contained humidity in dusty material；Polyether-ether-ketone powder is placed in mould before compression molding
Apply simultaneously and be not less than 35MPa pressure to exclude the air in mould.
9. the preparation method of bicontinuous composites according to claim 5, it is characterised in that：The foam nickel-base alloy
According to the structure of required bicontinuous composites, its specification and size are determined.
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| CN201610005393.4A CN105647110B (en) | 2016-01-06 | 2016-01-06 | For the polyether-ether-ketone under corrosive medium erosion operating mode/foam nickel-base alloy bicontinuous composites and preparation method thereof |
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